Frequency Selective Surface

THE NOTTINGHAM TRENT UNIVERSITY
Department of Electrical and

Electronic Engineering
An Investigation into the Feasibility of designing Frequency Selective
Windows employing periodic structures (Ref. AY3922)
Final Report
for
The Radiocommunications Agency
C. Mias, C. Tsakonas, C. Oswald
Dept. of Electrical & Electronic Eng.
The Nottingham Trent University
Burton Street
Nottingham
NG1 4BU
U.K.
Tel: +44 (0) 115 848 2069
Fax: +44 (0) 115 848 6567
Email: christos.mias@ntu.ac.uk
http://www.ntu.ac.uk
i
Acknowledgements
The authors would like to thank their supporting team for providing assistance with all
the measurements. In particular, Tian Hong Loh for assisting in the measurements,
preparation of the final report and presentation of results; Jeff Baines for constructing
the large measurement rig; Yiannis Passas for helping with the preparation of the
interim report and the presentation of results.
They also thank Dr. Wayne Cranton and Prof. Clive Thomas, of the thin film
laboratory, for allowing access to their clean room facilities. In particular, they would
like to thank Alan Liew and Demos Koutsogeorgis for assisting in the fabrication of
transparent oxides and the etching of FSS.
The authors would like to thank the following undergraduate students: Daniel
Monument, Minas Kanetos, Hussein Essajee, Chris Cherrington and Russell
Vickerman for assisting in the FSS and permittivity measurements.
The assistance of Mahesh Dudhia at the RAs Whyteleafe Laboratory and the helpful
discussions with Bill Martin are also gratefully acknowledged.
ii
Summary
It is the conclusion of this feasibility study that frequency selective windows with
good shielding characteristics can be constructed. At the moment, frequency selective
surfaces (FSS) made from silver paint (section 6), which is an opaque conductor,
outperform optically transparent conductor FSS. It was observed, however, that FSS
constructed from good quality, highly transparent in-house Indium Tin Oxide can
have a satisfactory performance (section 8). These results are encouraging as the
conductivity of the ITO can be reduced further (section 7).
For the FSS box, a 20dB attenuation performance was observed for the hexagonal
element frequency selective windows used to construct it. We believe that the
attenuation will increase further by employing a silver paint of higher silver
concentration and hence conductivity than the 60% silver paint employed in this work
(section 1). The microwave oven measurements in the presence of the FSS box
demonstrated that there is a satisfactory attenuation, around 20 dB. The performance
of the enclosure is improved by using absorbers to eliminate multipath propagation
effects (section 9).
iii
CONTENTS page
Section 1: Introduction to FSS 1
History of FSS ; Review of research on optically transparent
microwave FSS and frequency selective windows at 2.45 GHz.;
Applications of transparent or opaque conductor FSS Windows;
Design by example; Factors of influencing the FSS performance and
design; Fundamental theory of spatially periodic structures.
Section 2: Description of FSS filter types 16
FSS Filter types; Convoluted FSS ( Fratcal FSS).
Section 3: Investigation of band-stop FSS filters at NTU 22
Introduction; Experimental procedures and measurement set up;
Experimental investigations; Experimental Investigations; Appendices
(A-G).
Section 4: Techniques of measuring the dielectric properties of FSS
substrates 41
Introduction; Introduction to coaxial probe; Theory and Experimental
Results; The free space measurement method.
Section 5: Numerical techniques 56
Introduction; Equivalent circuit method; Method of moments.
Section 6: Opaque Conductor FSS 66
Conductive Paints; Fabrication overview; Fabrication methods.
Section 7: Review of Transparent and Conductive Oxides 75
Introduction; Growth Techniques; Chemical Vapour Deposition
(CVD); Vacuum Evaporation; Sputtering; In-House Deposition of
ITO; Ion-Assisted Deposition Techniques; Spray Pyrolysis; Sol-Gel
Technique; Laser-Assisted Deposition Techniques; Anodisation;
Commercially available sources of TCOs; Electrical Properties;
Optical Properties.
Section 8: Highly Conductive ITO Frequency Selective Structures 122
Introduction; In-House Fabrication and Characteristics of the ITO;
Experimental Procedures and Results; Conclusions.
Section 9: FSS Box and Microwave Oven Measurements 127
Introduction; Enclosure Structure; Hexagonal Element FSS;
Microwave Oven Measurements.
Section 1: Introduction to FSS Frequency Selective Windows
1
Section 1: Introduction to Frequency Selective Surfaces (FSS)
History of FSS
The frequency selective surfaces (FSS) are periodic structures in either one or two
dimensions (i.e. singly or doubly periodic structures) which perform a filter operation.
Thus, depending on their physical construction, material and geometry, they are
divided into low-pass, high-pass, band-pass and band-stop filters.
As can be seen in Figure 1 the FSS can be cascaded to form a triply-periodic structure
which is commonly known as a photonic crystal.
The FSS were intensively studied since the 1960s [12] although as early as 1919
Marconi patented such periodic structures [3]. From 1969 until the end of 2000, more
than 200 papers were published containing the keyword "frequency selective surface"
(INSPEC Catalogue search 12/1/2001). Early work concentrated on the use of FSS in
Cassegainian subreflectors in parabolic dish antennas. FSS are now employed in
radomes (terrestrial and airborne), missiles and electromagnetic shielding
applications.
The analysis of FSS started with mode matching techniques which were first applied
to aperture problems. In addition, the mode matching method led to the approximate
method of equivalent circuit analysis which gave some insight into the behaviour and
design of FSS. With the advent of computers more accurate numerical techniques
were developed for the analysis of FSS. The techniques used in the mode matching
method which initially was applied to solve aperture type FSS problems, were
employed to solve patch problems. Other powerful numerical methods such as the the
finite difference time domain method and the finite element method were also
employed to solve FSS problems.
Experiments are necessary to verify the performance of practical FSS structures,
confirm the accuracy of theoretical/numerical predictions and provide results for FSS
structures which are difficult to simulate.
Review of research on optically transparent microwave FSS and frequency
selective windows at 2.45 GHz.
To the best of our knowledge, there are three reports on optically transparent
conductor FSS and FSS windows:
Figure 1
2
1. A journal paper [4] authored by Prof. Parker and his research team at Kent
University, UK, detailing the effect of conductivity on the performance of
optically transparent conductor FSS situated on opaque dielectric substrates.
Circular patch (band-stop FSS) and slot rings (band-pass FSS) were employed as
FSS elements in a square lattice arrangement (figure 2). They were fabricated
using 20/! Indium Tin Oxide (ITO) and 4-8/! Thin-film Silver (Ag). The
bandstop/bandpass regions were above 10 GHz. Test at normal and angular (45)
plane wave incidence were made for both transverse magnetic (TM) and
transverse electric (TE) polarisations. By comparing the performance of these
transparent conductor FSS with copper FSS it was concluded that it is feasible to
construct optically transparent FSS provided the conductivity of the conductor is
below 4-8/!.
2. A conference paper by the Kajima Technical Research Institute, Japan [5]. They
employed silver paint (95% Ag). The silver paint was deposited directly on glass.
In the paper, the group presented two band-stop FSS structures. The first (Figure
3a) had a band stop frequency centered at 1.95GHz and employed tripoles as FSS
elements. The second FSS (Figure 3b) had two band-stop frequencies, at 1.9GHz
and 2.4GHz and consisted of 'hybrid' elements (tripoles within triangular shaped
elements).
The authors tested a variety of opaque materials. The choice of material was
influenced by two factors: (a) the conductivity of material which significantly
affects FSS performance and (b) the width of the material which affects both the
Figure 2: Circular patch (a)and slot rings (b) in a square lattice
arrangement.
(a)
(b)
Figure 3: (a) tripole element FSS; (b) tripole element within trianglular
element FSS.
(a)
(b)
3
resistance of the FSS element and the optical transparency. Silver paint was the
chosen material which allowed FSS elements of width diameters of 0.5mm to be
used with a resulting attenuation of 35dB or more. Wedged guide horn antennas
were used in the tests. The glass size was 60cm60cm. Test conditions allowed
for angles of incidence to be between 0 and 60 to the normal for both
polarisations (vertical and horizontal). Antenna distance was 60cm and 200cm.
The results in the paper are for the tripole structure and for normal incidence.
They cover the range of 1-3GHz.. The bandstop frequency is at 1.9GHz and the
frequency region over which transmission falls below 30dB has a width of
35MHz.
3. Nippon product page [6] on the World Wide Web (WWW). The company designs
transparent films for windows that can shield at some desired frequencies. Either
2.45GHz for wireless local area network (LAN) applications or 1.9GHz for
Personal Hand-Phone System (PHS) applications. They also indicate that their
product does not disturb mobile phone communication bands at 900 MHz and
television frequency bands.
The conclusions drawn from the above reports are:
(1) Transparent conductors can be employed provided that the conductivity is less
than 4-8/!.
(2) Silver paint FSS glass have a lower cost of production than other types of
shielding glass and much higher conductivity than transparent conductor
materials. The disadvantage is that the silver paint is opaque but it is compensated
by the fact that the width of the elements can be made very small because of the
enhanced conductivity of the paint.
(3) The problem of gaps between frames and window glass can be solved by using the
silver paint to cover them.
Applications of transparent or opaque conductor FSS Windows
1. Selective shielding of the electromagnetic interference from high power
microwave heating machines adjacent to wireless communication base-stations.
2. Selective shielding of frequencies of communication in sensitive areas (military
installations, airport, police etc.)
3. Protection from harmful electromagnetic radiation especially in the 2-3GHz band
[7] arising externally (wireless communication base stations) or internally
(microwave ovens) in the domestic environment, schools, hospitals etc.
4. Control of radiation at unlicensed frequency bands (eg. Bluetooth applications,
2.45GHz).
5. Picocellular wireless communications in office environments such as the Personal
Handy-phone System in offices whereas to improve efficiency each room needs to
prevent leakage of radio waves into another room. This implies that windows,
floor and ceiling need to be shielded.
6. Isolation of unwanted radiation. FSS windows can be incorporate in trains to
prevent mobile phone frequencies.
Note: that in the above applications one wishes to prevent certain frequency bands of
electromagnetic radiation to be transmitted whereas others are required to pass
4
(frequencies related to emergency services for example). Hence the use of a
broadband shielding material is not an option.
Design by example
Example 1 (the example was presented by G. Gregorwich [8] at the 1999 Aerospace
Conference).
Problem: Design an FSS structures that can transmit data across the 2.2 to 2.4 GHz
frequency range (in S-Band) and reject data across the 5.4 to 5.9 GHz frequency range
(in C-Band).
Step 1: Choose a suitable element or combination of elements. The choice depends on
the desired characteristics and the designers experience. The latter is accumulated via
experiments or numerical simulations. Table 1, presented in Wu [13], shows the
performance of some elements relative to others.
Table 1: Element shape and perfromance based on free-standing single screen
performance.
Ratings: best = 1, second best = 2 etc.
Type of Element Angular
insensitivity
Cross-
Polarisation
Larger
Bandwidth
Small band
separation
Loaded dipole 1 2 1 1
Jerusalem cross 2 3 2 2
Rings 1 2 1 1
Tripole 3 3 3 2
Cross dipole 3 3 3 3
Square loop 1 1 1 1
Dipole 4 1 4 1
In this example it was decided that a combination of a square grid and a Jerusalem
cross is used. The square grid acts as a high-pass filter and the cross as a band stop
filter. One could have chosen a square patch but the choice of the cross allows the
designer to employ more tuning parameters. Thus, maximisation of the bandpass
transmissivity and choice of bandstop frequency can be achieved simultaneously.
h
g
w
D
P
a
L
Figure 4: Gridded Jerusalem cross.
5
Let T be the thickness of the metal of the Jerusalem cross.
Step 2: Decide on the procedure (experimental or theoretical) to be followed to assess
the performance of the FSS structure. Let us, following Gregorwich, use the equations
he presents for the FSS. A very accurate analysis at this stage is no important. It is
important however to see, via the analytic equivalent circuit formulae, the effect of the
various geometric parameters on the FSS performance. His analysis assumes that
< << < << < << << D g P h P W T a T , , , (1)
The equivalent circuit of the gridded Jerusalem cross is a series LC circuit
According to the paper, for the Jerusalem cross,
,
_
w
P P
L

2
ln (2)
,
_
g
P D
C

2
ln
4
(3)
,
_

C
L j jX Z
1
(4)
Thus, from transmission line theory, the power transmitted through the FSS is
2
2
2 2
4 1
4
1
X
X
R T
+
(5)
In addition, at resonance
1 LC
r
or
LC
f
r
2
1
(6)
Hence,
,
_
,
_
g
P
w
P
PD
r

2
ln
2
ln 2 (7)
C
L
Z
0
=1
Z
0
=1 L C
Figure 5: Equivalent circuit of gridded Jerusalem cross.
6
Thus, to optimise the power transmission in the passband, X must be as large as
possible which implies that L or 1/(C) must be as large as possible. But the L-C
values must satisfy the resonance condition. So a compromise must be reached.
Step3: Based on FSS theory, numerical analysis and experiments, rules of thumb are
derived to assist in the design of the FSS structure. The guidelines for the design of
the Jerusalem cross structure are as follows:
Bandwidth of stopband increases as W and D increase .
Bandwidth of stopband increase by reducing h and g.
The passband approaches the stopband by increasing a and/or reducing g.
To avoid grating lobes keep the period less than 0.5.
More multigrid FSS, the effects of dielectric separation can be canceled out by
spacing the FSS grids /4 apart.
To avoid coupling phenomena the FSS grids must be placed at least /2 from the
transmitting/receiving antenna (in the specific example it was a phased array
antenna).
By stacking identical layers of FSS the bandstop attenuation increases.
If the FSS grid is placed inside a dielectric then the resonance frequency becomes
lower.
Step 4: Test and modify. From the rules, a structure of suitable geometrical
dimensions is constructed and tested. Since the equivalent circuit is true for normal
incidence, angular incidence experiments must be carried out. If there is attenuation in
the passband region then the square grid can be modified or eliminated. Furthermore,
if the equivalent circuit cannot take into account the dielectric substrate, the FSS must
be redesigned to allow for the effect of the substrate. Novel approaches can be
followed to improve further the FSS performance. For example if the bandwidth
needs to increase one may stack two Jerusalem FSSs with different geometrical
parameters.
Example 2 (the example was published by M.A.A. El-Morsy [9], E.A. Parker and R.J.
Langley [9])
Ideally one wishes to apply synthesis, based on a desired transmission response, to
obtain the desired parameters of FSS. Assume that the following FSS response is
required. This response can be recognised as that of a network with reactance
admittance given by
e

2

T
r
a
n
s
m
i
t
t
e
d

p
o
w
e
r
0
Figure 6
7
( )
( )
2
2
2
2
1
2

jH
Y (8)
At
1
there is a zero corresponding to a transmission resonance, at
2
there is a pole
corresponding to a reflection resonance and H is a scale factor. The above equation
can be expanded in partial fractions as follows:
2
2
2

+
B A
Y (9)
where A and B are coefficients to be determined.
The equivalent circuit described by the above equation is
A and B can be expressed in terms of H. Furthermore,
( ) ( )
2 / 1
2 0 2
1
1
L L C +
(10)
( )
2 / 1
2 2
2
1
L C
(11)
2 0
2 0
L L
L L
H
+
(12)
and
2 2
2
2
0
1
1
C L
C j
L j
Y

+ (13)
By specifying one more condition, say the transmitted power at
e
, the values of L
0
,
L
2
and C
2
can be uniquely determined. Once a suitable element has been identified, a
set of non-linear equations, involving the circuit component values and the
dimensions of the element, are solved to obtain the exact element geometry. In
general L and C are expressed in terms of the FSS period, widths of the various
conductor strips, gap distances between the conductors angle of incidence and
wavelength.
L
2
L
0
Figure 7: The equivalent circuit for equation (9).
C
2
8
) , , , , ( h w P L L (14)
) , , , , ( h w P C C (15)
Recenetly, genetic algorithms have been employed to construct FSS [14].
Example 3 (the example was published by M.A.A. El-Morsy, E.A. Parker and R.J.
Langley)
The spectral response in Figure 8 response below can be obtained from the
accompanied FSS element.
It is therefore natural to suppose that by cascading two such grids of different
geometrical sizes one can obtain more transmission resonances. As a matter of fact
El-Morsy found that provided the conductors are not closely spaced this cascaded
structure is equivalent to a gridded double square (Figure 9).
Example 4: Cascaded grids
Transmission line methods provide flexibility in designing cascaded FSS structures.
Consider a cascade of grids. The grids are modelled using the equivalent circuit
equations of Lee and Zarrillo [15]. Despite the fact that the formulae in [15] do not
take into account the evanescent harmonics there is a good agreement between
experimental and numerical results. The latter is obtained by making use of
transmision line formulae [16]. Numerical and experimental results for the grid
T
r
a
n
s
m
i
t
t
e
d
p
o
w
e
r
1

2
0
Figure 8: Response of gridded square.
1
2

T
r
a
n
s
m
i
t
t
e
d
p
o
w
e
r
0

3

4
Figure 9: Response of gridded double square.
9
structure shown in Figure 9 are plotted in Figure 10. Figure 10 shows transmittance
results for three grid separation distances. The presence of the polyester substrate,
which is not accounted for in the equivalent circuit model, contributes towards the
diferrence between the two sets of results. Experimental results, as explained in
section 3, should be ignored.
(c)
0 1 2 3 4 5 6 7 8 9 10
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
T
R
A
N
S
M
I
T
T
A
N
C
E

d
B
0 1 2 3 4 5 6 7 8 9 10
x 10
9
-45
-40
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
T
R
A
N
S
M
I
T
T
A
N
C
E

d
B
0 1 2 3 4 5 6 7 8 9 10
x 10
9
-50
-40
-30
-20
-10
0
10
FREQUENCY Hz
T
R
A
N
S
M
I
T
T
A
N
C
E

d
B
(a)
(b)
Figure 10: Transmittance through a cascade of two grids
p=19.4mm, d=17.7mm. (a) d=23mm; (b) d=46mm; (c) d=69
Figure 9: A cascade of grids.
p
h
d
Normally incident
plane wave
10
Example 5: Effect of lossy conductive material
Compared with copper which might be considered as a material of infinite
conductivity, the silver paint and the transparent conductor have much lower
conductivities resulting in a finite resistance value along the conductive elements. Let
this loss be represented by a resistance in series with the conductor inductance as
shown in Figure 11. The same figure also shows how by varying this resistance value
the transmitted power through a bandstop FSS varies.
The effect of resistance is indicated in the experimental graphs in Figure 12 where the
same FSS pattern is made from copper and silver paint.
0 0.5 1 1.5 2 2.5 3
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
angular frequency
n
o
r
m
a
l
i
s
e
d

t
r
a
n
s
m
i
t
t
e
d

p
o
w
e
r
Lossy FSS - parallel-LC (L=C=1) with loss R in series with L
i
n
c
r
e
a
s
i
n
g

R
Z
0
R
L
Z
0
C
Figure 11: Effect of lossy conductive medium.
1 2 3 4 5 6 7 8 9 10 11 12
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
m
)
Copper square loops
1 2 3 4 5 6 7 8 9 10 11 12
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
m
)
Silver square loops
Figure 12: Comparison of the trnasmittances of copper (very good
conductor) FSS and silver paint (lossy conductor) FSS
11
Factors Influencing the FSS performance and design
The performance and behaviour of the FSS filters depends on the following factors:
(1) The conductivity of the FSS conductor.
(2) The geometry of the FSS element (shape, with of conductive striplines, proximity
of conductive striplines, thickness of conductor)
(3) The permittivity of the FSS substrate.
(4) The period of the FSS array.
(5) The number of FSS arrays when these are employed in a cascade.
(6) The electrical distance between the FSS arrays in cascade configurations.
(7) The choice of element types in hybrid FSS configuration.
(8) The finite number of periods and the metallic frames surrounding the FSS
window.
The influence of some of the above factors can be quantified theoretically leading to
generic rules. The influence of the rest of the factors must be determined
numerically/experimentally leading, in some cases, to specific (to the element) rules
of thumb. Let us therefore determined the generic rules.
Fundamental Theory of Spatially Periodic Structures
Assuming that a periodic structure has an infinite number of periods, Floquets
theorem applies. The theorem states that:
For a given mode of propagation at a given steady-state frequency the fields (electric
or magnetic) at one cross-section differ from those a period away only by a complex
constant.
For simplicity, let us consider a singly periodic structure that is assumed to be infinite
and uniform in the y-direction. Therefore, for modelling purposes, it is assumed to be
two dimensional. From Floquets theorem, the field F (E or H) satisfies the following
equation,
z
D
z
z
e ) z , x ( ) D z , x (

+ F F (1)
where
z
is the Floquet constant. Consequently, the field in the periodic structure can
be described as,
z
z
p
e ) z , x ( ) z , x (

F F (2)
where Fp denotes the periodic part of the field. Since Fp can be represented by a
Fourier series. F is written as,
( )
n
z
z
D / n j
z
n
e ) x ( ) z , x (
2
G F (3)
12
Each of the terms of the series in equation (3) is called as spatial harmonic. For the
scattering problems, provided the incident plane wave is not attenuated or amplified in
the direction of the periodicity (i.e. there is no loss or gain in region 1 of Figure13), .
z z
j (4)
where
z
is a real value variable.
Figure 13: An 2D singly periodic structure. The unit cells is shown with a dashed
line. The structure is assumed to be infinite and uniform along the y-direction.
Therefore, each harmonic has a propagation constant, in the direction of periodicity,
given by,
z
z zn
D
n

2
+ (5)
In addition, in the direction of the periodicity, the Floquet constant is equal to the
propagation constant of the incident plane wave. If the incident plane wave is
assumed to be of the form,
z
inc
z
jk x
inc
x
jk inc inc
e e

A F (6)
then
inc
z zn
k (7)
inc
x
k
1
k
inc
z
k
Incident plane
wave
Unit cell 1 1
,
z
D
Y
Z
X
Region 1
Region 2
2 2
,
13
The scattered field in regions 1 and 2 of Figure 13 is represented by a superposition of
propagating and evanescent spatial harmonics, Figure 14, which are plane waves for
the 2D singly periodic structures. Thus, the total field in regions 1 and 2 of Figure 13,
is,
in the upper region, 1,
z )
z
D / n
inc
z
k ( j x
xn
jk
n
n
z
inc
z
jk x
inc
x
jk inc up
e e e e
2 +
+ R A F (8)
in the lower region, 2,
z )
z
D / n
inc
z
k ( j
x
m
x
jk
n
m
low
e e
2 +
T F (9)
Figure 14
Since the harmonics are solutions of Maxwells equations and hence of the wave
equation, they must satisfy the dispersion relation, i.e.
'
<

2 2
0
2
0
2
2 2
0
2 2
0
for
for
zn
r r r r
zn
zn
r r
zn
r r
xn
k k k k j
k k k k
k

(10)
where
z
inc
z zn
D
n
k k
2
+ (11)
It can therefore be concluded that:
An infinite sum of scattered waves, called harmonics, which are in the form of
plane waves are scattered (transmitted and reflected) from a periodic structure
when a plane wave is incident on the structure.
14
These harmonics are either propagating or evanescent depending on which
inequality holds. The latter depends on the frequency, permittivity and
permeability of the homogeneous medium in which the harmonic propagates and
the period of the periodic structure.
The frequency of onset of propagation of the higher order grating harmonics |n|>1
is given by
zn
r r
k k
0
(12)
Since the angle of the incident incident plane wave is known as well as the
constitutive parameters of all regions, the tangent of the angle of propagation of
each higher order harmonic can calculated from the ratio of k
zn
and k
xn
.
We note that the FSS is designed to operate in the frequency region over which no
higher order harmonic (|n|>1) can propagate.
The work can be extended to doubly periodic FSS structures in three dimensions. An
early analysis by Chen is presented in section 5.
References
[1] F. ONians and J. Matson ''Antenna feed system utilizing polarisation independent
frequency selective intermediate reflector'', US Patent 3,231,892, January 1966.
[2] B.A. Munk, ''Periodic Surface for Large Scan Angles'', US Patent 3,789,404,
January 1974.
[3] G. Marconi and C.S. Franklin, ''Reflector for use in wireless telegraphy and
telephony'', US Patent 1,301,473, April 1919.
[4] E.A. Parker, C. Antonopoulos and N.E. Simpson, ''Microwave Band FSS in
Optically Transparent Conducting Layers: Performance of ring element arrays'',
Microwave and Optical Technology Letters, vol. 16, no. 2, October 1997, pp. 61-63.
[5] J. Hirai and I. Yokota, ''Electro-magnetic shielding glass of frequency selective
surfaces'', Proceedings of the International Symposium on electromagnetic
compatibility, 17-21 May 1999, pp. 314-316.
[6] Nippon Paint world wide web address: www.nipponpaint.co.jp
[7] American Conference of Government Industrial Hygienists (ACGIH), 2000
Threshold Limit Values and Biological Exposure indices, www.acgih.org
[8] W. Gregorwich, ''The design and development of frequency selective surfaces for
phased arrays'', AerospaceConference, 1999, Conference Proceedings IEEE, vol. 5,
pp. 471-479
[9] M.A.A. El-Morsy, E.A. Parker and R.J. Langley, ''Application of Foster network
synthesis to frequency selective design'', International Journal of Electronics, vol. 62,
no. 2, 1987, pp. 193-198.
[10] E.A. Parker and S.M.A. Hamdy, ''Rings as elements for frequency selective
surfaces''. Electronics Letters, vol. 17, no. 17, August 1991, pp. 612-614.
[11] E.A. Parker, S.M.A. Hamdy and R.J. Langley, ''Arrays of concentric rings as
frequency selective surfaces'', Electronics Letters, vol. 17, no. 23,November 1981, pp.
880-881.
15
[12] R. Cahill and E.A. Parker, ''Concentric ring and Jerusalem cross arrays as
frequency selective surfaces for a 45 incidence diplexer''. Electronics Letters, vol. 18,
no. 17, April 1982, pp.313-314.
[13] T.K. Wu., Frequency Selective Surface and Grid Array, John Wiley & Sons Inc.,
1995.
[14]G. Manara., A. Monorchio and R. Mittra, Frequency selective surface design
based on genetic algorithm, Electronics Letters, vol. 35, no.17, 1999, pp. 1400-1401.
[15]S.W. Lee, G. Zarrillo, C.L. Law, Simple formulas for transmission through
periodic metal grids or plates, IEEE Transactions on Antennas and Propagation, vol
30, 1982, pp. 904-909.
[16]F.T. Ulaby, Fundamentals of Applied Electromagnetics, Prentice-Hall, 1999.
Section 2: Description of FSS filter types Frequency Selective Windows
16
Section 2: Description of FSS filter types
FSS filter types
Frequency selective surfaces are filters that can be designed to give the four standard
spectral responses: and stop, band pass, high pass and low pass. Many such designs
can be seen in Appendix 1. Providing that the structure is symmetrical Babinets
principle can be employed to produce from band-stop FSS band pass FSS, from low
pass FSS high pass FSS and vice versa. This means that to transform a high pass filter
into a low pass filter, the conductive and none conductive space are reversed as shown
in the Figure 2.1. Different characteristics are also obtained by cascading and/or
combining individual filters (into composite structures). For example, a band pass
filter could be formed by combining a number of band-stop filters. Hence, filters of
any desirable spectral response can be created. Depending on the design criteria, level
of attenuation, band-stop frequency, bandwidth, sensitivity to electromagnetic wave
incidence angle, the appropriate element is chosen. Typical examples of the four filter
types are outlined below.
Band Stop FSS: This filter has probably been the most widely used. This report
concentrates on this type filter too. It appears in the form of periodic planar arrays of
conductive elements of the following geometries [2]: dipoles, loop circles, loop
squares, loop hexagons, Jerusalem crosses, tripoles etc. A typical structure is shown in
Figure 2.1a.
Band Pass FSS: A typical band pass filter is shown in Figure 2.1b. It is the Babinet
compliment of the band stop filter (Figure 2.1a).
Low Pass FSS: These are typically of the mesh type (Figure 2.1c). They can be
constructed by perforating a conductive sheet.
High Pass FSS: High Pass filters can be the Babinet complement of the low pass
filter. Figure 21.d shows an example of an array of patches which the complement of
the FSS in Figure 2.1c.
These four basic designs may be combined [1] to generate many other novel FSS of
unique characteristics. Despite the many years of FSS research, new designs still
appear and no doubt will continue to do so. As shown in Munk [1] FSS elements are
categorised into four basic groups, these being
(a) (b) (c) (d)
Figure 2.1 The four basic filter types.
17
Group 1 Centre connected or N poles such as dipoles, tripoles and jerusalem
crosses.
Group 2 Looped types, such as circular, square and hexagonal loops.
Group 3 Solid interior or patch types of various shapes.
Group 4 Combinations of any of the above.
Each of these types has been discussed in many papers and technical journals. A
summary of some of the elements that appear in the literature follows:
Group 1: Centre Connected
The most popular members of this group are: (a) the Jerusalem Crosses [3],
[4]; (b) tripoles [5], [6],and [7]. Some of these elements have been combined
with other element types to produce novel single [1] and double layer FSS
configurations [30].
Group 2: Loop Types
This group is probably the most popular, with numerous papers written on
loop squares [12], [13], [14], rings (single and concentric) [8], [9], [10], [11],
[12], [16]. Looped tripoles [1], [5], [15] also fall into this category.
Group 3: Solid Interior Types
These structures usually take the form of apertures (mesh like) and patches.
They can appear in single or multi-layer configurations [18]. Single layer
aperture types are used as dichroic filters [17]. Ring slot FSS have been used
[19] as high pass and band reject filters. Adjustable frequency selective
surfaces using shorted ring slots have recently been published [32].
Group 4: Combinations
Combinations of FSS element types have been employed over the years to
alleviate some of the problems associated with single element FSS. For
example, a slotted square loop and patch structure has been employed in
attempt to overcome the angular sensitivity problems observed in square loop
FSS [20]. Such novel structures have also been used in reducing the radomes
radar cross section (RCS) [21].
Other types of FSS, which do not specifically fall into the sections above, are:
Convoluted FSS (fractal FSS)
There are advantages, particularly in FSS implementations on curved substrates in
reducing the unit cell size [24]. The design of frequency selective surfaces is usually
constricted to that of a flat surface, a distortion in geometry occurs when transferred to
curved surfaces such as those used in radomes. In order to reduce the effect of
substrate curvature, keep the same element geometry throughout the substrate and
maintain the same resonant frequency as in a flat design, the unit cell is reduced in
size.
Convoluted elements, such as those based on the the Hilbert Curve [24], have been
employed. Many novel convoluted element configurations have been developed at
Kent University. Some of these are listed below.
18
Figure 2.2 (a) Convoluted dipole array [22]; (b) tapered cross array [33]. This array
allows a fully interwoven pattern structure improving the packing density. It has an
improved resonant frequency stability as the angle of wave incidence changes; (c)
Crossed Convoluted Dipole.
Experiments on convoluted dipoles have been undertaken at NTU. Figure 2.3 shows a
typical transmitted power response for normal wave incidence.
Figure 2.3 Transmitted power response for normal wave incidence for a
convoluted dipole array.
Convoluted elements belong to the family of fractal elements. The latter have recently
been used to achieve multi-band frequency operation (Sierpinski [26], [27], cross bar
trees [28]).
Spirals
Several logarithmic and linear spiral structures on a square lattice have been
developed at Kent University. Some are shown in Figure 2.5.
(a) (b) (c) (d)
Figure 2.5 (a) Bifilar Spiral; (b) bifilar Spiral with alternate reversed elements; (c)
bifilar Spiral with rotated alternate elements; (d) a quadfilar spiral on a square
lattice.
1 2 3 4 5 6 7 8 9 10
x 10
9
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
m
)
Convoluted Crossed dipoles on square lattice
19
A logarithmic quadrifilar spiral on a triangular lattice has shown to have a very
narrow band response. Figure 2.6 shows one such type of spiral FSS and a typical
transmitted power response at normal wave incidence.
Figure 2.6 A logarithmic quadfilar spiral on a triangular lattice.
A novel linear quadrifilar spiral has also been developed at NTU (Figure 2.7). The
response from this structure is multi-band in nature shown by equally spaced
passbands with stability at all incident angles.
Figure 2.7 Linear quadrifilar spiral.
Finally, the importance of substrate dielectric properties must be emphasised. It was
shown that single and multilayer substrates can be employed to modify the
characteristics of FSS [29]. Hence it is necessary to know accurately the dielectric
properties of the substrate. Section 4 considers this issue.
References
[1] Munk B.A., Frequency Selective Surfaces, Theory and Design, ISBN 0-471-
37047-9, John Wiley & Sons Inc., 2000.
[2] Wu T.K., Frequency Selective Surface and Grid Array, ISBN 0-471-311-8, John
Wiley & Sons Inc., 1995.
[3] Cahill R., Parker E.A., Concentric ring and jerusalem cross arrays as frequency
selective surfaces for a 45 incidence diplexer. Electronic Letters, Vol. 18 No. 8,
April 1982, pp. 313-314.
1 2 3 4 5 6 7 8 9 10
x 10
9
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
it
t
a
n
c
e

(
d
B
m
)
Logarithmic Spirals ona triangular lattice
1 2 3 4 5 6 7 8 9 10
x 10
9
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
it
t
a
n
c
e

(
d
B
m
)
Logarithmic Square Spiral on square lattice
20
[4] Parker E.A., Hamdy S.M.A., Langley R.J., Modes of resonance of the Jerusalem
cross in frequency selective surfaces, IEE Proceedings, Pt. H, Vol. 130, No. 3,
April 1983, pp. 203-208.
[5] Au P.W.B., Musa L.S., Parker E.A., Langley R.J., Paremetric study of tripole
and tripole loop arrays as frequency selective surfaces, IEE Proceedings Pt. H,
Vol. 137, No. 5, October 1990, pp. 263-268.
[6] Mokhtar M.M., Parker E.A., Conjugate gradient computation of the current
distribution on a tripole FSS array element, Electronic Letters, Vol. 26, No. 4,
February 1990, pp. 227-228.
[7] Vardaxoglou J.C., Parker E.A., Performance of two tripole arrays as frequency
selective surfaces, Electronics Letters, Vol. 19, No. 18, September 1983, pp. 709-
710.
[8] Parker E.A., Hamdy S.M.A., Langley R.J., Arrays of concentric rings as a
frequency selective surface, Electronics Letters, Vol. 17, No. 23, November
1981, pp. 880-881.
[9] Parker E.A., Vardaxoglou J.C., Plane wave illumination of concentric ring
frequency selective surfaces", IEE Proceedings Pt. H, Vol. 132, No. 3, June 1985,
pp. 176-180.
[10] Parker E.A., Antonopoulos C., Simpson N.E., Microwave band FSS in optically
transparent conducting layers: Performance of ring element arrays. Microwave
and Optical Technology Letters, Vol. 16, No. 2, October 1997, pp. 61-63.
[11] Huang J, Wu T.K., Lee S.W., Tri-Band frequency selective surface with circular
ring elements, IEEE Transactions on Antennas and propogation, Vol. 42, No. 2,
February 1994, pp. 166-175.
[12] Lee C.K., Langley R.J., Parker E.A., Compound Reflector Antennas, IEE
Proceedings-H, Vol. 139, No. 2, April 1992, pp.135-138.
[13] Cahill R., Parker E.A., Performance of millimetre-wave frequency selective
surfaces in large incident angle quasioptical systems, Electronic Letters, Vol. 28,
No. 8, April 1992., pp. 788-789.
[14] Wu T.K., Four-Band frequency selective surface with double-square-loop patch
elements, IEEE Transactions on Antennas and Propagation, Vol. 42, No. 12,
December 1994, pp. 1659-1663.
[15] Pelton E.L., Munk B.A., A streamlined metallic radome, IEEE Transactions on
Antennas and Propogation, Vol. 22, No. 11, November 1974, pp.799-803.
[16] Wu T.K., Lee S.W., Multi band frequency selective surface with multi ring
elements, IEEE Transactions on Antennas and Propagation, Vol. 42, No. 11,
1994, pp. 1484-1490.
[17] Winnewisser C., Lewen F., Weinzierl J., Helm H., Frequency-selective surfaces
analyzed by THz-time-domain spectroscopy. IEEE Sixth International
Conference on Terahertz Electronics Proceedings. THZ 98, (Cat. No.98EX171).
IEEE 1998, New York, NY, USA, pp.196-198.
[18] Wakabayashi H., Kominami M., Kusaka H., Nakashima H., Numerical
simulations for frequency selective screen with complementary elements, IEE
Proceedings Microwave Antennas and Propagation, Vol. 141, No. 6, December
1994, pp. 477-482.
[19] Kondo A., Design and characteristics of ring slot type FSS, Electronics Letters,
Vol. 27, No. 3, January 1991, pp. 240-241.
[20] Shaker J., Shafai L., Removing the angular sensitivity of FSS structures using
novel double layer structures. IEEE Microwave and Guided Wave Letters, Vol. 5,
No.10, January 1995, pp. 324-325 (Erratum, Vol. 6, No. 1, 1996, p.58).
21
[21] Wahid M., Morris S.B., Metal radomes reduced RCS performance, GEC
Journal of Research, Vol. 9, No. 3, 1992, pp. 166-171.
[22] Parker E.A., El Sheikh A.N.A., Convolted dipole array elements, Electronics
Letters, Vol. 27, No. 4, 1991, pp. 322-323.
[23] Parker E.A., El Sheikh A.N.A., Lima A.C. de C, Convoluted frequency selective
array elements derived from linear and crossed dipoles, IEE Proceedings-H, Vol.
140, No. 5, October 1993, pp. 378-380.
[24] Parker E.A., El Sheikh A.N.A., Convoluted array elements and reduced size
unit cells for frequency selective surfaces, IEE Proceedings-H, Vol. 138, No. 1,
February 1991, pp. 19-22.
[25] Churpin A.D., Parker E.A., Batchelor J.C., Convoluted double square: single
layer fss with close band spacings, Electronics Letters, Vol. 36, No. 22, October
2000, pp. 1830-1831.
[26] Romeu J., Rahmat-Samii Y., Dual band FSS with fractal elements, Electronics
Letters, Vol. 35, No. 9, April 1999, pp. 702-703.
[27] Romeu J., Rahmit-Samii Y., Fractal FSS: A novel dual-band frequency selective
surface, IEEE Transactions on Antennas and Propagation, Vol. 48, No. 7, July
2000, pp. 1097-1105.
[28] Werner D.H., Lee D., Design of dual polarised multiband frequency selective
surfaces using fractal elements, Electronics Letters, Vol. 36, No. 6, March 2000,
pp. 487-488.
[29] Parker E.A., Vardaxoglou J.C., Influence of single and multiple-layer dielectric
substrates on the band spacings available from concentric ring frequency-selective
surface, INT. J. Electronics, Vol. 61, No. 3, 1986, pp. 291-297.
[30] Vardaxoglou J.C., Hossainzadeh A., Stylianou A., Scattering from two-layer
FSS with dissimilar lattice geometries, IEE Proceedings H, Vol. 140, No. 1,
1993, pp. 59-61.
[31] Callaghan P, Parker EA., Experimental investigation of closely packed spiral
element FSS yields narrowband designs, Seventh International Conference on
Antennas and Propagation ICAP 91, London, UK, IEE (Conf. Publ. No.333),
1991, vol. 2, pp.636-639.
[32] Martynyuk A.E., Martinez Lopez J.I., Frequency-selective surfaces based on
shorted ring slots, Electronics Letters, Vol. 37, No. 5, March 2001, pp. 268-269.
[33] Parker E.A., El Sheikh A.N.A., de C Lima A.C., Convoluted frequency selective
array elements derived from linear and crossed dipoles, IEE Proceedings-H, Vol.
140, No. 5, February 1993, pp. 378-380.
Section 3: Investigation of band stop filters at NTU Frequency Selective Windows
22
Section 3: Investigation of band stop filters at NTU
Introduction
In order to obtain a feeling for the performance of band stop elements, several
experiments were undertaken to help assess various FSS structures in order to identify
a suitable one for the FSS box. There are a few parameters to consider in assessing the
FSS performance: (a) the level of attenuation; (b) bandwidth; (c) band-stop frequency
and its insensitivity to angular plane wave incidence; (d) cross-polarisation; (e) optical
transparency. The values of these parameters are affected by various factors: (a) the
thickness and dielectric constant of the substrate; (b) FSS element geometry and
conductivity; (c) inter-element spacing; (d) the presence of more than one FSS layers
(multi-layer FSS structures).
The optical transparency of the FSS, particularly when the conductor is opaque, is
very important. Hence, convoluted elements such as tapered spirals and crossed
dipoles were dismissed due to their close segment packing, and thus poor optical
transparency. In contrast, loop elements, such as squares, circles and hexagons were
preferred. In addition, since there is a need for the presence of many periods, the
dielectric constant of the substrate must be large. Thus, glass was chosen as the
preferred substrate. The results of various investigations follow.
All FSS structures were made by silk screen printing high conductivity ink onto a thin
acetate film, and subsequently placing the acetate on glass substrates.
Experimental procedures and measurement set up
In this section, the procedures used in obtaining the transmission, reflection and cross
polarisation FSS results of this report are outlined.
Equipment
The following microwave measurement equipment was used: An HP 8722D vector
network analyser operating in the range from 50 MHz to 40 GHz, an HP8566B
spectrum analyser operating in the frequency range 100 Hz-22 GHz and an HP8671B
synthesized CW generator operating in the range 2-18 GHz. A Labview programm
was employed to control the spectrum analyser and the microwave signal generator.
The FSS windows were mounted on an FSS test rig. Two different test rigs were used
(figure 1). They both had an aperture window 60 cm60 cm wide. The front side was
fully covered with absorbers. One of them (the largest) was capable of both azimuth
and zenith rotation while the other one (the smaller and more flexible) of zenith
rotation only.
The rigs were positioned inside different rooms at NTU which were not shielded from
enviromental microwave radiation because an anechoic chamber was not available.
Hence, in the results presented the FSS spectral response below 1GHz should be
ignored.
23
Three sets of wideband horn antennas from Qpar Angus Ltd operating between 1.5-
18GHz (Antenna 1), 0.5-2GHz (Antenna 2) and 2-8 GHz (Antenna 3) were employed.
The antennas were mounted onto tripods and were positioned at the height of the
centre of the aperture.
Measurement of the transmitted power
To measure the transmitted power (transmittance) at any angle of incidence a free
space calibration had to be performed (with the rig in place but no FSS) to take into
account the antenna and cable losses. The calibration data were subsequently
subtracted from the measured FSS data.
In a lot of the measurements the transmitting antenna was located at a distance of
177cm from the stand and the receiving one at 87 cm. (see Fig. 2).
Both antennas had the same orientation.
Figure 1: Photos of the test rigs and figures indicating the aperture window rotation.
Small rig
Large rig
Tx Rx
Angle of rotation
Side View
Tx Rx
Angle of rotation
Top View
Zenith Azimuth
24
Cross-polarisation Measurement
The measurement was performed for normal plane wave incidence only. The free
space calibration was performed with the transmitting and receiving antennas having
the same polarisation. The cross-polarisation measurement was done by placing the
FSS in the rig and rotating the receiving antenna by 90
0
.
Measurement of the reflected Power:
During this measurement both antennas were place on the same side w.r.t. to the rigs
position (see figure 3). The calibration was performed by placing a perfectly reflecting
surface at the aperture (here copper was used). In most of the measurements both
antennas were placed at a distance of approximately 177cm from the stand. During
the FSS measurement if both antennas have the same orientation a copolar
measurement is obtained otherwise if they have orthogonal orientations a cross-polar
measurement is made.
Network Analyser
Tx
Absorbing
Material
Absorbing
Material
Rx
45
45
Copper
Plate
Figure 3
177 cm 87cm
Tx
Rx
Absorbing
Material
Absorbing
Material
FSS under
test
Network Analyser
Figure 2
25
Preliminary results relating to FSS measurements:
The cross polarisation performance of the antennas was measured within and outside
their specified frequency range of operation. The aim was to identified which antenna
set to use for cross-polarisation measurements over a given frequency band. The
results are shown in figure 4.
If a screened room is not available to make measurements then the receiving antenna
will measure unwanted background noise. This noise is particularly strong below
1GHz. Figure 5 shows how this noise affects the vector network analyser
measurements. It is a plot of the S
21
level after free space calibration.
In some experiments it is desirable to use a glass sheet of certain thickness. Such a
thickness is achieved by cascading glass sheets of smaller thickness. Figure 6 shows
Figure 5
1 2 3 4 5 6 7 8 9 10
x 10
9
-40
-30
-20
-10
0
10
20
Background Radiation
Frequency
R
e
f
l
e
c
t
a
n
c
e
S
2
1
(Hz)
Figure 4
0 2 4 6 8 10 12 14 16 18
x 10
9
-45
-40
-35
-30
-25
-20
-15
-10
-5
0
5
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B

Blue: Antennas 1 Green: Antennas 3 Red: Antennas 2
C
r
o
s
s

p
o
l
a
r
i
s
a
t
i
o
n

g
a
i
n

(
d
B
)
26
transmission results for (i) a glass sheet of thickness of 4mm and (ii) for a glass of
thickness 4mm that consists of a stack of two sheets of glass of 2mm thickness each.
In case (ii), care has to be taken to ensure there is no air gap between the two sheets.
The effect of an air gap can be seen in Figure 7. The AS FSS (see Appendix, Section
3) is employed. It is sandwiched between two 4mm-thick glass substrates. The FSS
structure is subsequently inserted in the measurement rigs aperture. It is held in place
by locking clips. The latter ensure that the glass substrates are tightly stack together
(minimum air gap). Figure 7 shows that when one locking clip (air gap) and four
locking clips (minimum air gap) are employed different results are obtained.
0 1 2 3 4 5 6 7 8 9 10
x 10
9
-10
-8
-6
-4
-2
0
2
4
6
8
10
Frequency, (GHz)
A
t
t
e
n
u
a
t
i
o
n
,

(
d
B
)

1 x 4mm glass
2 x 2mm glass
Figure 6
Frequency (Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
0 2 4 6 8 10 12
x 10
9
-25
-20
-15
-10
-5
0
5
10
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
Blue: 1 Locking clip (Top Side) Red:4 Locking Clips (One on Each Side)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
Figure 7
27
Finally, calibration is done for every angle of incidence. The calibration cannot
account for diffraction effects hence the position of the antennas is important: far
enough to be in the far field (plane wave measurements) and near enough to avoid
diffraction phenomena due to the finite window aperture. Unfortunately, the
effective aperture gets smaller as the angle of plane wave incidence increase and its
effect on the FSS measurements should be investigated in the future.
Experimental investigations
Dielectric substrate
Two types of lattice are considered, a triangular (figure 1) and a square (figure 2). The
effect of having a single layer glass substrate of thickness 2mm on one side of the
substrate compared to that of two glass substrates (each of 2mm thickness too) with
the FSS sandwiched in the middle, is shown in figure8.
As indicated in the introductory theory on FSS, the structure with glass on one side of
the FSS will exhibit its band-stop behaviour at a higher frequency. This is due to the
fact that the FSS elements are in a sense situated in an effective medium of lower
permittivity than those of the FSS sandwiched between two glass substrates.
Of course a similar effect also appears when, in sandwiched FSS structures, the
thickness of the glass substrate and superstrate increases. Consider again the
sandwiched FSS structure in figure 8 and let the thickness of the glass layers increase
to 4mm and then to 6mm. It can be seen from figure 9 that as the thickness increases
the bandstop frequency decreases. Furthermore, for thick substrates (4mm and 6mm)
the difference in the bandstop frequency is small. This result agrees with those
published in the literature.
Figure 8: Structure A. Glass on one side of FSS
(blue line). Glass sandwiching FSS (red line).
0 5 10 15
x 10
9
-25
-20
-15
-10
-5
0
5
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
Glass on one side
FSS sandwitched
between glass sheets
2mm glass sheets, Structure A
28
Angular Sensitivity
Consider again structure A sandwiched between two 2mm-thick glass sheets. The
antennas (transmitter and receiver) are vertically polarised and the angle of the plane
of the stand changes w.r.t. to the normal (from 0 to 45 in steps of 15). The
transmitted power results are shown in Figure 10, where a variation in the resonance
frequency of the FSS is observed. The variation is not substantial but the common (to
all angles) bandstop region has a reduced attenuation. Therefore care must be taken in
designing FSS structures in cases where the incident wave is a beam or when there is
multipath propagation (as in the case of the FSS box).
0 5 10 15
x 10
9
-20
-15
-10
-5
0
5
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
Blue:0 deg Red:15 deg Green:30 deg Yellow:45 deg
Figure 10:Variation of band-stop frequency
with angle of incidence.
Figures 9: Substrate and superstrate thickness effects
0 5 10 15
x 10
9
-25
-20
-15
-10
-5
0
5
10
Frequency
T
r
a
n
s
m
i
t
a
n
c
e

d
B
2mm glass
4mm glass
6mm glass
(Hz)
29
Lattice type
At normal incidence there is not difference between the bandstop frequency of the
triangular and square lattice ring FSS (see Figure 11).
Lattice spacing
Figures 12 and 13 show that by changing the lattice spacing the FSS band-stop
frequency changes. Structures A and C were considered in the experiments. Both
are triangular lattice FSS structures. In A the spacing between the centres of the
ring elements (situated on the vertices of the equilateral triangle) is 22.24 mm
whereas in structure C the spacing is 22.7 mm.
0 2 4 6 8 10 12 14 16 18
x 10
9
-20
-15
-10
-5
0
5
10
Frequency, (GHz)
A
t
t
e
n
u
a
t
i
o
n
,

(
d
B
)

Triangular Lattice
Square Lattice
Figure 11: Normal plane wave incidence. Square
and Triangular Lattice.
Figure 12: FSS structures sandwiched between two 2mm-thick
glass sheets. Normal plane wave incidence.
0 5 10 15
x 10
9
-25
-20
-15
-10
-5
0
5
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
sp=22.24mm
sp=22.7mm

30
Single/Double Layered
In figure 14 the effect of cascading FSS layers is considered. A square loop element
FSS is chosen, structure AS. The plane wave is normally incident onto the FSS
structure (for both cases). The transmitting and receiving antennas are vertically
polarised. There is an increase in the bandwidth of the bandstop region. For the single
layer FSS (single grid) the elements are sandwiched between two 4mm-thick glass
substrates (symbolised as 4|4). Whereas, for the double grid, the two FSS are
separated by a 4mm-thick glass and on either side of the combination there is also a
4mm-thick glass. The configuration is symbolised as (4|4|4).
0 5 10 15
x 10
9
-25
-20
-15
-10
-5
0
5
10
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
sp=22.24mm
sp=22.7mm
Figure 13: FSS structures sandwiched between two 4mm-
thick glass sheets. Normal plane wave incidence.
Figure 9: Comparison between single and double layer square loop
element FSS.

0 2 4 6 8 10 12
x 10
9
-25
-20
-15
-10
-5
0
5
10
Frequency, (GHz)
Att
en
uat
ion
,
(dB
)
Single Grid
Double Grid
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
Frequency (Hz)
31
Cross Polarisation
The cross polarisation response for a double layer square loop FSS (structure AS) is
shown in figure 15. The plane wave is incident normally. The crosspolarisation result
when compared with that of the antenna (without FSS) shows that there is practically
no FSS cross-polarisation at normal incidence.
Hexagonal loop element FSS: Angular Sensitivity
The sensitivity of the bandstop frequency of the hexagonal loop element FSS for
various incident wave angles is shown for a single layer and a double layer structure
in Figure 16. It can be seen that there is considerable stability in the resonant
frequency.
Hexagonal loop element FSS: Lattice spacing.
The effect of changing the size of the lattice pitch is shown in figure 17. Two
structures are considered: HA and HB. It can be seen that the closer the hexagons are
together, the deeper the attenuation at resonance.
0 2 4 6 8 10 12
x 10
9
-50
-45
-40
-35
-30
-25
-20
-15
-10
-5
0
Frequency, (GHz)
A
t
t
e
n
u
a
t
io
n
,

(
d
B
)

Cross Polarized
TE
Figure 15: Cross polarisation of double layer FSS.
Crosspolarisation
Copolarisation
frequency (Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
frequency (Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
(a) (b)
Figure 16: Single and double layer FSS performance w.r.t. to plane
wave angle of incidence.
32
Conductive Element
The FSS elements were made from conductive silver paint (60% Ag). The finite
conductivity of the paint coupled with the width of the conductive element influence
the resistance of the element. To demonstrate the effect conductivity two FSS were
made consisting of identical elements (squares) and lattice spacings. One was made
out of the silver paint and the other out of copper. It can be seen, in figure 18 that the
material with the highest conductivity (Copper) gives the highest attenuation.
The effect of conductor width is shown in Figure 19. The ring FSS structures A
(width = 0.5mm) and B (width = 1.5mm) are considered. Structure B shows greater
Figure 17: Element Gap
3mm Gap
13 mm Gap
Frequency (Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
)
1 2 3 4 5 6 7 8 9 10 11 12
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
Frequency(Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e

(
d
B
m
)
Silver and Copper square loops
Figure 18: Copper and Silver based FSS.
Copper
Silver
33
attenuation at the resonance frequency and a wider resonant bandwidth than structure
A.
0 5 10 15
x 10
9
-30
-25
-20
-15
-10
-5
0
5
10
15
Frequency Hz
T
r
a
n
s
m
i
t
a
n
c
e

d
B
0.5 mm
1.5mm
Figure 19: Effect of conductor width.
34
Appendix 3A
Structure A: Loop circles (rings) in a triangular lattice.
Element:
Diameter (d): 20.34 mm
Conductor width (cw): 0.5 mm
Triangular lattice (rings on the vertices of an equilateral triangle):
Element gap (g): 1.9 mm
Distance centre to centre (p): 22.24 mm
DC Resistance: 2.4
12 rings
(column)
11 rings
(column)
19 rings (row)
18 rings (row)
434mm
Figure 3A(b)
d
cw
p
g
Figure 3A(b)
35
Appendix 3B
Structure B: Loop circles (rings) in a triangular lattice.
Element:
DC Resistance: 1.72
d
cw
p
g
Figure 3B(b)
12 rings
(column)
11 rings
(column)
19 rings (row)
18 rings (row)
434mm
Figure 3B(b)
36
Appendix 3C
Structure C: Loop circles (rings) in a triangular lattice.
Element:
DC Resistance: 2.4
12 rings
(column)
11 rings
(column)
19 rings (row)
18 rings (row)
434mm
Figure 3C(a)
d
cw
p
g
Figure 3C(b)
37
Appendix 3D
Structure D: Loop circles (rings) in a triangular lattice.
Element:
Element gap (g): 0.0 mm (not electrical contact)
DC Resistance: 1.69
d
cw
p
g
Figure 3D(b)
11 rings
(column)
11 rings
(column)
20 rings (row)
19 rings (row)
434mm
Figure 3D(a)
38
Appendix 3E
Structure K: Loop circles (rings) in a square lattice.
Structure K
Element:
DC Resistance: 2.4
20 rings
(row)
20 rings
(column)
434mm
Figure 3E(a)
d
cw
p
g
Figure 3E(b)
39
Appendix 3F
Structure AS: Loop squares in a square lattice.
Element:
Side length (C): 12.0 mm
Period (p): 15.3 mm
DC Resistance: 2.04
36 squares
(column)
36 squares
(row)
571 mm
Figure 3F(a)
cw
g
p
cw
C
g
Figure 3F(b)
40
Appendix 3G
Structure AH: Hexagonal Loop elements (equilateral lattice)
Structure BH: Hexagonal Loop elements (not equilateral lattice)
Element:
Side length, (C) : 8.3mm
Conductor Width (cw): 1mm
Lattice:
Element Spacing, (a) : 13.2mm
Element Spacing,: 11.9mm
Period (p): 27.2mm
Element:
Side length (C) : 8.3mm
Conductor Width (cw) : 1mm
Lattice:
Element Spacing, (a) : 2.9mm
Element Spacing (g) : 2.9mm
Period (p) : 17 mm
g
C
a
cw
p
g
a
C
cw
p
Figure 3G(a)
Figure 3G(b)
Section 4: Techniques of measuring the dielectric properties of FSS substrates Frequency Selective Windows
41
Section 4: Techniques of measuring the dielectric properties
of FSS substrates
Introduction
Since the substrate dielectric constant affects the FSS performance it is necessary to
be able to evaluate the permittivity of the substrate. In this work, the substrate must be
an optically transparent material. The permittivities of the following materials have
therefore been evaluated: (i) glass; (ii) polycarbonate; (iii) polyester; (iv) thin film
acetate. In addtion, the permittivity of ordinary printed circuit board (PCB) substrate
was measured.
The choice of measurement technique and the required measurement uncertainties
depend on the available dimensions and the shape of the material under test, the
matching tolerances if the material needs to be machined into a specific form, cost,
the microwave frequency range and the anisotropy of the material.
The different measurement methods can be divided into two categories: high-Q
resonance methods for low loss materials and broad band free space/transmission line
methods for medium to high loss materials. In contrast to the broad band methods,
resonance methods are generally limited to single frequencies or to harmonically
related frequencies and they are very accurate. Sometimes, the resonant set up can be
mechanically tuned to different frequencies. On the other hand, transmission line
methods are prone to measurement errors caused by the influence of air gaps,
especially for high permittivity dielectrics.
Resonant methods employ open or closed resonators, cavities and microstrips. They
are used at high frequencies because their size becomes excessively large at
frequencies lower than 100MHz.
The capacitance method does not belong to the above categories. In this method the
material should be lossless and sandwiched between two conducting electrodes. The
capacitance measured across the electrodes can give the permittivity of the material.
Introduction to coaxial probe
Openended coaxial lines are used by many researchers in non-destructive
measurements of the complex permittivity and permeability of materials. These
techniques are especially attractive for in vivo measurements of biological materials
[1]. Open-circuited air-filled coaxial lines are also used as calibration standards for
microwave measurements [2, 3]. The probe is placed in contact with the material
under test and the reflection coefficient is measured at a desired frequency and
temperature. Knowledge of the relationship between the measured reflection
coefficient () (and consequently of the input admittance) and the permittivity () then
allows one to determine the latter. The main problem is that there is not an analytical
relationship between the aperture admittance and the material characteristics. Ideally,
a closed form expression for the permittivity as a function of the reflection coefficient
is required. Some attempts have been made to this end and different models were
proposed. However, the results are based on static or quasi-static approximations and
are valid for restricted frequencies. Initially, the circuit equivalent model was
introduced. The relative permittivity of this model allows a rapid inversion from the
measured reflection coefficient to the dielectric constant. Unfortunately, this model is
42
not accurate in the GHz range due to fringing fields, and at even higher frequencies
due to radiation. Several approximate, but more exact models have been developed,
based on rigorous solutions of the electromagnetic field equations that relate the
permittivity to the reflection coefficient. Although accurate numerical methods exist
for the calculation of for a given , in practice one is interested in the inverse
problem. Only simplified approximate expressions are used to determine the dielectric
properties because of the complexity of the inversion process. Additionally, iterative
procedures are time consuming and yield no information regarding the measurement
uncertainty. In one of the different approaches for quickly relating the reflection
coefficient to the permittivity of the material, nomograms are generated for SR7
coaxial cable at different frequencies [4]. The complex permittivity of the material is
determined from these nomograms for a given reflection coefficient. In the initial
stages of the theoretical analysis of the probe only infinitely thick materials were
considered. Only lately models are developed that take into account finite thickness
materials or even layered materials. As to the materials that have been measured, the
emphasis has always been placed on biological materials like water and human or
animal tissue. Usually, the medium at the end of the coaxial cable is linear, isotropic,
homogenous and non-magnetic with complex permittivity.
Theory and experimental results
Theoretical analysis
The most widely used lumped-element model for the aperture admittance of the probe
is:
5 . 2
0
4
0
) ( ) , (
m m m f
G C j C j Y + +
where is expressed in rad/sec, C
f
is the capacitance inside the coaxial probe due to
evanescent modes close to the aperture, C
0
is the capacitance due to the fringing field
in the material under test, and G
0
is the factor accounting for the radiation loss. A
simple expression of this model, where the two capacitances were assumed to depend
only on the dimensions of the probe while the conductance was neglected,

was first
presented by Stuchly et al [1, 5, 6]. The model was further improved by considering
frequency dependence [7] and nonlinear characteristics [8] of the various parameters.
Brady [9] and Stuchly [10] included the radiation effects by including the factor G
0
for frequencies with wavelengths smaller than the radius of the internal conductor.
Misra developed a quasi-static model by simplifying the equation for the admittance
by a series expansion of the integral equation [11] in order to determine the
parameters.
However, at high frequencies (where (b-)/
m
>2.5 where
m
is the wavelength inside
the material) the lumped model fails due to the effect of the higher order modes at the
aperture. Then, a full wave analysis [4] has to be made to determine the parameters as
was done by Otto and Chew [12].
More elaborate models and expressions were subsequently developed with wider
application to experimental measurements. Misra [13] put forward the model of
Marcuvitz [14] and the formulation of Levine and Papas [15] and approximated by a
series expansion. References [14, 15] do not take higher order modes into
consideration. They only consider the dominant TEM mode propagating in the coaxial
cable. Grant [16] used the full wave analysis of [4] with a Newton-Raphson routine to
43
invert the measured data. Alternatively, Sibbald [17] put forward an interpolation
scheme that combines the accuracy of a full-wave solution with fast computation [18].
The most recent efforts in the modeling of open-ended probes consider the finite
thickness of the material to be measured. Anderson [18] investigated the influence of
the finite thickness of the material under test by a quasi-static analysis. The material
was either backed by a metal plate or by air. In [19] a static approximation is given for
a two-layered medium. It is concluded that the thickness of the material has to be
larger than the outer radius of the probe in order to be able to use the probe as if for an
infinitely thick dielectric medium. Xu [20] used an integral equation considering only
the lowest order mode and measured thin substrates that terminated in free space. He
also measured the conductivity of thin films of ITO deposited on plastic substrates.
He found that the conductivity of ITO at microwave frequencies (0.5-4GHz) is the
same as the one measured with four-probe technique for DC voltages. This result
agrees with the results of Abouzahra [21] who concluded that the resistivity of
different space-cloth materials stays the same for frequencies up to 5.85 GHz.
Reference [22] Li et al obtained a closed form expression of a two-layered material,
and took the higher modes into account for arbitrary parameters of the coaxial cable.
They express the fields in the coaxial line as the addition of the dominant mode and
the azimuthally-symmetric higher order (TM) modes reflected from the medium. The
orthogonality of the radial eigenfunctions of the modes was used to calculate the
expressions for the amplitudes of the higher order modes reflected back into the
coaxial line. Thus, an expression for the input admittance containing a sum of
integrals involving the mode amplitudes is obtained. The summation for the higher
modes converges very rapidly after the first three modes. They were thus able to
measure the thickness of the moisture outer layer of human skin.
A full wave analysis of a stratified finite medium of different permittivity materials
was also examined by Li CL et al [23]. This time an integral equation for the
unknown electric field is derived, and the method of moments is applied to solve the
electric field integral equation. After the aperture electric field is accurately
determined, other quantities of interest such as the input impedance of the probe and
the EM field inside the material can be calculated. This theoretical analysis predicts
the existence of surface waves and radiative waves for the open circuit case i.e. when
the stratified medium is backed by air, and radial guided waves for the short circuit
case i.e. when the stratified medium is backed by a metal plate. The radiated powers
associated with these waves are computed using the Cauchy residue theorem and the
saddle-point method.
The surface waves are the evanescent waves that travel on the surface of the material
that is in contact with the probe aperture. This effect is usually neglected in the
analysis of the flanged open-ended probe. This can be justified in the case of a finite
size material if it is sufficiently lossy so that the surface waves decay sufficiently
before they reach the end of the material edge so when they are reflected back they do
not interfere with the measurement. They also proved that at frequencies lower than 4
GHz the total power carried away by the surface and radiative waves is sufficiently
small that the total field is localized around the probe aperture. This finding justifies
the quasi-static assumptions of the previous researchers in the case where the effects
of surface and radiative waves can be neglected.
Jenkins et al [24] came to the conclusion that only lossy dielectrics can be used in
finite sizes in the probe measurements. They used the method of images to analyze the
experimental results which were taken with a metal plate backing the material under
test. Their technique is not suitable for hard laminar specimens, because it is difficult
44
to avoid the presence of air gaps at the faces of such samples, and for low-loss
materials because of the edge reflections. De Langhe et al [25] presented a closed
form expression for the admittance of the probe on a planar stratified medium backed
by a metal plate. The material of each layer is considered homogenous, nonmagnetic
and isotropic. The model is based on a spectral domain analysis. The advantage of this
method is that the material parameters of each layer (thickness and dielectric constant)
only appear in a kernel function in the integral equation. Changing the parameters of
the material under test only results in changing the kernel. The dimensions of the
probe used in their experiments were bigger than the commercially available
HP85070 that has been used mostly in the previous studies. The reason being that
coaxial probes with small dimensions cannot be used to measure materials with low
dielectric constants (smaller than 5) at low frequencies (smaller than 7 GHz). They
used a custom made bigger probe of 1.74 cm in the diameter of the inner conductor, 4
cm in diameter of the outer conductor extended by 4cm on either side in order to form
the flange. The space between the two conductors was supported by a thin teflon disk
(dielectric constant 2.1). A gradual transition was made from the coaxial line to a N-
type connector to reduce reflections. This transition was designed using finite
difference time-domain methods (FDTD) approach presented in [26]. The new model
can give accuracy within 2% of 1cm sample thickness, while 15% accuracy is
expected for the model of Levine and Papas [15].
Industrial permittivity measurement providers:
During the project some of the industrial permittivity measurement providers have
been identified. These were: Damaskos Inc in USA (damaskos@aol.com), the
National Physical Laboratory (www.npl.co.uk), and the National Institute of
Standards in USA (www.nist.gov). Damaskos Inc is capable of providing free space
measurements of the conductivity of thin film ITO.
In house experimental results using the HP85070C:
At Nottingham Trent University the HP85070C probe was used to estimate the
permittivity of four different materials:
2 mm thick polycarbonate sheet,
2mm thick polyethylene sheet,
4mm thick standard glass pieces 7cm square,
multiple stack of acetate sheets ,
and PCB substrates.
According to the manual of the probe, the measurement procedure requires the use of
isotropic and nonmagnetic semi-solids with smoth flat surface in order for the
permittivity results to be reliable. Liquids can be used as well.The probe consists of a
stand with porcelain base and metallic support that slides up or down on a metallic
arm. A coaxial cable connects the probe to the Network Analyser. A program supplied
by Hewlett Packard must be followed in a step by step fashion in order to complete
the measurements. Three calibration standards are used to calibrate the Network
Analyser: open ended probe, short circuited probe and probe immersed in dionised
water at 25C.
In the course of our investigations we discovered that it requires considerable care in
positioning the probe in perfect contact with the flat, rigid surface of glass in order to
get meaningful results. If there is a thin layer of air between the probe and the
substrate the results are corrupted and the estimated permittivity is lower that the real
45
value of the measured material. The less rigid is the material the easier is to achieve a
perfect contact between its top surface and the probe.
It was observed that depending on the permittivity of the material the substrate had to
consist of a certain thickness of this material. For example 8 mm thick glass was
enough in order to make meaningful measurements. To obtain the necessary thickness
of the material the latter consisted of a stack of layered pieces as it is shown in figure
1. Each substrate piece of a particular material had the same thickness, a length of
6cm and a width of also 6cm.
The effect of thickness of the stack (i.e. number of pieces) and the effect of the
supporting substrate, which is either an absorber or a metal plate, are examined below.
Figure 1. The HP85070C coaxial probe used to measure the permittivity of 12 mm
thick glass.
Permittivity vs frequency results:
Standard Window Glass:
Figure 2.Two pieces of glass rested on piece of absorber.
0 2 4 6 8 10 12 14 16 18 20
6
6.5
7
7.5
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1
-0.5
0
0.5
1
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
46
Figure 3. The same two pieces of glass rested on a piece of metal.
Figure 4. Five pieces of glass were placed on top of an absorber.
0 2 4 6 8 10 12 14 16 18 20
6
6.5
7
7.5
8
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1.5
-1
-0.5
0
0.5
1
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
0 2 4 6 8 10 12 14 16 18 20
6
6.5
7
7.5
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1
-0.5
0
0.5
1
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
47
Figure 5. Five pieces of glass were placed on top of a metal plate.
Figure 6. Two (blue), five (red) and eight (magenta) pieces of glass on top of
absorber.
0 2 4 6 8 10 12 14 16 18 20
6
6.5
7
7.5
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
6
6.5
7
7.5
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1.5
-1
-0.5
0
0.5
1
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
48
Polycarbonate (poly):
Figure 7. Nine pieces of polycarbonate on top of absorber.
Polyester:
Figure 8. Four pieces of polyester on top of absorber. It seems that four pieces are
not enough and considerable power is absorbed by the absorber distorting the results.
0 2 4 6 8 10 12 14 16 18 20
2.7
2.8
2.9
3
3.1
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1.5
-1
-0.5
0
0.5
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
0 2 4 6 8 10 12 14 16 18 20
1.5
2
2.5
3
3.5
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-3
-2
-1
0
1
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
49
Figure 9. Nine pieces of polyester on top of absorber. There is obvious difference with
the permittivity estimation when four pieces of polyester were used. This signifies the
importance of using the adequate thickness of material.
PCB:
Figure 10. Five pieces of PCB on top of absorber. The similarity of the permittivity
graph with those of the above four pieces of polyester shows that that the
measurement is not accurate. This can be attributed to either the form or thickness of
the substrate. The PCB pieces used were deformed and possibly they did not have
good contact to each other.
0 2 4 6 8 10 12 14 16 18 20
2.8
2.9
3
3.1
3.2
3.3
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1.5
-1
-0.5
0
0.5
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
0 2 4 6 8 10 12 14 16 18 20
2
3
4
5
6
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-10
-5
0
5
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
50
Figure 11. Six pieces of PCB substrate on top of absorber.
Acetate:
Figure 12. Thin sheets of acetates were packed together to form a substrate of
thickens of about 8mm.
0 2 4 6 8 10 12 14 16 18 20
3
3.2
3.4
3.6
3.8
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-1.5
-1
-0.5
0
0.5
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
0 2 4 6 8 10 12 14 16 18 20
2.7
2.8
2.9
3
3.1
3.2
R
e
a
l
(
r
)
Frequency (GHz)
0 2 4 6 8 10 12 14 16 18 20
-0.6
-0.4
-0.2
0
0.2
0.4
Frequency (GHz)
I
m
a
g
i
n
a
r
y
(
r
)
51
In conclusion, when the material reached a certain thickness the permittivity
measurements did not depend on the type of substrate support (i.e. absorber or metal).
However, there is some error in calculating the imaginary part of the relative
permittivity of the materials (values opposite signs exist).
The free space measurement method
Throughout the free space measurements, two identical broadband horn antennas were
employed. The top and front views of the experimental set up are shown in Figures 13
and 14(a). The antennas are placed at an appropriate height to avoid ground
reflections. The angular incidence measurements are done as shown in Figure 14(b).
Figure 13. Diagram to show position of absorbers in experiments (top view).
Figure 14(a). Diagram of structure to hold device under test (front view).
Surrounding
pyramidal
absorbers
Window to hold the
device under test
h
Receiving
antenna
Material under test
Transmitting
antenna
Pyramidal
absorbers
Stand to hold
the absorbers
and dielectric
material
52
Figure 14(b). Experimental setup at Oblique incidence.
The measurements are done using an HP8722D Vector Network Analyser. A
calibration is performed the is identical to that of the transmission and reflection
measurements of Frequency Selective Surfaces.
Using the standard plane wave reflection and transmission equations through a
dielectric slab the permittivity is obtained by matching the experimental with the
theoretical results. The latter is done with the aid of a Matlab programme. Only a
single permittivity value is obtained and thus may be considered as an average one
over the frequency range of measurements. From the probe results we note that the
real part of the relative permittivity does not vary significantly from 1.5GHz to 6GHz.
Only the real part of the relative permittivity is obtained (the glass is assumed to be
lossless).
For the standard window glass (substrate of FSS) a number experiments results were
performed by varying the angle of plane wave incidence and the thickness of the
material under test. Figure 15 shows theoretical and experimental results for normal
plane wave incidence. By matching the experimental with the theoretical results an
average permittivity value of
glass
=6.633. for a 12mm thick window. From the
measurements at other angles and thicknesses (a TM plane wave incidence was
considered) the relative permittivity results varied as 6.550<
glass
<6.650.
Measurements of reflected power at various angles of TM polarised plane wave
incidence were also done (see Figure 16). An average permittivity of 6.23 was
obtained. These values compare well with the coaxial probe permittivity
measurements shown in Figures 2-6 where an average permittivity of approximately
7.3 was obtained over the same frequency range (1.5-6GHz.)
Angle of
incidence
h
53
Figure 15. Plot of Transmitted power against frequency for a 1 2mm thick glass at
normal plan wave incidence.
Figure 16 A plot of Reflected power against frequency for a 12 mm glass and TE
polarisation at 15 degress.
Similar measurements for the polycarbonate material indicated an average relative
permittivity of around 2.6 (2.1<
polycarbonate
<2.92). This value also compares well with
the average value of 3 obtained by the coaxial probe method (see Figure 7).
REFERENCES
[1] T.W. Athey, M.A.Stuchly et al, Measurement of radio frequency permittivity of
biological tissues with open-ended coaxial line: Part 1, IEEE TRANS.
MICROWAVE THEORY TECH.,1982, vol 30, pp. 82-86
[2] B. Bianco, A. Corana et al, Open-circuited coaxial lines as standards for
microwave measurements, ELECTRON. LETT., 1980, vol 16, pp.373-474
[3] J. Dibeneditto, A. Uhlir, Frequency dependence of 50- coaxial open-circuit
reflection standard, IEEE TRANS. INSTRUM. MEAS., 1981, vol 30, pp. 228-
229
1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-7
-6
-5
-4
-3
-2
-1
0
1
Transmittance against frequency(at normal incidence)
Frequency(Hz)
T
r
a
n
s
m
i
t
t
a
n
c
e
(
d
B
)
0 1 2 3 4 5 6
x 10
9
-50
-40
-30
-20
-10
0
10
Reflectance against frequency(angle of incidence=15 degrees)
Frequency(Hz)
R
e
f
l
e
c
t
a
n
c
e
(
d
B
)
54
[4] J.R. Mosig, J.C.E. Besson et al, Reflection of an open-ended coaxial line and
application to non-destructive measurement of materials, IEEE TRANS.
INSTRUM. MEAS., 1981, vol 30, pp. 46-51
[5] M.A. Stuchly, S.S. Stuchly, coaxial line reflection methods for measuring
dielectric properties of biological substances at radio and microwave frequencies-
A review, IEEE TRANS. INSTRUM. MEAS., 1980, vol 29, pp. 176-183
[6] G. Gajda, S. Stuchly, Numerical analysis of open-ended coaxial lines, IEEE
TRANS. MICROWAVE THEORY TECH., 1983, vol 31, pp. 380-384
[7] A. Kraszewski, S. Stuchly, Capacitance of an open-ended coaxial line-
Experimental Results, IEEE TRANS. INSTRUM. MEAS., 1983, vol 32, pp. 517-
519
[8] G. Gajda, S. Stuchly, An equivalent circuit of an open-ended coaxial line, IEEE
TRANS. INSTRUM. MEAS., 1983, vol 32, pp. 506
[9] M. Brady, M. Symons et al, Dielectric behavior of selected animal tissues in vitro
at frequencies from 2 to 4 GHz, IEEE TRANS. BIOMED. ENG., 1981, vol 28,
pp. 305-307
[10] M. Stuchly, M. Brady et al, Equivqlent circuit of an open-ended coaxial line in a
lossy dielectric, IEEE TRANS. INSTRUM. MEAS., 1982, vol 31, pp. 116-119
[11] D.K. Misra, A quasi-static analysis of open-ended coaxial line, IEEE TRANS.
MICROWAVE THEORY TECH., 1987, vol 35, pp. 925-928
[12] G. Otto, W. Chew, Improved calibration of a large open-ended coaxial probe for
dielectric measurements, IEEE TRANS. INSTRUM. MEAS., 1991, vol 40, pp.
742-746
[13] D.K. Misra, M. Chabbra et al, noninvasive electrical characterization of materials
st microwave frequencies using an open-ended coaxial line: Test of an improved
calibration technique, IEEE TRANS. MICROWAVE THEORY TECH., 1990,
vol 38, pp. 8-14
[14] N. Marcuvitz, Wavequide Handbook, New York: McGrawhill, 1951, p 213-216
[15] H.R. Levine, C.H. Papas, Theory of circular diffraction antenna, J. APPL.
PHYS., 1951, vol 22, pp. 29-34
[16] J. Grant, R. Clarke et al, A critical study of the open-ended coaxial line sensor for
medical and industrial dielectric measurements, J. PHYS. E: SCI. INSTRUM.,
1989, vol 22, pp. 757-770
[17] C. Sibbald, S. Stuchly, A new aperture admittance model for open-ended
wavequides, IEEE TRANS. MTT-S SYMP. DIG., 1992, pp. 1549-1552
[18] L. Anderson, G. Gajda et al, Analysis of an open-ended coaxial line terminated
by layered media, IEEE TRANS. INSTRUM. MEAS., 1986, vol 35, pp. 13-18
[19] S. Fan, K. Staebel et al, Static analysis of an open-ended coaxial line terminated
by layered media, IEEE TRANS. INSTRUM. MEAS., 1990, vol 39, pp. 435-437
[20] Y. Xu, R. Bosisio, Nondestructive measurements for the resistivity of thin
conductive films and the dielectric constant of thin substrates using an open-
ended coaxial line, IEE PROC. H, 1992, vol 139, pp. 500-506
[21] M.D. Abouzahra, Automated wide-band surface resistivity measurements of
resistive sheets, IEEE TRANS. INSTRUM. MEAS., 1987, vol 36, pp. 1031
[22] L. Li, L. Ismail et al, Flanged coaxial microwave probes for measuring thin
moisture levels, IEEE TRANS. BIOMED. ENG., 1992, vol 39, pp. 49-57
[23] C.L. Li, K.M. Chen, Determination of electromagnetic properties of materials
using flanged open-eneded coaxial probe: Full-wave analyis, IEEE TRANS.
INSTR. MEAS., 1995, vol 44, pp. 19-27
55
[24] S. Jenkins, A.G.P. Warham et al, Use of open-ended coaxial line sensor with a
laminar or liquid dielectric backed by a conducting plane, IEE PROC H, 1992,
vol 139, pp. 179-182
[25] De Langhe, K. Blomme et al, Measurement of low permittivity materials based
on a spectral domain analysis for the open-ended coaxial probe, IEEE TRANS.
INSTRUM. MEAS., 1993, vol 42, pp. 879
[26] J. Van Hesse, D. De Zutter, Modeling of discontinuities in general coaxial
waveguide structures by the FDTD-method, IEEE TRANS. MICROWAVE
THEORY TECH., 1988, vol 36, pp. 875-881
Section 5: Numerical Techniques Frequency Selective Windows
56
Section 5 Numerical Techniques
Introduction
Fully vectorial numerical methods such as the method of moments (mode matching
method, spectral domain method), the finite element method and the finite difference
time domain method are essential in order to accurately model and design frequency
selective surfaces. They are however computationally expensive. The equivalent circuit
method is a less accurate technique but requires very limited computational resources.
The equivalent circuit expressions are analytic and allow an insight into the FSS
performance.
Equivalent circuit method
The method represents the frequency selective surface by an equivalent circuit. The
free space is represented by a 377 transmission line and transmission line equations
are solved to obtain the power reflected and transmitted from the FSS.
The equivalent circuit method is a scalar technique and hence it cannot model the
cross-polarisation of the FSS. Equivalent circuit simulations account for the angle of
incidence and the substrate permittivity.
The standard equivalent circuit technique is an emperical extention of the equivalent
circuit modelling equations of parallel strips developed by Marcuvitz [1] and Wait [2].
For example, for a frequency selective surface of square loops, assuming a plane wave
incidence in either the E or H plane [3], the equivalent circuit consists of a series LC
resonant circuit.
The values of L and C can be found from a modification of the strip array formulae
developed by Marcuvitz. The strip array is shown in Figure 1.
Figure 1
When the incident electric field is polarised parallel to the strips (F = E) the array
behaves as a shunt inductive reactance with a value given by [1],
1
1
]
1
,
_
,
_
) , , , (
2
cos ln
cos
) , , (
0
w p G
p
w
ec
p
w p F
Z
X
(1)
where is the free space wavelength, w is the width of the conductive strips, is the
angle of incidence and G(p,w, ) is a correction term
Front View
F
Side View
w g p
F
57
+ +
+ +
+ +
,
_
+ +
,
_
1
1
]
1
+ +
,
_

1 1
6
1 1
4 2
2
2
1 1
2
1 1
2
2 2
2 ) (
8 2
1
4
1
4 ) (
4
1 ) 1 ( 5 . 0
) , , , (
A A A A
A A A A
w p G (2)
1
1
sin
1
2
2
2
1

,
_
t
p p
A (3)
and = sin(0.5w/p).
Similarly, for the magnetic field vector polarised parallel to the conductive strips (F =
H), the strip array behaves as a shunt capacitive susceptance with a value given by [1],
) , , ( 4
) (
0
g p F
Z
g B
(4)
where g is the width of the gaps between the conductive strips.
For the square loop array, in Figure 2, the reactance X
L
is
) , 2 , (
0
s p F
p
d
L
Z
X
L
(5)
Figure 2
where the reactance is reduced by a factor d/p since the strip is not continuous but
consists of a series of finite strips (square loop sides) of length d. It is logical to assume
that for g<<p the width of the finite strips is w=2s.
The susceptance B
C
of the capacitance is given by
) , , ( 4
0
g p F
p
d
C
Z
B
C
(6)
s
d
p
g
L
Z
0
=1 Z
0
=1
Z
in
C
58
where g is the gap between the loop sides. Again the impedance is reduced by a factor
d/p from the value corresponding to the array of infinite strips.
From electrostatics, the presence of a thin dielectric substrate affects the capacitance
and not the inductance. Hence one can assume that the presence of a thin dielectric
substrate will affect the value of B
C
only. In the equivalent circuit method, this is
accounted for as follows
) , , ( 4
0
g p F
p
d
C
Z
B
eff
C
(7)
where
eff
is an effective dielectric constant which is related to the relative permittivity
of the substrate. The value of
eff
cannot be greater than the relative permittivity and is
calculated by matching the experimental with the predicted results.
Hence the equivalent impedance of the square loop array is given by
,
_

c
L sc
B
X j Z
1
(8)
For the normalised impedance transmission line circuit in Figure 2, the input
impedance is given by
sc
sc
sc in
Z
Z
Z Z
+

1
|| 1 (9)
The corresponding reflection coefficient R is
1
1
+
in
in
Z
Z
r (10)
and the grid power transmission is therefore
2
| | 1 r T (11)
The equivalent circuit formulations are valid for [1]
1 / ) sin 1 ( < + p (12)
and the accuracy of these approximate formulae increases as w<<p, g<<p and p<<.
In Figure 3, equivalent circuit and experimental results are compared for a frequency
selective surface of square loops (Figure 2). For this array, p = 13.6 mm, d = 10.6 mm,
s = 1.2 mm and g = 3 mm. The FSS elements were made of very thin silver paint of
finite conductivity. The substrate was an acetate film of relative permittivity
r
=3.1 and
of thickness 0.4mm (thicker than the silver paint). For an e
ff
=1.8 there is a good
agreement between the equivalent circuit and the experimental results. If we assume
that the FSS elements are completely immersed in a medium of relative permittivity
r
=
eff
then the rule of thumb suggest that the expected FSS band-stop frequency will
59
occur at 5.9GHz. At least for these particular FSS structures, the rule of thumb fails to
predict the band-stop frequency [3].
Using a similar approach to the one described above, equivalent circuits can be
identified for other FSS elements such as gridded squares (Figure 4) [4,6], double
squares (Figure 5) [4,5,7], gridded double squares (Figure 6) [7], Jerusalem crosses
[8,9] and gridded Jerusalem cross [10,11]. Reference [10] contains also a summary of
equivalent circuits of periodic structure filters and their qualitative frequency
responses.
1 2 3 4 5 6 7 8 9 10
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
frequency (Hz)
t
r
a
n
s
m
i
t
t
e
d

p
o
w
e
r

(
d
B
)
Figure 3
Figure 4: Gridded squares
L
2
L
1
C
1
Figure 5: Double square
L
2
L
1
C
1
C
2
60
Alternative formulations also exist that attempt to account also for the presence of a
dielectric [12]. Furthermore, the accuracy of the equivalent circuit models can be
improved by adopting a multimode network description in which an arbitrary number
of higher modes can be included, with different dielectric media on each side of the
surface [13].
The equivalent circuit method rapidly provides an overview of the performance of a
frequency selective structure as various of its geometrical parameters are modified
such as the gap between elements, the width of the conductors and the period.
Furthermore, the transmission line representation of the FSS can easily be modified to
allow for multilayer FSS designs.
With modern computer power, the advantage of speed of the equivalent circuit method
has diminished and more computationally demanding, but also more accurate,
techniques, such as the method of moments, are widely used instead.
Method of Moments
There are many variations of the application of the method of moments in the solution
of frequency selective surfaces. The approach presented by Chen [14] is outlined
below which is one of the earliest reported in the literature. Reference to the work of
other authors is subsequently listed.
According to Chen, the electromagnetic field distribution near the array of conducting
elements is expanded into a set of Floquet spatial harmonics also known as Floquet
mode functions. By requiring the total electric field to vanish on the conducting FSS
elements, an integral equation for the unknown current is obtained. The integral
equation is solved by expressing the current in terms of a complete set of properly
chosen orthonormal, over the element, mode functions. The coefficients of these mode
functions are then determined using the method of moments. The accuracy of the
method depends on the number of modes employed in the computation. As the number
of modes is equal to the order of the final matrix to be solved, the larger the number the
greater are the computer time and memory requirements.
Consider the periodic array in Figure 7. The conducting elements are periodically
arranged along the skew u(=x) and v axes. The angle between the two axes is . In the
figure, is the angle between the propagation vector k and the normal to the FSS
known as zenith angle. The azimuth angle is the angle between the x-axis and the
projection of k to the x-y plane. All the elements in the array are assumed to be
L
2
L
1
L
2
C
2
C
1
Figure 6: Gridded double squares
61
perfectly conducting, identical and infinitecimally thin. In addition, since the field is
periodic, i.e. it satisfies the periodicity requirements imposed by Floquets theorem, its
tangential component to the x-y plane can be expanded into transverse electric (TE)
and transverse magnetic (TM) Floquet spatial harmonics.
(a) (b)
Figure 7 Plane wave incidence on a periodic structure with non-orthogonal axes of
periodicity: (a) top view; (b) side view.
For the tangential electric field,
t
E , the TE and TM Floquet modes are
( )
TE for
mn
y x tmn
xm yn
e
mn
R
D D k
k k j i
E

(1)
( )
TM for
mn
y x tmn
yn xm
h
mn
R
D D k
k k j i
E
+
(2)
2 2 2
yn xm tmn
k k k + (3)
2 2
0
2
tmn r r zmn
k k k (4)
) z jk exp( ) y jk exp( ) x jk exp( R
zmn ymn xm mn
(5)
where m,n indicate the order of the Floquet harmonic and
0 0
2 2
0
k . The signs in
equation (5) are modified appropriately to allow for propagation along the positive or
negative Cartesian axis direction. The modal propagation constant
zmn
k must be
positive for propagating harmonics and negative imaginary for evanescent harmonics
2 2
0 tmn r r zmn
k k k for
2 2
0 tmn r r
k k > (6)
Plane wave projection
on u-v plane

x, u
v
y
D
x
D
y
z
x, u
incident plane
wave
62
2 2
0 tmn r r zmn
k k j k for
2 2
0 tmn r r
k k < (7)
Furthermore,
x
inc
x xm
D
m
k k

+
2
(8)
+ cot
D
m
D
n
k k
x y
inc
y ymn
2 2
(9)
where D
x
and D
y
are given by,
u x
D D (10)
sin
v y
D D (11)
In addition,
inc
y
inc
x
k , k are the propagation constants of the incident plane wave along the
axes of periodicity,
cos sin
0 r r
inc
x
k k (12)
sin sin
0 r r
inc
y
k k (13)
Where
r
,
r
represent the relative permittivity and permeability respectively of the
medium in which the FSS elements are situated. In the case of Chen the medium was
free space
r
=
r
= 1.
The transverse electric and magnetic fields are related by the modal impedances,
mn z
r TE
mn
k
h

0
(14)
r
mn z
TM
mn
k
h

0
(15)
Thus, the tangential field of the incident plane wave can be decomposed into TE and
TM harmonics of order m = n = 0,
2
1
00 00
r
r r
i
t
A
E
E (16)
( )

2
1
00
00
00
r
r
r
r i
t
h
A
E
k H (17)
where k is the unit vector in the positive z-direction and A
00r
is a measure of the
magnitude of the incident plane wave. The subscript r = 1 or 2 indicates the TE and
TM Floquet harmonics respectively.
The tangential reflected field is also expressed in terms of Floquet harmonics,
63

+

+

2
1 r
r mn r mn
n m
R
t
Q
E
E (18)
( )

+

+

2
1 r
r mn
r mn
r mn
n m
R
t
h
Q
E
k H (19)
From the orthonormality property of the Floquet harmonics one may obtain the
reflection coefficients of each of the propagating and evanescent harmonics as follows,

element
conductive
*
r mn
R
t r mn mnr
dS h Q
E
H k (20)
where indicates the complex conjugate of.
Chen subsequently specifies the following boundary conditions on the conducting
plates
0 E E +
R
t
i
t
over each plate (21)
( ) K H H k +
R
t
i
t
2 over each plate (22)
K being the surface electric current.
By inserting equations (16), (18) and (20) in (21) the following equation is obtained,
+

+

element
conductive
*
r mn
R
t
r
r mn r mn
n m r
r r
dS h A
E E E
H k
2
1
2
1
00 00
(23)
To solve equation (23), Chen expressed the induced current
R
t
H k in terms of
another set of modal functions,
l pq
, which are appropriate for the conductive FSS
element under consideration and satisfies the elements boundary conditions. These
modal functions are also orthonormal and provide a faster convergence than the
Floquet harmonic expression in equation (19). The subscripts p,q indicate the mode
order and the subscript l indicates the polarisation type TE or TM ( l= 1 or 2
respectively). Thus,

2
1 0 0 l
l mn l pq
q p
R
t
B H k (24)
In order to eliminate the magnetic field in equation (16) and obtain the matrix equation
to be solved, both sides of equation (16) are multiplied by the complex conjugate of
64
L PQ
. Both sides of the subsequent equation are integrated over the FSS element area
S. The following equation is therefore obtained,
+

+

element
conductive
*
r mn
R
t
r
PQL *
mnr r mn
n m r
PQL *
r r
dS C h C A
E
H k
2
1
2
1
00 00
(25)
where

element
conductive
*
r mn L PQ
PQL
mnr
dS C
E
(26)
From equation (25) a matrix equation can be set up with the mode coefficients B
mnl
as
the unknowns,
] [ ] ][ [
PQL pql
pql
PQL
D B Z (27)
where ] [
pql
PQL
Z is a square impedance matrix. Its row index is designated by P,Q,L, and
the column index is designated by p,q,l. The matrix elements are
pql
mnr
r
PQL *
mnr r mn
n m
pql
PQL
C C h Z

+

+

2
1
(28)
and
2
1
*
00 00
r
PQL
r r PQL
C A D (29)
Hence, by solving the matrix, the unknowns B
mnl
and subsequently the reflected
Floquet harmonics amplitudes and power can be obtained.
Chen also suggests that the functions
l
pq
, which are also known as entire domain
basis functions [17], are the dual functions for the transverse electric field functions for
the equivalent waveguide problem. He provides an example of a set of functions for
the rectangular patch based on the rectangular waveguide modal functions.
The work of Chen was subsequently extended to allow for the calculation of
transmitted fields. Montgomery [15] showed how a dielectric substrate can be
incorporated in the calculations. He also indicated that the coupling coefficients C in
Chens work can be evaluated in closed form. Entire domain basis functions for other
conducting elements are presented by Mittra, Chan and Cwik [17]. Subsectional
(subdomain basis) current functions were subsequently introduced. The advantage, as
Rubin and Bertoni [16] indicate, is the ability to model conductive elements (or
apertures) of arbitrary shape. The price paid is an increase in matrix size [17] with
consequent increase in computer memory and time requirements. The memory
requirements can be minimised by using iterative methods of matrix solution
(conjugate gradient method) [17]. A summary of techniques for analysing frequency
selective structures was published by Mittra, Chan and Cwik [17]. The spectral domain
method is also considered in Wu [18], Scott [19] and Vardaxoglou [20]. An alternative
approach to solution of FSS is presented by Munk [21].
65
References
[1] N. Marcuvitz, Waveguide Handbook, McGraw Hill, 1951.
[2] J.R. Wait, Reflection at arbitrary incidence from a parallel wire grid, Applied Sci.
Res., 1954, vol. 4, pp. 393-400.
[3] R.J. Langley and E.A. Parker, Equivalent circuit model for arrays of square
loops, Electronics Letters, vol. 18, no. 7, 1982, pp. 294-296.
[4] C.K. Lee, R.J. Langley, Equivalent-circuit models for frequency-selective surfaces
at oblique angles of incidence, IEE Proceedings Pt. H, vol. 132, no. 6, 1985, pp. 395-
399.
[5] R.J. Langley and E.A. Parker, Double-square frequency-selective surfaces and
their equivalent circuit, Electronics Letters, vol. 19, no. 17, 1983, pp. 675-677.
[6] C.K. Lee and R.J. Langley, Design of single layer frequency-selective surface,
International Journal of Electronics, vol. 63, no. 3, 1987, pp. 291-296.
[7] R.J. Langley and C.K. Lee, Design of single-layer frequency selective surfaces for
multiband reflector antennas, Electromagnetics, vol. 5, no. 4, 1985, pp. 331-347.
[8] I. Andersen, On the theory of self-resonant grids, The Bell System Technical
Journal, vol. 54, no. 10, 1975, pp. 1725-1731.
[9] R.J. Langley and A.J. Drinkwater, Improved empirical model for the Jerusalem
cross, IEE Proceedings Part H, vol. 129, no. 1, 1982, pp. 1-6.
[10] J.A. Arnaud and J.T. Ruscio, Resonant-grid quasioptical diplexer, Electronics
Letters, vol. 9, no. 25, 1973, pp. 589-590.
[11] J.A. Arnaud and F.A. Pelow, Resonant-grid quasi-optical diplexers, The Bell
System Technical Journal, vol. 54, no. 2, 1975, pp. 263-283.
[12] S.W. Lee, G. Zarrillo, C.L. Law, Simple formulas for transmission through
periodic metal grids or plates, IEEE Transactions on Antennas and Propagation, vol.
30, no. 5, 1982, pp. 904-909.
[13] A.N.A. El-Sheikh and R.J. Langley, Multiport network analaysis f frequency-
selective surfaces, IEE Proceedings on Microwave Antennas and Propagation, vol.
141, no. 3, 1994, pp. 229-231.
[14] C.C. Chen, Scattering by a two-dimensional periodic array of conducting plates,
IEEE Transactions on Antennas and Propagation, vol. 18, no.5, 1970, pp. 660-665.
[15] J.P Montgomery, Scattering by an infinite periodic array of thin conductors on a
dielectric sheet, vol. 23, no. 1, 1975, pp. 70-75.
[16] B.J. Rubin and H.L Bertoni, Reflection from a periodically perforated plane
using a subsectional current approximation, IEEE Transactions on Antennas and
Propagation, vol. 31, no. 6, 1983, pp. 829-836.
[17] R. Mittra, C.H. Chan and T. Cwik, Techniques for analyzing frequency selective
surfaces a review, Proceedings of the IEEE, vol. 76, no. 12, 1988, pp. 1593-1614.
[18] T.K. Wu, Frequency selective surface and grid array, Wiley, 1995.
[19] C. Scot, The spectral domain method, Artech House, 1989.
[20] J.C. Vardaxoglou, Frequency Selective Surfaces Analysis and Design, RSP,
1997.
[21] B.A. Munk, Frequency Selective Surfaces - Theory andDesign, Wiley, 2000.
Section 6: Conductive Paints and Opaque FSS fabrication Frequency Selective Windows
66
Section 6: Opaque Conductor FSS.
Conductive paints
Conductive paints come under the term thick film laminates and are composed of a
medium such as resin or more recently water, with a pigment of metallic particles.
They have many properties such as particle size and shape, amorphous structure,
porosity, layout properties in medium vehicles, percentage of conducting material
loading, particle compaction and dispersion additives. All these properties have an
effect on its electrical properties.
The electron flow from one pigment particle to another within the paint is determined
by such properties as the resistance of the particle pigment, the construction of
particle chains within the holding medium and the inter particle gaps that form after
applying the coating.
Typical conductive additives are made from solid spherical glass beads coated with
silver between 10 and 100 microns in size. The amount of silver coating can also be
adjusted, typically between 4% and 33% by weight. Other metals such as copper and
aluminum are used as well as different pigment shapes such as flakes and powders.
These conductive pigments are used in a wealth of EMI/RFI shield products including
adhesives and sealants.
The effects of paint conductivity are determined by the degree of pigment loading
within the medium, how compact the pigment particles are within the medium, the
uniformity of particle size and particle to particles contact. The typical pigment
loading levels for conductive paint are above 65%, below this conduction will not
occur and above this there is no great improvement although at higher levels the
application can be thinner. Manufacturing processes are not the only parameters that
affect conductivity, environmental conditions such as heat and humidity stability,
oxidation of the metallic particles and general wear and tear can also be important.
Substantial progress has been made in the last few years in developing resin systems,
which are not only mechanically compatible with the substrate materials, but which
also exhibit vastly improved shielding characteristics. It was not long ago that the
prime complaint against makers of paint coatings was that the slightest abrasion or
flexing of a plastic substrate resulted in conductive coating flaking off.
Twenty years ago conductive paints consisted mainly of nickel as the pigment, and
were dispensed by spray or brush. With the introduction EMI/RFI regulations
considerable interest has evolved in using other metal pigments and modern dispersal
techniques. This technology is evolving rapidly and with current developments the
conductivity at lower applied thickness has continued to improve. Consequently the
cost of coatings has continually reduced in cost.
With this increase in usage, the price of silver loaded paints has fallen significantly in
recent years and many products such as mobile phones are shielded using this
product. Hybrid blends such as silvered copper pigments will offer the high
conductivity of traditional silvered paints at lower thickness. New technologies are
likely to produce water-based products that will reduce the hazardous materials that
are currently used in thinners and screen wash products. Development of short steel
67
fibre paints will produce comparable conductive products without the use of precious
metals and will consequently reduce cost.
Three main metals are used in conductive coatings, with each one having a different
performance characteristic (Table 1). Silver is a highly conductive metal imparting
excellent corrosion resistance. While cost is high, EMI/RFI shielding attenuation can
range between 50-75dB at most frequencies and surface resistivity comes down to
0.01 ohms/ . Silver coatings are frequently specified for military applications where
electromagnetic pulse protection (EMP) is required. For example, a 0.030mm dry film
thickness of silver will provide the same or better protection than a 0.225mm dry film
thickness of copper coating.
Copper has nearly the same electrical conductivity as silver, but at a lower cost. Only
recently has it been possible to provide a stable copper-based paint, by providing a
special treatment to the copper flake filler to overcome its oxidation. Current
conductive acrylic paints consist of a water-based acrylic/urethane polymer and a
silver plated copper filler. These offer electrical conductivity of 20 to 30 m/ at a
thickness of 50 microns. They also offer high levels of abrasion and environmental
resistance.
Nickel has also been the subject of recent development work. Although not quite as
good a conductor as copper or silver, it absorbs more electromagnetic radiation on
account of its magnetic permeability. The majority of nickel coated systems are air-
drying and are applied with conventional spray equipment at a dry film thickness of
between 0.025mm and 0.05mm. This will yield greater than 40dB across a frequency
range of between 5 MHz and 1.8 GHz and a surface resistivity of less than 10 ohms/ .
Nickel conductive paints offer a most economic shielding for the majority of plastics.
There is little or no surface preparation requirement and the spray application allows
for high-speed production, resulting in low labour costs. Enclosures and cabinets with
complex geometries can be coated without fear of incomplete coverage.
The main nickel systems for use on plastics are based on acrylic or polyurethane. One
factor in the selection of the paint is the degree to which it can chemically attack and
permanently bond itself to the substrate, such that it cannot be readily abraded.
Silver 1.05 Nickel 0.20
Copper 1.00 Iron 0.17
Gold 0.70 Tin 0.15
Aluminum 0.61 Steel 0.10
Magnesium 0.38 Lead 0.08
Zinc 0.29 Stainless Steel 0.02
Brass 0.26
Table 1. Relative conductivity of metals
Improvements in wear and abrasion properties have made silkscreen printing of
conductive paints popular today in the manufacture of car windscreen de-foggers and
printed circuit board production particularly when surface mount technology is used.
Carbon based paints are silkscreen printed directly onto printed circuit boards in the
use of membrane switch contacts.
68
The manufactures of frequency selective surfaces are ideally suited towards silk
screen techniques deposited on different types of substrate etc.
The chosen material for pattern prototyping was a high performance conductive silver
ink (XZ250) supplied by Coates Circuit Products. This is screen printable ink used
typically in the manufacture of membrane switches and flexible circuits and is capable
of being printed on a variety of substrates. This ink is suitable for automatic and
semiautomatic printing machines and where quick drying is required. Typical
properties are shown in the following table:
This ink is suitable for application onto a wide variety of substrates, including
untreated and treated polyesters, which are commonly used for membrane switch
assembly. Treated polyester is particularly recommended to ensure good adhesion of
subsequent inks such as UV dielectrics and graphics inks.
It can also be used on other substrates such as polymide, PVC, ABS rigid PCB
substrates (phenolic and epoxy), glass and card etc. Compatibility tests of the
substrate should be undertaken before print runs are carried out. Successful printing
onto float glass and acetate film was undertaken for the prototype structures.
Conductivity is governed to a large extent by film weight. Therefore the mesh should
be selected to give the best combination of conductivity and economy.
Mono-filament polyester meshes of 49 90T/cm. (125 230T/inch) can be used with
most types of photographic stencil. Thread pitch is a compromise between the film
conductivity and structure resolution, a mesh of 62T/cm provided adequate resolution
and conductivity for the prototypes. The paint is manually applied using medium
hardness squeegees.
The table below shows typical surface resistivity values obtained with different
polyester screens. In order to ensure a sufficient conductivity of the deposited paint, a
technique whereby the screen is placed slightly removed from the substrate giving an
improvement in the film thickness.
All prints were dried as soon as possible after deposition in a fan convection oven,
ideally at 120C (248F) for 30 minutes. Adequate drying is critical in achieving
optimum conductivity. Drying at higher temperatures or for longer times will reduce
surface resistivity. The conductivity of the film can be significantly degraded if it is
not cured suitably after application.
Pigment Silver
Medium Thermoplastic Resin
Viscosity 30 50 Poise 25C (77F)
Solids 70%
Specific Gravity 2.000
Shelf Life 6 months sealed container
Sheet Resistance <0.04/ @ 15m (0.6mil) dry film thickness
Pencil Hardness 3H 4H
Theoretical Coverage 9m/kg @ 0.015mm dry film thickness
69
Mesh Count (TPC/TPI ) 49/125 62/120 77/195 90/230
Surface Resistivity (m/ )
As printed 32 22 39 50
Normalized to 0.015mm dft 32 39 36 30
Dry film thickness (mm) 0.015 0.0027 0.014 0.009
Many applications use the ink as supplied, but where a reduction in viscosity is
required thinners may be added to a maximum of 5% may be added. The final surface
resistivity depends on the dry film weight, addition of thinners will increase this, and
thus the use of thinners was avoided.
Conductivity of pure metals may not always relate to shielding effectiveness. The
surface of the metal, if exposed to air, may be chemically oxidised. Conductivity of
the metal oxide would then be a better indication of shield effectiveness. For example,
pure copper has excellent conductivity, but its oxide exhibits relatively poor
conductivity. Therefore, any shielding system that uses copper must protect its surface
against oxidation. The use of a thin coat that acts as an oxidation barrier is the most
common method of protection.
References:
[1] Dr. Yasin Zaka, Overview of Techniques for Applying Conductive Coatings to
Plastics for EMI/RFI Shielding. International Conference, Conductive Coatings
and Compounds. 21-22 June 1999. Brussels.
[2] Dr. Claudio PAGELLO, Test Methods for EMC Coatings Performance
Assessment. International Conference, Conductive Coatings and Compounds.
21-22 June 1999 Brussels.
[3] GE Plastics, Product Assembly Guide, Coatings/Shielding. Designing for
Electromagnetic Compatibility.
[4] Coates Circuit Products. Technical Information. XZ250 High Conductivity
Silver Touchkey Ink, December 1996. T039/0. Coates Electrographics Ltd,
Norton Hill, Modsomer Norton, Bath, Avon BA3 4RT.
www.coates.com/electro/circuits/home.html
[5] T.K. Wu, Frequency Selective Surface and Grid Array John Wiley & Sons Inc.
1995. ISBN 0-471-31189-8
[6] Chapter 6, Gregory S. Hickey, Frequency Selective Surface Materials and
Fabrication.
[7] Lt-Col. J.W. Molyneux-Child, Comparing Metals for Conductive Coatings
Surrey Electro-Shielding Ltd.
www.industrialtechnology.co.uk/surrey.html
[8] Chromerics Europe.
70
Parker Hannifin PLC., Parkway, Bucks, SL7 1YB.
Tel: +44(0) 1628 404000 Fax: +44(0) 1628 404890
www.chromerics.com
[9] Potters Ballotini
Bury St. Edmunds. UK.
Tel: +44(0) 1284 715400
www.pottersbeads.com
Fabrication Overview
The accurate modelling of frequency selective surfaces is a costly process in time and
computer resources. In order to assess a structures full performance it is often less
expensive and quicker to fabricate the structure and electrically measure its
parameters.
The fabrication process usually initially needs a mask, which supplies the pattern
information for etching or depositing conductive materials and is usually written in
graphical language with the following prerequisites
1. Efficiently reproduce repetitive patterns at the required resolution.
2. Identical output regardless of the computing platform, and output plotting device.
The interpreted Postscript language or its GPL equivalent Ghostscript meet the
above requirements. This is a popular stack orientated language and has sufficient
inherent mathematical functions to produce repetitive geometrical output on various
page sizes. Dedicated Postscript printers or Ghostscript drivers for current printers
enable plotting output to be easily obtained. Source files are written in ASCII format
and can be created or edited using many text editors. Commercial photographic
lithography equipment supports the language, and thus professional output on
photographic film is easily obtained.
Adhesives play an important part in bonding the conductive layer to required substrate
and fall into two categories, wet and dry.
Dry adhesives take the form of a laminar structure, adhesive on both sides of the
material and give a dry bond between the required layers. Such an example is Mactac,
which is optically transparent.
Wet adhesives, are obviously liquid in nature and are available in varying bond
strengths and viscosity. In the case of glass substrates, specialised ultra-violet curing
metal to glass adhesives such as Loctite 350. This adhesive leaves an opaque
appearance after etching.
Careful attention needs to be made when bonding the conductive layer to the substrate
such that the bond is uniform and contains no deformations such as air bubbles, which
will degrade the efficiency of the structure. Many structures are fabricated using an
etching process, and the adhesive must be capable of withstanding the temperatures
and chemicals during this process.
Printing of conductive inks using the silkscreen process are common in surface mount
technology, this can also be used to create structures of various sizes. Structures of
various sizes were fabricated by silk-screen printing onto acetate film and glass
71
Figure 1
Figure 2
substrates. The silk screens are actually nylon and are re-useable, the printing pattern
is generated in similar way to pcb technology using ultra-violet sensitive materials
and techniques. Special screen washes applicable to the ink have to be used to clean
the screens.
Fabrication Methods
The following describes various fabrication techniques, each method was selected to
meet specific physical properties. The main objective is to produce a fss on a glass
substrate.
Traditional Printed Circuit Board. (Figure 1)
Copper laminated fibre-glass backed printed circuit board with an ultra-violet
sensitive layer applied to the copper side is used. After exposure to ultra-violet light
through a pattern mask, It was developed and wet etched. Permitivity of the fibre-
glass dielectric is not well documented for frequencies up to several GHz. This
method is used primarily to assess the properties of the geometric pattern within the
structure.
Copper on Glass substrate using wet adhesive. (Figure 2)
Copper laminates have to be bonded individually if custom substrates are to be
considered. This sample was made by using Loctite 350 adhesive to bond the copper
laminate to the glass, and then exposing the bond to ultra-violet light. The main
problem is getting a uniform bond due to air bubbles forming between the layers, this
may be alleviated by using an adhesive with a lower viscosity. This technique is only
suitable for transparent substrates. The copper is then sprayed with an ultra-violet
sensitive lacquer and exposed via a mask to ultra-violet light. This is then developed
and etched. The adhesive stands up well to the etching process, although there is
degradation around the edges.
The adhesive also leaves an opaque appearance to the substrate after etching.
72
Figure 3
Figure 4
Copper on Glass substrate using dry adhesive. (Figure 3)
A dry adhesive (Mactac Permatrans) which is transparent is used to adhere the copper
laminate to the glass. Care during this process is again needed to eliminate all air
bubbles, this being easier to achieve than wet adhesive. The same etching process as
Figure 3 was used, the adhesive withstood the temperature and etching process well
although degradation was found at the edges. The result produced a more transparent
substrate than Figure 2 and had a more uniform laminate structure.
Copper on dry adhesive. (Figure 4)
To test a particular structure on different substrates, the copper is bonded to the dry
adhesive only, the protective backing on the reverse side left on. The etching
procedure again was that of Figure 2. The resulting structure was uniform with a small
degradation in the adhesive around the edges. The protective backing of the opposing
side to the copper could be removed and applied to a substrate of choice. The
structure could also be carefully removed from the substrate and applied to a different
one, this can be repeated many times giving a quick flexible test of substrate
characteristics upon the structure.
Silver paint on Glass/Acetate Substrate. (Figure 5)
With advent of highly conductive printing inks, silk screen printing methods using
silver inks are assessed. A silk screen mask of the required properties is produced
from the pattern mask, traditional silk screen printing methods are used to print the
pattern through the screen onto the required substrate. Due to the thickness of the
paint shims are needed between the mask and substrate during printing in order to
reduce flaring of the pattern. To obtain maximum conductivity, the structure should
be heat cured. This method produces multiple structures
quickly and sizes up to 3m.
73
Figure 5
Figure 6
Silver paint on Acetate with dry adhesive. (Figure 6)
In an attempt to obtain maximum testability of different lattices and substrates a
combination of techniques from methods 3 and 4 are used. This structure is silk screen
printed onto acetate film and then backed by the dry adhesive. This gave maximum
flexibility in that the structure could be adhered to differing substrates and the
individually pattern elements could be cut away and repositioned on a different lattice.
Also structures could be placed on top of one another allowing the testing of multi-
layer structures.
In performance testing of the above structures, it has been assumed that the various
adhesive and acetate films have no significant effect, this needs to be investigated
further. All the methods produced working frequency selective surfaces, by far the
most versatile being method 6. New materials are being developed rapidly, such as
transparent metals on film, these still have to be investigated. The most critical factor
in creating a fss is using a material with suitable conductivity, if the conductivity is
poor it will not operate at high frequencies.
Material References
1. PCB Photo-Resist copper clad FR4 board.
RS Components, PO Box 99, Corby, Northants, NN17 9RS
Tel: 01536 201201 Fax: 01536 201501
http://rswwww.com
2. Domestic Float Glass
Pope & Parr, 118/120 Talbot St., Nottingham, NG1 5HH.
Tel: 0115 9473015, Fax: 0115 9473015.
74
3. PRP 200 Positive Photoresist
Electrolube, Wentworth House, Blakes Rd., Wargrave, Berkshire. RG10 8AW.
Tel: +44 (0) 1189 404031. Fax: +44(0) 1189 403084.
www.electrolube.com
4. Loctite 350 (35038) UV Curing Adehesive glass/metal.
Henkel Loctite Adhesives Ltd., Watchmead, Welwyn Garden City, Hertfordshire,
AL7 1JB.
Tel: +44(0) 1707 358800. Fax: +44(0) 1707 358900.
www.loctite-europe.com
5. Mactac Permatrans 2113 film adhesive
Mactac UK Ltd., 4-6 The Britannia Trade Centre, RyeHill Close, Lodge Farm,
Northampton, NN5 7UA.
Tel: +44(0) 1604 756521 Fax: +44(0) 1604 758150
www.mactac-europe.com
6. XZ250 High Conductivity Silver Ink
Coates Screen., Cray Avenue, St. Mary Cray, Orpington, Kent BR5 3TT.
Tel: +44(0) 1689 875201. Fax: +44(0) 1689 878262
7. Copper Clad Laminate
Crossley & Bradley Ltd.
Ulneswalton Lane, Leyland, Preston, Lancs. PR26 8NB.
Tel: +44(0) 1772 452236. Fax: +44(0) 1772 456859.
Section 7: Review Of Transparent And Conductive Oxides Frequency Selective Windows
75
Section 7: Review Of Transparent And Conductive Oxides
Introduction
Among the aims of this feasibility study is the investigation of the possibility of
replacing the conductive metal in the FSS structures with equally conductive but
transparent material (TCO) for aesthetic as well as practical purposes. It is more
appealing to the eye if the total transparency of the window is not disturbed by the
opaque nature of the most metals. On the other hand working conditions in spaces
protected by FSS structures might necessitate visual continuity through these
structures.
The first semitransparent and electrically conductive CdO film was reported as early
as 1907. However substantial technological advances were only made after the 1940s
when interest on these materials was generated by their potential applications in
industry. Such films have been used as transparent electrical heaters for windscreens,
as gas sensors, in solar cells, heat reflectors, protective coatings, light transparent
electrodes, laser resistant coatings, anti-static surface layers in satellites, surface layers
in electroluminescent devices, and recently in horticultular glasshouses.
Such transparent conductive materials are mainly oxides of indium, zinc, cadmium,
tin, and combinations between these oxides.
Thin films of metals (gold, silver, copper, iron ) have also been found to have similar
properties but in general are not very stable and their properties change with time.
They are also inferior to the former in terms of hardness and transparency.
The basic properties of these films that are most important for practical applications
are their structure, morphology, electrical conductivity and optical transparency.
These properties can be altered selectively by introducing different dopants and also
by using different growth techniques.
Ideally both optical transmission and electrical conductivity should be as large as
possible. However the simultaneous accomplishment of both high transmission and
conduction is not possible since these parameters are inversely proportional. You
cannot have optimum conductivity without sacrificing transparency.
In this report we will summarize the findings of different research groups according to
their electrical and optical properties after we have introduced the different growth
techniques with their corresponding merits.
Immediately after the introduction of each technique a section follows with the
summary of the different experimental results that have been presented in the
literature.
A number of different deposition techniques have been used to deposit TCOs. Since
the electrical and optical properties of these films depend strongly on their
microstructure, stoichiometry, and the nature of the impurities present during growth,
each technique yields films with different behavior. This is also particularly true when
the same technique is used by different research groups, since identical arrangement
of the growth systems in conjunction also with the growth parameters is the exception
rather than the rule.
The main TCOs that we shall discuss are tin oxide (SnO
2
), indium oxide (In
2
O
3
),
indium tin oxide (ITO), and zinc oxide ZnO).
If these semiconductors are prepared intrinsically i.e. without intrinsic or extrinsic
dopants their resistivity is very high (of the order of 10
7
cm). The low resistivity
that is required for their application as TCOs can be achieved in two ways:
76
Creation of intrinsic dopants by lattice defects. These can be oxygen vacancies or
metal atoms on respective lattice sites, and with
Introduction of extrinsic dopants (atoms of materials foreign to the pure form of
the original compound). These can be either metals with one additional
conduction electron on zinc lattice sites or halogens with one additional electron
on oxygen lattice sites.
Among them the most popular are the ITO and the ZnO. The ZnO based TCOs are
favoured over to ITO due to the lower production cost, lower toxicity and greater
stability in atmospheric environment.
Growth techniques
The growth technique plays a significant role in controlling the properties of these
films because the same material deposited by two different techniques usually has
different physical properties.
This is due to the fact that the electrical and optical properties of these films strongly
depend on the structure and morphology of the film, and on the nature of the
incorporated impurities. These properties are depended in turn on the various
deposition parameters used which when properly chosen can produce films with the
desirable characteristics.
In these section we will discuss numerous deposition techniques that have been
employed to grow transparent conductive oxide films (TCOs).
Chemical vapour deposition (CVD).
This technique is widely used in the semiconductor industry for its capability to
produce high quality thin films without the need for high vacuum. This technique
involves the reaction of one or more gaseous species on the surface of the substrate.
A vapour containing the condensate material is transported to the substrate surface
where it is decomposed.
A thin film is deposited as a result on the substrate. For TCOs usually volatile
organometallic compounds are used. A carrier gas such as oxygen, water, argon or
nitrogen carries the vapours of these compounds. The decomposition process should
be such that the reaction occurs only at the substrate surface and not in the gaseous
phase. The quality of the films depends on various parameters, such as substrate
temperature, gas flow rate and system geometry. In order to obtain the best quality
films these parameters should be optimized.
Particularly for TCOs if the substrate temperature is low, carbon occlusions are found
in the films because of the incomplete oxidation of the organic material. However, if
the substrate temperature is too high it will result in the decomposition of the
organometallic compounds in the gas phase rather than the substrate, thereby
producing powder-like deposits instead of a smooth film.
The main advantages of CVD are the simplicity, reproducibility and large-scale
production capability without the need for high vacuum as an essential requirement
for deposition. Moreover, due to the low cost of the equipment used, the cost of
production is low. Unfortunately the nature of the chemical reaction demands high
deposition temperatures, in excess of 450C.
77
In some variations of the main method the creation of a plasma around the substrate
results in better quality films at lower deposition temperature. This is called plasma
assisted CVD.
The gasses that are generally used are very toxic to humans and extremely flammable,
needing special handling requirements. Most of them are not harmful to ozone layer,
though. This information was provided by EPICHEM (contact Mr Colin Overton, Tel:
01513342774)
Atomic layer epitaxy
Like CVD atomic layer epitaxy (ALE) is an epitaxial chemical vapour process
producing, like all epitaxial processes, good quality films. ALE relies on the self-
limiting reactions between alternately dosed gaseous precursors, and is capable of
producing films with uniformity and excellent thickness control even on complex
surfaces. At first, the precursor of the first atomic constituent atom of the film to be
deposited, is flushed into the high vacuum chamber where it breaks down at the
surface of the substrate depositing a thin layer of a few atomic distances in thickness
of the first constituent. A rapid cycle of purging with inert gas follows to clear any
remains of the first gas, followed by the next flushing of the precursor of the second
constituent. Again the same process leaves an atomic layer of this constituent which
now reacts with the previous atoms to form well-ordered crystals. At the moment this
method is used predominantly for the production of high quality electroluminescent
devices with II-VI phosphors. Due the slow growth rate it is not very cost efficient.
Experimental and comparative results
CVD has been extensively used for the production of tin oxide and with some success
for zinc oxide.
For the former stannous and stannic chloride, tetramethyl tin, dimethyl tin dichloride
and dibutil tin diacetate are most commonly used. These gases are oxidised at high
temperatures by oxygen or water. When water is used lower deposition temperatures
are employed.
Regarding indium oxide the cost of the relevant organometallic compounds is
prohibitive, so the CVD method rarely has been used. When indium acetylacetonate is
used, oxygen must be used for the oxidation. On the contrary two-ethylhexanoaate is
used with inert nitrogen only.
When indium and tin acetonates (In(C
5
H
7
O
2
)
3
and Sn(C
5
H
7
O
2
)
2
) are used for
deposition of indium tin oxide low resistivities and high transparencies are achieved.
For tin oxide, tetramethylin or TMT (Sn(CH
3
)
4
) is used with oxygen as reactants.
Although TMT is flammable and toxic, it is stable in air and moisture and can be
safely contained in a glass or quartz vessel.
For zinc oxide deposition organometalic compounds are substituted by zinc vapour. A
mixture of nitrogen with water or hydrogen is used to start the reaction. When
ammonia is used instead, better films are produced but at lower rate. Alternatively,
Zn(C
5
H
7
O
2
)
2
was used as a precursor for Zn and In(C
5
H
7
O
2
)
2
was used as a precursor
for In. The carrier gas was nitrogen and the deposition temperature was 525 C.
It is reported in one very recent study that ZnO doped with Ga and In is more
conductive than when Al and In are used as dopants. In the same study it was
commented that CVD prepared ZnO is more stable in harsh atmospheric conditions
than the sputterd ZnO.
78
Generally there are not many publications for CVD deposited TCOs in comparison
with sputtered and evaporated ones.
Regarding ALE research have been carried on since 1994 mainly by the University of
Helsinki where the process first originated. InCl
3
and SnCl
3
are the precursors for
Indium (In) and tin (Sn) respectively. H
2
O or H
2
O
2
are used to initiate the chemical
reaction. There are many publications were the process is explained and different
designs are proposed.
The following table summarizes the above comments:
TABLE 1
TCO Substrate
Temperature
C
Rate
A/min
Resistivity
cm
Transmission
%
Remarks Ref.
SnO
2
250-400 ------ 10-10
-3
80-95 SnCl
4
+H
2
O 50
SnO
2
480-680 ------ 4x10
-2
-10
-3
90 ------ 2
SnO
2
420 ------ 5x10
-3
90 O
2
+H
2
O 3
SnO
2
:P 400 ------ 7.5x10
-4
83 ------ 4
SnO
2
:F 570 3600 3.3x10
-4
90 ------ 5
In
2
O
3
527 7980 9.3x10
-4
89 ------ 6
ZnO:Al 367-444 ------ 3x10
-4
85 ------ 7
ZnO:Ga ------ ------ 1.2x10
-4
85 Very stable 8
ZnO:In ------ ------ 1.1x10
-4
85 Very stable 9
ZnO:In 525 ------ 4.6x10
-3
90 ------ 10
ITO 450 ------ 1.8x10
-4
90 Sn/In=0.0
31
11
ITO 300-500 6.5 3.9x10
-4
------ ALE 242
Vacuum evaporation.
Vacuum evaporation is one of the oldest and most widely used methods for depositing
thin films. The Joule conductive heating of metal wires which in the form, generally,
of baskets or boats are used to house the source material, is employed to decompose
this material into different chemical constituents (thermal or flash evaporation). These
then are deposited to form thin films on the opposite situated substrate.
An appropriate heater can heat the substrate if it is so required. The evaporation can
be carried out in vacuum or in the reduced environment of a selected gas. For TCO
evaporation, oxygen or an argon-oxygen mixture is usually used. The important
control parameters are the substrate temperature, evaporation rate, source-to-substrate
distance and oxygen partial pressure. The TCOs can be evaporated in three ways: (i)
by directly evaporating metal oxides, (ii) by reactive evaporation of the metal in the
presence of oxygen, or (iii) post-oxidation of metal films. It is common to heat-treat
the grown films at high temperatures in water, hydrogen or oxygen environment to
improve further the conductivity.
79
As in CVD different versions of evaporation exist to facilitate the reaction between
the evaporants and the gas, such as in a plasma or in a low power laser source shining
at the substrate so chemical reactions can be promoted further.
The vacuum thermal evaporation is a cost- effective method with high deposition
rates (R), albeit suitable only for small substrates. The deposition temperature is also
high enough for this method to be prohibitive for glass substrates. The possibility of
introducing impurities from the material of the crucible is also high.
Electron beam evaporation
This method is another form of evaporation where a beam of electrons is used to
vaporize the material of the target. It is more controlled and cleaner than thermal
evaporation with the result of producing higher quality films. It is also suitable for
many materials. A continuous source of electrons can be used to vaporize a material
locally. It can be used for deposition on large substrates and so, it is suitable for
industrial applications. Contrary to the sputtered or ion plated films were ion
bombardment can cause damage to the growing film, e-beam evaporated films are
more crystalline (they have larger grain size and lower defect density). Usually due to
the high quality of these films, lower substrate temperature is used without the
necessity of post-deposition annealing.
There are variants of this technique as well.
By creating an arc between the cathode and anode the deposition rate increases
dramatically (usually it is between 6-20nm/sec).
There are different types of arcs depending on the manner that are created at the
electrodes. Glow cathode, cold cathode as well as hollow cathode variations can be
used.
This method is very sensitive to the presence of water vapor in the system, and the
films show poor quality when this occurs.
Alternatively by introducing an ion source where the ions are bombarding the
substrate during growth, denser and more adhesive films are created, even at room
temperature without any post-deposition annealing. These ions can be monomer
oxygen ions or clusters of oxygen ions with mean size of 3000 atoms per ion or even
argon ions. Their size of course can vary to suit different applications. Cluster ions
due to their size interact only with the surface of the growing film resulting in
smoother, cleaner and well ordered films. The deposition temperature can be low as
well. Changes in the angle of incidence of the ions to the substrate have been found to
be important in tailoring the properties of the films.
We can say that ion assisted evaporation results in improved film properties, like
increased adhesion, hardness, and packing density compared to sole e-beam
evaporation. More on the subject of ion-assisted deposition will be discussed in the
section dedicated to ion deposition processes later on.
Recently, a process where the deposition is achieved by e-beam evaporation at very
slow rate and a temperature gradient is present across the substrate has resulted in the
lowest resistivity in ITO ever reported (4.4x10
-5
cm). The slow rate allows
deposited atoms to diffuse and be positioned favourably on the substrate, where as the
temperature gradient promotes the formation of crystalline grains with similar
orientations at neighbouring sites. This method is called zone-confinement.
80
Usually the deposited ITO film is formed in a mixture of hexagonal and cubic
crystalline grains. This is an arrangement that can create scattering in the moving
electrons when crossing through neighbouring grains due to very defective boundary
that separates them. This causes reduction in mobility and thus lowers the
conductivity.
In any deposition process the first atoms that arrive at the clear substrate surface
segregate at distinct places called islands of formation and form crystallites if the
temperature of deposition is high enough. Otherwise these islands are made from
amorphous material. These crystallites eventually grow and merge into each other to
form a film. In non-epitaxial processes, like the ones we are discussing here, these
crystallites contain material in different orientations called grains. When there is a
temperature gradient between two crystallites the defects that have been formed, or
dopant atoms that have not been integrated are pushed to the boundaries (this is
especially true for ITO). The result is that grains within a zone (i.e. crystallites that
happen to grow at almost uniform temperature) are oriented in the same direction and
the boundaries that separates them are twin boundaries that cause little scattering in
the moving electrons. So higher conductivity is achieved due to increased mobility
along certain planes.
A wide range of vacuum evaporation techniques has been used to deposit tin oxide
films. Flash evaporation [13] has been nowadays substituted by e-beam evaporation
[14,15] for the reasons we stated above. Tin can be used as target in oxygen
atmosphere or instead a tin oxide target can be employed in vacuum. The as-
evaporated films mainly have SnO phase (which is semi-transparent), and is produced
by decomposition of SnO
2
molecules during evaporation. Post-deposition is generally
necessary in order to obtain transparent conducting oxides. If the films are amorphous
post deposition is carried out in the presence of oxygen. The angle of incidence of
SnO
2
vapour onto the substrate significantly affects the growth behaviour of these
films [16,15]. Films grown at incidence angles less than 60 are highly resistive and
yellowish brown in colour and rich in SnO phase. Heat treatment must follow to turn
the films that are opaque into transparent.
In a recent study arc discharge vapour deposition was used for tin oxide. Parallel to
the deposition an electrical current was applied with two electrodes on the substrate.
The electric field is possibly causing intensified electromigration along high
resistance paths. SEM data show that the imposition of an electric field parallel to the
substrate causes a modified microstructure to form. This growth might be aided by
intensified electromigration or by a thermodynamically favoured condition by the
presence of the field.
Vacuum evaporation is more commonly used for indium oxide than tin oxide [20-26].
Again the same general remarks that have been stated above are true. However, it was
observed that incorporation of metallic indium in the evaporation source not only
significantly enhanced the rate of evaporation, but also significantly improved the
optical and electrical properties of the films.
In one study [19,20] it was found that films grown with tantalum (Ta) or tungsten (W)
heater had the worst conductivity. It was suggested that a chemical might had been
taken place between the indium and these metals. As a remedy a proper combination
of crucible and a heater element or a crucible with a high lip might be used instead.
81
A plasma can be used close to the substrate to enhance the reactivity of In vapour with
oxygen so as lower temperature can be used [21,26]. A tungsten (W) emitter and a
voltage supply can create the plasma.
There are many reports on the deposition of ITO by evaporation as well [27-36]. Most
researchers have deposited these films by reactively evaporating either metallic alloy
or an oxide mixture. Some times two metallic sources are used. Sequential metallic
evaporation of In and Sn is used as well, followed by annealing [28,41]. The
advantage of this method is that the composition of the films can be controlled
accurately. The substrate temperature has to be more than the crystallization
temperature of ITO which is 150C in order to avoid deposition of amorphous films
[37]. However, it has been argued that the deposition rate is more important than the
substrate temperature in producing transparent films [38]. Although very high
deposition rate results in worse conductivity and transparency, and increase in the
deposition temperature can not offset this effect. In this study the deposition rate was
varied from 2-120 A/min [38].
The method of applying an electric field parallel to the substrate during growth has
also been tested on ITO deposition [43]. The DC electric field was varied between 0-
110 Volts. However, the resistance of the films was high, being between 100-10
8
.
No other parameters were given to deduct the resistivity. The high resistance might be
explained by the poor vacuum conditions.
Below follows a table that summarises the most significant results that have been
reported in the literature concerning the evaporation deposition of some of the TCOs.
TABLE 2
TCO Substrate
Temperature
C
Rate
A/min
Resistivity
cm
Transmission
%
Remarks Ref.
SnO
2
480 60-120 0.03-40 >85 In O
2
17
SnO
2
:Mo 480 60-120 3x10
-3
>85 In O
2
17
SnO
2
RT ------ 5x10
-4
------ Arc+cur 18
In
2
O
3
320-350 ------ 1.8x10
-4
>95 Flush+O 19
In
2
O
3
350 or 200 ------ 3.2x10
-4
>96 Flush ,Ar+O 21,26
ITO 400 ------ 2x10
-4
80 Flush+O 44
ITO 350 400 8.8x10
-4
88 Plasma
flush+O
26
ITO ------ ------ 4x10
-3
>90 Sequential
+O
28
ITO 200 96 2.4x10
-4
90 e-beam+O 29
ITO ------ 4000 1.7x10
-4
80 e-beam,large
area
applications
45
ZnO 150-200 ------ 1.5x10
-3
89 Flush+O 46
Sputtering
Sputtering is one of the most versatile techniques used for the deposition of
transparent conductors when high quality films are required. It is widely used in
different versions and modifications. Recently, a highly conductive and transparent
ITO was produced in the opto-electronics lab of Nottingham Trent University, which
competes favourably worldwide with the best reported ITO [47]. Additionally,
82
literature survey done in order to complete the current report revealed the wide extent
of the use of sputtering in research labs and industries around the world.
So, there are enough reasons to cover in detail this versatile technique. However, we
will concentrate only on these variations of the main technique that have been used
successfully in developing good quality TCOs.
Compared with other techniques, sputtering produces films with higher purity and
better-controlled composition. It provides films with greater adhesive strength and
homogeneity and permits better control of film thickness [48]. Many different
methods are categorized as sputtering because they have in common the ionization of
a material by generation of a plasma, which is in close confinement and next to a
substrate where deposition subsequently occurs.
The sputtering process involves the creation of a gas plasma (usually it is an inert gas
such as argon) by applying a voltage between an anode and a cathode. The cathode is
used as a target holder and the anode is used as a substrate holder. The voltage
potential causes the dissociation of gas atoms into ions and free electrons. The ions
are attracted to the cathode where by momentum transfer, particles are ejected from
the surface of the target and they diffuse away from it been deposited onto the
substrate. When the kinetic energy of the ions exceeds the heat of sublimation (or
chemical bond energy) of the target material (roughly by four times) sputtering
happens. The electrons are responsible for the sustenance of the plasma because there
are smaller and move quicker [49, 50]. By this reason they diffuse quickly and they
bombard the substrate, thus increasing its temperature sometimes by a couple of
hundred of degrees Celsius. Across the plasma a negative potential forms, and over
the electrodes an even bigger negative potential drop exists due to the
thermodynamics of the whole process. The difference between these two potentials
determines the energy of those ions, which strike the electrodes and the ejected
charged species.
The ions also diffuse and can cause problems. There can be positive and negative ions
in a plasma. Usually a source of the former is the inert gas and of the later the reactive
gas. The sputtered material mostly exists in atomic form, and so it is neutral [51]. A
cause of film degradation is the production usually of negative ions, also, during
sputtering of the target. This is especially true for oxide targets, where production of
negative oxygen ions is frequent. These negative oxygen ions will suffer additional
acceleration due to their charge and re-sputter the substrate [52- 55]. Other research
done on this topic failed to detect any negative ions, all the observed ions were
positive and existed either in elemental or compound form [56]. However, re-
sputtering is a serious problem and causes degradation of the film.
The main merits of sputtering are:
Different materials can be sputtered at almost comparable deposition rates. This is
not true for evaporation where the same temperature can give widely ranging
growth rates for different materials. So, with sputtering different materials can be
co-deposited.
One can sputter films of complicated materials, like stainless steel, pyrex,
permalloy et al without composition changes between target and film.
Film-thickness control becomes relatively simple.
Sputtering can be accomplished from large area targets.
In sputtering there are no difficulties with spitting or ejection of large
agglomerates instead of simple ions. This often occurs in vacuum evaporation.
There are also no restrictions with substrate arrangement. So, often downward
83
sputtering, where the target is positioned above the substrate is preferred. If the
discharge is operated at gas pressures lower than about 5mTorr, the sputtered
atoms arrived at the substrate with high kinetic energy. This maybe beneficial to
film structure and the adherence to the film.
The main disadvantage is the relatively low deposition rates.
There are two methods of powering the sputtering system: by DC or by RF source.
In a DC sputtering system a direct voltage is applied between the anode and the
cathode. It takes a considerable voltage drop across the electrodes to start initially the
plasma. The bombardment of the target by the gas ions not only ejects target material
species but also produces stray electrons, called secondary electrons [57]. These
electrons are responsible for sustaining the plasma, since in DC excitation electron
recombination with ions is frequent. In some cases the plasma can be excited or
sustained by a hot thermionic cathod, which emits electrons to replace the lost ones, in
order to use less voltage across the electrodes.
Stabilization of the plasma in DC excitation mode has been a challenging task for
many years. Arching is among the factors that can destabilize the plasma. It happens
mainly when insulating or compound materials are used as targets. During the
process, thin dielectric layers grow in the non-eroding areas of the target which
steadily charge up due to the bombardment of the positive ions. Arching then occurs
which generates particulates and contaminates the film. If arching will not terminate
the process, eventually after sputtering for a period, the walls and the anode would be
covered with insulating material, which will disrupt the process [58]. So, DC
sputtering is used mainly for conducting films such as metals like indium, tin or zinc
and leads to very high deposition rates. This is an advantage because metallic targets
are easier to manufacture with high purity, and are thermally conductive, so they do
not crack easily. However, in this case higher quantities of oxygen must be present in
the system for reactive deposition to take place. This also causes reactions to take
place at the surface of the metallic target transforming it into a compound insulating
material, which sputters at lower rate [59]. This happens suddenly at some rate of
reactive gas flow because the window for allowable oxygen rate is very small. The
effect is called target poisoning and leads to poor quality films.
Because of this main problem and the interdependence of the sputtering parameters,
DC sputtering is considered a very complicated process and in depth theoretical
modeling has been investigated [59]. A lot of methods have been proposed in the past
[60] to rectify these problems.
A feedback control of the oxygen gas pressure has been offered as a solution. This can
happen by observing directly the spectral emission of the reactive gas ions, or by
monitoring the voltage drop at the target [61]. For constant pressure and power, the
cathode voltage can be used as an indirect measure of the degree of the target oxide
coverage [62-65]. Pulsing of the oxygen gas line has also been used, to reduce
momentarily the oxygen environment. Another method to overcome this problem as
well as arching is by using medium AC frequencies (AM) in the range 20-100 KHz
[66-68]. They have the advantage of being as simple to handle as DC, and do not
require load matching and tuning like the RF frequencies. Design details for a AM
power supply that has industrial applications can be found in a detailed paper by
Wallace [69], along with list of references.
A set up of two-leveled magnetron electrodes powered by medium AC frequencies
has been evolved as a solution, also, to all the above problems, with mass production
capabilities [58, 70]. At any time, one of the magnetrons is on negative potential and
84
acts as a sputter cathode, while the second one acts as an anode. The momentary
cathode is generating secondary electrons, which are accelerated towards the anode
and neutralize positive surface charges having built up during the negative half cycle.
These charges build-up when compound materials are sputtered. These positive
charges will create eventually arching. In growing SnO
2
and ITO with this system, the
deposition rate can be up to three times more than a single DC magnetron system.
Recently, a variation of some of the above methods has been tried with good results:
in an unbalanced magnetron electrode with pulsing of oxygen. This method has been
called plasma anodization [71-74]. The pulsing happens at 1sec intervals. When
oxygen is absent in the inert gas, metal is sputtered, otherwise the oxygen ions are
released slowly to the substrate to chemically react with the thin layer of metal which
was previously deposited.
There are other methods of stabilization of the DC magnetron sputtering and a list
with comments can be found in a review paper by Safi [60]. These involve varying
the pumping speed of the vacuum, increasing the target-to-substrate distance, feeding
the reactive gas close to the substrate and away from the target, monitoring the gas
pressure by optical or electrical means and others.
Generation of a highly ionised plasma, with optimised substrate ion bombardment and
subsequent decrease of deposition temperature can be achieved also with electron
cyclotron resonance sputtering (ECR) [75-80]. In this case a microwave source (2.45
GHz) is placed behind a DC magnetron electrode, and another DC magnetic coil is
placed behind the substrate. This configuration results in precise control of ion
energy, and thus ion bombardment of the substrate is greatly reduced. However,
positive ion bombardment is not totally undesirable. In one study by using ECR it was
found that Ar ion bombardment, with a separate ion source, with energies lower than
40 eV enhances crystallization whereas bombardment with higher energies suppresses
crystallization [79].
The stabilisation of the plasma becomes extinct in the case of RF sputtering where
oxide targets are used, so the partial pressure of oxygen does not need to be big.
However, this comes at an increased cost and complexity of the power supply.
In RF sputtering, which is suitable for both conducting and insulating films, a high
frequency generator (usually 13.56MHz) is connected between the electrodes. In this
case the cathode (target) becomes momentarily, for a cycle, the anode, and it will
attract the free electrons. Otherwise it will attract the positive ions. Because of the
difference in the ion and electron currents (due to their difference in the respective
masses) every insulator or floating electrode will be at somewhat negative voltage
with respect to the plasma. This has to be so in order to repel some of the more
abundant arriving electrons and thus keep the total current at zero since an insulator is
involved in the circuit and current should not be flowing through the circuit. So, if an
insulator is placed at either electrode a negative potential will build up. This potential
depends on the frequency of the plasma. For absolute value of 100 Volts or lower
voltage build up on the cathode, frequencies greater than 10 MHz should be used.
This potential is usually called target potential, self-bias potential or discharge
potential. The deposition rate is proportional to this potential. Incidentally, for DC
magnetron sputtering is about 350 Volts and decreases with increasing input power.
Due to this difference between the two processes, the deposition rate for the DC is
1.5-2 times higher than the RF process.
As we discussed earlier on, the DC excitation of a magnetron is based on the delivery
of the secondary electrons from the target. Therefore, a large discharge voltage is
necessary to sustain the plasma because the secondary electron emission increases
85
monotonically with the required ion energy. On the other hand the RF plasma is
mainly driven by the ionization of gas atoms by the oscillatory mode of the voltage,
and is more stable because the electrons and ions are in continuous motion, and
mutual recombination is prohibited. However in this kind of excitation the magnetic
confinement of electrons is not as good as in DC magnetron sputtering.
It was observed that by reducing the input power or by increasing the target potential,
films with lower resistivity result [81]. This is particularly true for oxide films,
because the increase in the target bias suppresses the bombardment of the film surface
by the highly energetic negative oxygen ions. Subsequently, it follows that in RF
discharge the mean kinetic energy of electrons is higher than in DC plasma. It was
calculated that for DC plasma one gets 3.9eV where as for RF 9.6eV.
The same effect can be obtained by just increasing the RF frequency. Recently
frequencies between 10-100MHz have been compared [82]. The target potential
becomes higher than 60V for frequencies above 50MHz. However, with the joint use
of a DC and RF magnetron system is easier to control the deposition conditions [82].
The RF power was used to produce the plasma in the space in front of the target, and
the DC power was used to control the energy of the ions when they impinge on the
target.
Circular magnets at the back of the target in magnetron sputtering are used to
concentrate the plasma in a tight sphere around the cathode (target), an electrode from
which would normally be repelled, making it easier to sustain a plasma at a lower
pressure. The circulating electron follows a continuous path over the target and is only
stopped when collides with a gas particle causing ionization or excitation of it.
Although the plasma is concentrated over a restricted region of the target with a
resultant poor energy efficiency (most of the energy loss is heat loss to the target),
high deposition rates, low substrate temperatures and higher quality films are the
merits of magnetron sputtering.
A common technique to improve the quality of the films is to apply a bias on a
floating substrate to attract the ions. The bias can be positive or negative depending on
which ions need to be more energetic when impinging onto the substrate. This usually
can be detected experimentally.
An obvious technique in order to avoid the energetic ions damaging the substrate is to
have the plasma concentrated between two electrodes carrying similar targets. The
substrate can then be mounted on a separate electrode that is positioned outside the
immediate boundaries of the plasma [83].
Although all sputtering processes take place in low vacuum, recently a new
configuration has been developed and is called atmospheric RF plasma deposition
technique [84-86]. A mist of a chemical agent is carried by an inert gas in a chamber
where is vaporized with the use of an RF supply. The deposition takes place in high
substrate temperatures but it does not need high vacuum. It has been developed for
mass production of thin films.
The same sputtering systems that have been used in semiconductor integrated circuit
industry has also been tried successfully in the production of ITO. The system is
called cluster-sputtering system and is comprised of a series of sputtering chambers
arranged in a circle, where deposition takes place. The substrate is circulated from one
end to another and successive depositions take place [87-89].
86
Experimental and comparative results:
The research on the sputtering of different TCOs usually involves the study of the
influence of the different process parameters; mainly the deposition temperature, post-
deposition annealing, microwave power input and pressure. More detailed studies
look into other parameters like the target-substrate distance, surface and bulk
morphology and target preparation. Some studies have tried to correlate the
observation of the optimum electrical and optical properties to that of a certain
crystallographic orientation with equivocal results. There is not any preferred
orientation that favours the electrical conductivity and/or transparency. On the
contrary different methods of preparation result in different crystallographic
orientations, but otherwise not so diverse optical and electrical characteristics.
Despite decades of research the mechanisms for the electrical conduction and the
crystalline growth have not been completely determined, probably because of their
complex nature. The main obstacle in the theoretical characterization, mainly of ITO,
has been its complicated molecular structure. The unit cell of the ITO contains 40
atoms and this makes any detailed analysis difficult. We could not find but one recent
paper dealing with band structure calculations [90].
Both reactive and non-reactive sputtering have been employed for growing TCOs.
Sputtering from oxide targets is significantly different from sputtering of metal
targets. The control of the film stoichiometry is easier when oxide targets are used, at
expense of deposition rate. Generally post-deposition annealing is not required when
oxide targets are used. In the case of reactive DC sputtering of metallic targets the
deposition rate and the structural properties of TCOs are strongly depended on the
oxygen partial pressure. Due to the problems of the DC process which were discussed
above, expensive control mechanisms are used to avoid the oxidation of the target if
high partial pressure of oxygen is necessary [91]. These extra expenses are justified
since DC sputtering has the highest deposition rates among the different sputtering
processes. Recently a new type of magnetron electrode was introduced for economical
utilisation of the target material [92]. All current magnetron electrodes confine the
plasma around a circular ring resulting in selective sputtering of the target (called
racetrack). The target needs replacing before all the material is been utilized. The new
electrode is comprised of a sophisticated mechanism to move the magnets around in a
lot of different modes, so selective sputtering is prevented.
Recently, attempts also at improving the twin magnetron electrode system described
above (called Twin Mag I by Leybold Systems), have been announced [93]. The new
version comprises the two electrodes at a slant, and has improved design of the
magnets. The new magnets improve the target utilisation by 45%.
In both modes of sputtering and all TCOs the rate of deposition is a strong function of
RF power and the total pressure of argon, and partial pressure of oxygen.
As in evaporation, in sputtering of SnO
2
adequate quantities of oxygen must be
present to avoid formation of opaque SnO, which has a yellowish brown color [94-
96]. X-ray studies have shown that polycrystaline films grow in (111) orientation
when sputtered in reduced oxygen enviroment. With increasing oxygen concentration
the (101) becomes predominant. Sometimes the presence of (110) orientation is
observed instead of the (101) [97-98]. The SnO
2
grown by the Twin Mag system
shows a mixture of orientations that change according to pressure [99]. The same
work presents data of the superior quality of these films compared with the ones by
original DC magnetron sputtering in terms of hardness and internal stress.
Unfortunately there are no data concerning the conductivity of these films. In general
87
there is not a lot of work on sputtered tin oxide compared with the extensive number
of publications on ITO.
The most frequently used dopant in SnO
2
is antimony (Sb) [100-106] at a
concentration of 10 at%. Unfortunately the conductivity of these films can only be
improved by annealing at high temperatures (400-600 C).
Indium oxide has been grown by reactive sputtering of a metallic target, or by
sputtering of oxide targets [108-118]. The effect of the substrate bias on the
deposition rate and structural properties of RF sputtered films was studied in Ref 109
and 110. The deposition rate initially increases with increase of substrate bias.
However, as substrate bias is further increased, the deposition rate starts decreasing
due to re-sputtering of the substrate. X-ray diffraction and electron microscope
studies indicate that the effect of the substrate bias on the microstructure of the films
is quite significant. The degree of (100) orientation increases and the density of
structural defects decreases with the increase of the substrate bias up to 60V.
In structural studies [110, 118] films grown along (222) orientation showed excellent
electrical and optical properties. It should be noted that films produced by other
techniques have a variety of preferred orientations as is expected, but the (222)
orientation is normally produced by annealing the films at high temperatures (400 C).
In contrast to the two previous materials, ITO has been a very successful TCO. A lot
of work has been published and is currently, along with ZnO:Al, favoured in the mass
production of electrodes in organic electroluminescent devices and solar cells [119-
124, 125-128 respectively]. Due to their high conductivity they can also be used as
heat reflecting coatings [129-131]. The sputtering process is preferred over the other
production methods because of the high reproducibility and controllability of the
films.
The main crystallographic orientations of ITO are the same as those of indium oxide:
(222), (400) and (440). One of the factors that affects the structure and intensity of the
peaks is the energy of the sputtered particles arriving at the substrate. Kumar and
Mansingh [132] examined the properties of ITO films by varying the target-substrate
distance in RF sputtering. Although this process is rarely used nowadays, is indicative
of the difference between sputtering and evaporation. The sputtered particles or
molecules undergo collisions during their passage through the plasma and they
continuously losing their initial energy and change direction. After a certain number
of collisions their energy reduces to the thermal energy (kT) and the motion becomes
random. This happens at a certain distance that is called thermalisation distance, after
which the transport of atoms occurs, by diffusion [133, 134]. At this distance a virtual
source can be considered to exist in place of the original, since the original source
loses its characteristics after this distance. The thermalisation distance increases with
increasing RF power and decreasing total gas pressure because the ions are more
energetic and travel further. Two orientations, (222 and 400), were significant in the
study of Kumar and Mansingh and seemed to indicate the quality of the films
regarding its position to the virtual source. Varying either the RF power or the
pressure shifted the position of the virtual source. The (222) orientation was
prominent whenever the substrate was above the virtual source. Otherwise, the (400)
orientation was dominant. These observations suggest that the energy of the arriving
species at the substrate influence the structural quality of the films. So, the
thermalized sputtered atoms prefer to get oriented in the (222) direction and the
particles with higher energy prefer the (400) direction.
Song and others [135] performed similar experiments in the same line of
investigation. The pressure and the target-substrate distance was varied while the
88
crystalline structure was analyzed with XRD. For a fixed distance, as the pressure was
increased the films became amorphous after a certain value. Otherwise, they were
polycrystalline. This value was higher for smaller target-substrate distances, as it is
expected. The polycrystalline films were oriented towards the (222) and (400). These
peaks were absent in the amorphous films. These results were attributed to the energy
of neutral argon ions, which bombard the growing film. These are causing re-
sputtering, if very energetic, or enhancing the surface migration of sputtered species
and thus improving the crystallinity of the film, if they have average energy. Not all
the pollycrystalline films showed good conductivity. Only for certain window in the
pressure values the electrical conductivity showed a maximum. The more conductive
films had also the bigger grain size crystals. The estimated energy of the argon
neutrals, calculated by the Meyer formula [136] , in order to get the optimum
crystallinity was found to be 37.8 eV. Bigger energies will result in damaging the
growing film instead of aiding the surface migration, to obtain films with higher
crystallinity. These results were corroborated by studies of the same group on the
effect of using different sputtering gas [137]. Two gases were chosen xenon and
helium. Xenon has bigger mass than argon, and helium smaller. So, the virtual source
was moved closer or further away from the substrate respectively compared with
argon. Based on the assumption that the sputtered and gas particles suffer hard sphere
collisions, a model was build to explain the results [57, 126]. According to this model
for Xe, Ar and He gases, the sputtered ions have to suffer 5.4, 7.2 and 46 collisions in
order to be thermalised.
Shigesato et al compared the XRD data for e-beam evaporation and dc magnetron
sputtering and found that the first films showed (222), preferred orientation and the
later (400) [138]. This is in accordance with the results of Kumar and Mansingh
where less energetic species crystallize along (222). The (400) is predominant in
sputtered films because the grains at this direction show more durability than (222) to
re-sputtering [139]. Other works showed enhanced (222) direction [140, 141].
Another difference between evaporated and sputtered films is the creation of sub-
grains inside bigger grain regions called domains in the latter [142, 143]. It is not clear
how these sub-grains influence the electrical properties, but it seems not as much as
the domains [143].
Variation of the annealing temperature and the substrate temperature were also
studied regarding their influence on the conductivity. The general rule is that the
conductivity of amorphous films is increased if subsequently are annealed at high
temperatures. Various temperatures were used at various lengths of time [144-146].
When annealed, amorphous deposited ITO crystallizes along (440) orientation.
Usually the conductivity deteriorates with annealing if a certain temperature is
exceeded. The increase in conductivity is dramatic if the films have been grown in
room temperature rather than at an elevated temperature. All the above refer to
thermal annealing treatments. If the annealing temperature is high Na and K from the
glass substrate will diffuse into the thin film and will neutralize the electrons by
creating traps. If the diffusion is extensive increase in resistivity will result.
Laser irradiation can produce similar results by annihilating dislocations and
promoting grain growth [183]. However, laser treatment of ITO by our research group
in the laser facilities of Appleton Rutherford Laboratory failed to produce any
improvements. On the contrary the treated ITO was peeled off from the wafer, or
vaporised after the treatment [184].
The substrate temperature is another important factor that determines the conductivity
of the ITO films [147, 148]. For films grown at substrate temperature of 100 C,
89
mainly (222) orientation is present, with little indication of the (400) plane. At
substrate temperatures above 200 C, the intensity of the (400) peak increases rapidly
and at temperature greater than 300 C, exceeds that of (222) [148]. Films grown by
electron cyclotron resonance were an exemption to the above statement. Films
deposited at 100C exhibited the (400) orientation and those deposited at 400C, the
(400) was reduced and the (222) appeared [75].
As already discussed, the oxygen flow-rate and deposition rate, play crucial roles in
determining the properties of reactively sputtered ITO films [149-152]. For the
production of low resistance ITO films, one requires a low deposition rate/oxygen
flow rate ratio [149] in DC magnetron sputtering. When the power to the sputtering
target was increased in order to increase the rate of deposition, the oxygen partial
pressure was observed to fall to zero. The stoichiometry of the films produced can
only be produced by balancing the oxygen input rate against the sputtering rate of the
metal. For mass production of reproducible quality of ITO films, the required oxygen
rate is very critical. Low sheet resistance combined with high transparency occurs for
a small range of oxygen partial pressures. This is particularly true for films grown at
low substrate temperature (<100 C).
The thickness of the films is another important parameter [153, 154] that affects the
conductivity. A decrease in resistivity with increasing film thickness is often observed
[169-173]. However, the described behaviour of the free carrier concentration and
carrier mobility in relationship to the film thickness is not constant in the literature.
The resistivity decreases as the film thickness increases sometimes due to monotonic
increase in the carrier density [154]. Jan and Lee [171] on the other hand observe a
decrease in carrier concentration and an increase in mobility. Vossen and Poliniak
[155] found films deposited to a thickness less than 100nm to be quite unstable.
Others [152, 153] found that the films resistivity drops significantly with thickness but
almost stabilizes after 100 to 270 nm. If the deposition time is increased, there is a
considerable reduction in transmittance ( around 20%) which can be attributed to the
rougher surface, small grains and micropores in the film If the deposition rate is
increased, there is a considerable reduction in transmittance ( around 20%) which can
be attributed to the rougher surface, small grains and micropores in the film [152].
There is also a concomitant increase in resistivity which can be attributed to surface
roughness and internal film stress [152]. The refractive index can be used to assess the
film density and stoichiometry. The films showed an increase in refractive index with
deposition time and attain the highest value (2.3). Increasing the deposition still
further results in index reduction, owing to film degradation and internal stress. Argon
partial pressure (Ar
pp
) has been found to play an important role in affecting the
internal stress of the film. If Ar
pp
is small (1mTorr) the compressive stress and the
resistivity are high because the structure is more densely packed. Increasing the Ar
pp
a
decrease occurs in both the stress and resistivity. Increasing further the Ar
pp
the
particles arriving at the substrate have lower energy leading to a more porous film
[156, 157]. Consequently both stress and resistivity increase and the refractive index
decreases [152].
The deposition rate is also affected by the oxygen partial pressure [158]. The decrease
in effective sputtering yield due to change of plasma ions from Argon (Ar) to Oxygen
(O) is the main reason for this. Oxygen has smaller mass than Argon and is inefficient
when bombarding the target. Another result of increased O content is that the
thermalisation length becomes smaller and due to the diffused nature of the sputtered
species the film thickness is more uniform across the substrate. This does not happen
when sputtering takes place in pure Ar [158]. However, when only argon is used as a
90
sputtering gas the oxygen content in the films changes with thickness [159]. This
change of oxygen composition is due to the bombardement of Ar ions during
deposition. For a certain low target bias the oxygen composition did not change. As
we have seen the target bias is a very important parameter in developing ITO films of
good quality. This is particularly true for both DC and RF magnetron sputtering.
Regarding the uniformity of the film thickness across the substrate, the position
directly opposite the target has better crystalline structure and composition than the
place at the edge [160].
As will be explained in the next section on the electrical properties of TCOs
amorphous films prepared by sputtering have higher resistivity than films that are
polycrystalline. For this reason Sun et al [161] applied a buffer layer of insulating
ZnO that shows good crystalline quality when grown directly on glass instead of ITO.
Next conductive ITO was grown on top of ITO. With this method the conductivity of
their ITO has shown a remarkable increase of 50%. Incidentally this ITO was
crystallized in only the (222) direction. Without the buffer layer the (222) and (400)
directions were observed. It is not certain if this decrease will show when the growth
takes place at room temperature. These results were obtained for growth at 300C.
Usually, better quality films result when the substrate temperature is high because the
stress value decreases monotonically [162]. The reason is that the lattice constant
approaches the standard value of powder form.
Another method of obtaining high quality crystalline ITO is by growing the material
on crystal substrates like yttria stabilised zirconia (YSZ) ones [163, 164]. When YSZ
was used the ITO showed only a (400) orientation. The resultant films were not any
better than those grown on standard glass, regarding conductivity.
Using these gases in the mixture of sputtering gas, or even annealing in reducing gas
like hydrogen or water vapour [141, 174, 175], has also been tried in order to get films
with lower resistivity [141, 165-168].
When ITO was deposited by introducing water or hydrogen in the gas lower
resistance was achieved when the partial pressures of the reducing gases did not
exceed a certain value. These films showed an enhanced (222) preferential
orientation. Zhang et al [168] estimated also the lattice constants of these films from
XRD data. It was observed that the lattice constant is smaller when hydrogen is
added to the mixture, which is a sign of reduced stress, as was mentioned above.
The lattice parameters for cubic systems as that of ITO can be calculated from the
following equations:
n d sin 2
) ( l k h
d
+ +
) cos (
r
where is the angle of reflection, is the wavelength of Cu-K
a
radiation used in the
XRD measurement equipment, d is the distance of the planes, n is the order of
interference, h, k, l are the Miller indices, is the lattice constant, is the half-peak
width and r is the size of crystallites.
The last equation is called the Laue-Scherrer formula and is used to calculate the
average grain size.
Harding and Window [166] demonstrated that reproducible quality ITO films can be
deposited over a wide range of oxygen partial pressures in the case of metal targets, if
91
hydrogen is added to the sputtering gas. This facilitates mass production because the
process window is broadened.
Regarding annealing in forming atmosphere whenever the films were heated in
hydrogen or inert gas the resistivity kept dropping with temperature [175].
One possibility for the further improvement of the conductivity of is to use the multi-
layer system of ITO-metal-ITO. The transparency in the visible spectral range of
such multi-layers is comparable to that of ITO films of the same thickness, while the
sheet resistance decreases to about a quarter of the ITO value. Silver is used as the
thin metal sheet sandwiched by ITO [176-179]. Thin metal films of equal conductivity
reflect light because they have to be of a certain thickness so as a continuous film is
formed, instead of isolated islands. Additionally, metal films suffer from corrosion in
wet atmospheric conditions.
The usual thickness of silver is about 10nm in the multi-layer structures. With 30nm
silver layer the sheet resistance dropped to 1/ , and the transparency was 50 %
[178]. When 10nm silver was used the sheet resistance was decreased by 80% from
22.6 to 4.7 / , while the transparency was around 88% [178]. Both the ITO and the
silver layers were prepared by DC magnetron sputtering.
Although the ITO is produced from doping the intrinsic indium oxide by tin,
additional dopant atoms can be used. These can be fluorine as oxygen substitute
[180], or silver in the place of indium [181].
In the case of silver a small amount of 1% lowers the conductivity by almost 30%. At
a substrate temperature of 250 C and 0.6 at % silver resistivity of 2.0x10
-4
cm was
obtained. These small quantities of added silver did not affect the lattice constant.
Improvements on the density of the ITO sputtering target has resulted in high
conductivity when the DC magnetron sputtering process was used [182, 187]. In the
first study [182] the resistivities of the three thin film were obtained at 0.1% O/Ar for
three targets with different densities. For a 99% target the resistivity was 1.49x10
-4
cm, for 97% target was 1.59x10
-4
cm (an improvement of 6.7%), and for 90%
target was 1.61x10
-4
cm (an improvement of 8%). No structural differences were
observed between the different films in spite of the resistivity change. The dominant
orientation for all films was the (222) [182].
Generally, whatever has been said above for ITO holds true for the ZnO thin films.
The undoped ZnO films are always unstable, irrespective of the growth process. For
this reason ZnO is doped with impurities that take the place of Zn like, Indium (In),
Gallium (Ga), Aluminium (Al), Tin (Sn), Sc, Yttrium (Y,); and of Oxygen (O) like,
Florine (F), Clorine (Cl), B. This metals, when substitute Zn in the crystal lattice, act
as donors, thus changing the carrier density of the material. The most successful and
most widely used is ZnO:Al. The Al content of this TCO is about 2-4% weight.
Compared to ITO, doped ZnO has higher stability against temperature and hydrogen
plasma. It is cheaper material to manufacture, and non-toxic. Zinc is 1300 times more
abundant on earths crust than In , and because of it is stability it is preferred over ITO
as an electrode in solar cells.
As above, reactive or non-reactive sputtering of metallic or oxide targets is used.
When metallic targets are used all the afore-mentioned problems of the stability of the
target are encountered. In order to have the largest deposition rate, suitable for
industrial uses, the flow of oxygen must be kept steady inside a small window of
values. However, experiments have shown that it is possible to obtain high quality of
films in metallic mode of the target if the power density is increased [188, 189]. In
this case fine control of the partial pressure of oxygen is not necessary because of
92
higher consumption of the gas. If the partial pressure of oxygen is less than the one
allowed by the process window, the deposited film will be rich in metallic zinc but
will have high resistivity and be semi-transparent. This is because the metallic zinc
will be un-oxidised, surrounded by oxidised phases [189].. Lack of oxygen leads to
low optical transmittance, coloration, cracking and peeling. If higher oxygen
concentration is present again the films will be resistive. This is because the excess
oxygen will inhibit the grain growth by segregating at the grain boundaries in the
form of aluminium oxide [189-193]. Oxygen has stronger affinity to aluminium than
zinc and zinc can be re-sputter easier because of its lower melting point
If an oxide target is used the deposition rate is more controllable, and the process can
result in lower conductivity films if the deposition is slow [194, 195]. This is because
the surface of the growing ZnO is chemically active to the presence of oxygen, which
diffuses more easily with higher deposition rates [194]. The process is called
chemisorption, and the oxygen atoms increase the potential barrier when absorbed at
the surfaces of the grains. As with all high rate depositions the growing film will
suffer from the bombardment of negative ions, if the target bias is high enough [196].
Usually, the resistivity reaches a minimum as the deposition rate increases, and with
further increases starts to increase [189, 193, and 197].
Ellmer et al [198] used a simultaneous excitation of the plasma by using an RF and
DC power supply. They varied the deposition rate by varying the ratio of DC to RF.
The resistivity and the deposition rate were at their lower point when 100% RF was
used. The internal stress was at its lowest point since the lattice constant difference
from its bulk value was the smallest as well [56].
Same behaviour of resistivity is observed, as expected, as the partial pressure of
oxygen is increased [189, 199]. Usually, in thin film growth the lower the deposition
rate and the higher the substrate temperature is at the start of deposition, the lattice
constant is expected to approach the value of the bulk material. As the deposition
continues and the film increases in thickness it may introduce dislocation releasing the
internal stress. In the opposite case a lot of different grains with diverse orientations
will form a mosaic structure instead of a uniform one [194]. This happens at higher
deposition rates and lower substrate temperatures with concomitant increase in
resistivity. Igasaki and Saito [194] grew ZnO:Al in a quartz crystal substrate that has a
similar lattice constant to test this and came to the same conclusions. In this occasion
epitaxial growth of ZnO:Al resulted in highest resistivity reported to date of 1.4x10
-4
cm.
The main crystal orientations that are examined in ZnO in correlation to its optical
and electrical properties are (100), (002), (001) and (110). Most frequently observed
among them are the first two. Especially the (002) is correlated to the electrical
properties of the films. In an XRD spectra the different orientations are recorded as
peaks at different angles of incidence of incoming radiation. When there is a mosaic
of different grains in the film the peak corresponding to the particular orientation in
the grain has low intensity and is broad. When the film is stressed the peak is shifted
from the reference value of the bulk material, for the particular orientation [200, 201].
Ellmer examined the variation of intensity and breadth of the (002) peak with
different oxygen partial pressure in DC sputtering [200]. He observed a deep at a
particular pressure in the stress and a peak in the grain size for a particular value
which, interestingly, corresponded to the lowest resistivity [200]. As it was stated
above, this correlation of grain size and maximum conductivity is not observed in ITO
growth where diverse and even conflicting statements were made.
93
The (002) is also a preferable orientation for the ZnO films used in piezoelectric
devices [202, 203]. These devices are required to have high resistivities and they are
perfect insulators. Recently, the chopping effect of a rotating substrate over the target
on an axis deviated from the center of the target was reported [204].It was showed
that a certain frequency of rotation resulted in films grown in optimal crystallinity,
(002). A modified RF magnetron sputtering system, a ZnO target, 0.11% Oxygen
partial pressure, and substrate temperature of 200C were used. This method has not
been tried in conductive films.
Recently, Tominaga et al [205] examined the effect of UV irradiation, from a
0.5Kwatt Hg lamp, on the conductivity of ZnO:Al during growth. Under UV
irradiation the film resistivity decreased by about 30% for the films deposited below
250C but above 50C. However when the substrate temperature was increased to
300C no difference in resistivity was observed, indicating that the influence of UV
light is considerably smaller than that of high substrate temperature. This result shows
that the effect of UV is not a thermal effect but a photochemical effect. The UV does
not affect the resistivity at room temperature. The resitivity keeps increasing
monotonically with increase in substrate temperature up to 300C. This trend was
assumed to happen due to re-evaporation of Zn during growth which gave rise to Zn
defects. To test this hypothesis they co-sputtered a Zn target alongside the ZnO:Al.
The resistivity of the resultant films was the lowest observed, 2x10
-4
cm, on films
grown on glass. We should add here that the used a special target configuration; the
substrate was situated outside the plasma which was created by two facing targets
[83]. One target was loaded with ZnO:Al and the other with Zn.
The following table offers the above information in more compact form so as different
preparations and treatments can be compared, in terms of the respective conductivity
of the thin films they produce.
TABLE 3
TCO Substrate
Temperature
C
Rate
A/min
Resistivity
cm
Transmission
%
Remarks Ref
.
SnO
2
RT 1800 3x10
-3
75 Ar/O, Sn target 107
SnO
2
:Sb 400 ------ 2x10
-3
80 Ar/10%O 104
In
2
O
3
----- ------ 1.3x10
-3
77 In Ar 112
In
2
O
3
300 1200 1.4x10
-4
87 O+Ar 148
In
2
O
3
450 ------ 1.8x10
-4
90 2%O+Ar 185
In
2
O
3
RT 182 7x10
-4
90 9%O+Ar 186
In
2
O
3
200 ------ 1.49x10
-4
95 0.1%O+Ar,
99% target
density
182
In
2
O
3
:Ag 250 ------ 2x10
-4
82 0.5%Ag 181
In
2
O
3
:Ag RT ------ 4x10
-4
82 0.5%Ag 181
ITO 300 ------ 1.4x10
-4
High ZnObuffer,Ar+
O,
Reduction by
2%
161
ITO 200 ------ 1.33x10
-4
92 Microwave
plasma
76
ITO 400-550 Big 0.1 100 Atmospheric
RF
84
ITO RT 100 5x10
-4
------ 30 MHz, 98%
target density
82
94
ITO 255 1100 1.6x10
-4
89 Dual DC,oxide
targ
68
ITO 255 1100 2.3x10
-4
89 Dual MF,oxide
targ
68
ITO 300 ------ 2.7x10
-4
89 Ar+H,oxide
target
168
ITO 400 ------ 1.46x10
-4
------ DC Mg 154
ITO RT 16200 2.5x10
-4
89 Cluster
dep,25/
88
ITO RT ------ 5x10
-4
------ Ar+H
2
O,Anneal
in N
2
at 600C
141
ITO RT ------ 4.7 / 84 300C anneal,
10nm Ag
multilayer
178
ITO 400 ------ 1.4x10
-4
------ ECR 75
ITO 400 ------ 1.3x10
-4
87 Unbalanced DC
M
70
In
2
O
3
:F 80 ------ 6.5x10
-4
80 Rf sputter only 180
ZnO:Al 300 ------ 4.2x10
-4
------ DC Magnetron 206
ZnO:Al RT ------ 7.7x10
-4
ZnO:Al RT ------ 6.5x10
-4
------ RF Magnetron 208
ZnO:Al 270 ------ 2.7x10
-4
ZnO:Al 250 ------ 1.9x10
-4
ZnO:Al 150 ------ 4.7x10
-4
------ RF magnetron 211
ZnO:Al RT ------ 4.5x10
-4
85 DC Magnetron 189
ZnO:Al 250 ------ 2x10
-4
85 RF +excessZn 201
ZnO:Al 200 ------ 1.4x10
-4
85 Epitaxial on
quartz
194
ZnO:Al RT ------ 2x10
-4
85 RFMS+Anneal
at 400C
199
ZnO:Sc 200 ------ 3.1x10
-4
85 RF Magnetron 212
ZnO:Ga RT ------ 5.9x10
-4
ZnO:In 250 ------ 7x10
-4
85 RF Magnetron 213
Zn
2
In
2
O
5
------ 3x10
-4
------ RF Magnetron 214
In-House Deposition of ITO
At the Department of Electrical Engineering in NTU we have an optoelectronics lab
equipped with a new clean room (grade 10) which is a controlled temperature and
humidity area and is divided into three parts. The clean room consists of a UV
shielded area for photolithographic processing, an area for optical and electrical
characterisation of devices, and working areas devoted to different growing systems.
The lab is equipped with 5 working sputtering systems for growing different
materials. The systems are all-stainless steel made, capable of achieving very high
vacuum (less than 10
-7
mTorr). There are also, two more systems that can be used for
sputtering and electron beam deposition, currently not in use. Three of the sputtering
systems are loaded with 4, 3 and 1magnetron electrodes, respectively. One of the rest
two systems is allocated to etching purposes and the other is an evaporation system.
All magnetron electrodes are RF powered by 5 power supplies equipped with
automatic matching units. The main research in our group is concentrated in
producing new generation electroluminescent devices.
95
The clean room is equipped with a photoresist spinner and a UV exposition machine.
Two furnaces and an asher are also in use as part of a standard photolithographic
process. Fig 1 shows the photoresist spinner, and Fig 2 the UV exposurer.
The ITO development project initially started with the aim to develop transparent and
conductive conductors that can be used in electroluminescent devices as top
electrodes.
The ITO is grown in 100mm glass wafers using RF magnetron sputtering at 280C for
50min. The lowest conductivity we have ever achieved was 1.23 / which at
transparency 90% and thickness of 8000, translates to 9.84x10
-5
cm. We have to
add that this film was stressed but it was particularly resistant to enviromental factors.
In the next step photoresist is applied followed by baking and UV exposure to define
the FSS pattern. After more baking developing of the pattern follows and then etching
to define the pattern.
Figure 1, Photoresist spinner used at NTU.
Figure 2, UV exposition system used at NTU.
Ion-assisted deposition techniques
These are similar to a sputtering process with the main difference being that the
region between the anode and the cathode is field free. As in sputtering gas ions are
used to eject forcibly the atoms of the target material, which subsequently are been
deposited onto the substrate. The main difference is that the ions in sputtering are less
energetic.
96
It is acknowledged that the structural, electrical and optical properties of thin films
depend mainly on the energies of the deposition species. In thermal evaporation the
source material atoms have energies less than 1eV. Although in sputtering these
energies reach 10eV, the structure and quality of TCOs is improved even further if
ions of higher energy are used. Unlike conventional sputtering, ion beam deposition
involves minimal intrinsic heating of the substrate due to electron bombardment. This
is particularly convenient when the nature of substrate limits the maximum allowable
deposition temperature. The deposition energies in these processes are of a few
hundred eV.
The ion-assisted deposition techniques are broadly divided into (i) ion-beam
deposition and (ii) ion plating.
Ion beam deposition
Depending on the nature of the gas ions i.e. their being reactive or non-reactive the
ion beam deposition can be further categorised as ion beam sputtering or ion beam
evaporation.
In ion beam sputtering an ion source (such as a Kaufman source) is used to generate
highly energetic ions that are directed towards a target. The energy of these ions can
be anything up to 1000-1500eV. The ions are usually incident on the target at an angle
of 45deg to maximize yield.
In the case of ion evaporation, while thermal energy is used to evaporate the material
(electron bombardment or Joule heating) an ion beam of reactive gas ions is directed
towards the substrate and reaction of the two species takes place at the substrate.
A hybrid of the two methods can be used to successfully deposit TCOs. In this case
the target material is ejected with a beam of non-reactive gas ions while at the same
time a beam of reactive gas ions is aimed at the substrate.
Ion beam plating
As before ion beam plating can be used in evaporative or sputtered mode. In both
cases the deposition species are ionized after leaving the target. For the first method
the chamber is filled with inert gas atoms and a DC bias voltage is applied to the
substrate in order to create a plasma between the substrate electrode and a another
electrode situated closely. Sometimes only the substrate is biased. The plasma is
enhanced by the incorporation of a hot filament for the creation of extra electrons. For
the evaporation of materials an electron beam is usually used.
In the sputtering mode, in addition to the DC power supply connected to the cathode
and which starts up the plasma, there is an extra RF power supply connected to the
substrate. In both cases the deposition energies are significantly enhanced by
continuously bombarding the substrate and growing films with energetic particles.
There are very few studies available on ion deposition of SnO
2
[215-217]. Only
recently [216, 217] it was possible, though to grow SnO
2
because it crystallizes during
deposition at room temperature, and does not require post-deposition treatment [215].
Unfortunately the latest studies involve only crystallographic investigations and they
do not give any data regarding respective conductivities. It was found though that in
order to get pollycrystalline SnO
2
it was necessary to bombard the growing film with
97
oxygen ions from another ion source. Higher oxygen ion energies (up to 100eV)
produced more ordered films.
There is considerable more literature on ion beam deposition techniques on indium
oxide and ITO.
Ion assisted deposition by means of a cluster ion source can be considered as a variant
of evaporation since the metal species are created by a standard evaporation source.
This method has been used to form transparent and conductive indium oxide [218].
The deposition system consists of a low vacuum chamber where the evaporation
source and the substrate holders are situated. The evaporation source was a carbon
crucible, and the substrate holder was capable of holding six silicon size substrates in
hexagonal configuration. When two evaporation sources are used ITO can also be
deposited. Helium and oxygen gas were mixed and cooled by liquid nitrogen before a
fine spray was passed through an ionising source. Thus, cluster ions of average size of
2000 were formed and accelerated to 10KeV, or to 5eV per atom. As a result, the
interactions between the cluster ions and substrate atoms occur near the surface region
at relatively low deposition rate (60 A/min). Furthermore, the irradiation of low
energy ions at high densities in very localized regions is able to produce low damage
films and smooth surface. The cluster ion method is a non-critical process because the
properties of the films do not depend on the deposition rate. It also produces films
with the lowest resistivity value compared with other methods that need extra post-
annealing. So, these films are suitable for opto-electronic applications such as liquid
crystal displays and solar cells [219-221]. There are not many publications on original
ion sputtering [222-229]. These studies are involved mostly in explaining the physical
mechanisms behind the behaviour of indium oxide and ITO. The TCOs that have been
produced by these groups are very good conductors showing very high transparency
and they were deposited at very low temperatures (<100C [223, 224] or at room
temperature [225-229]).
The films deposited at room temperature are highly amorphous [225-229], as revealed
by x-ray and electron diffraction studies. Although amorphous the transparency and
conductivity is equivalent to these polycrystalline TCOs produced at elevated
temperatures. More on the nature of conduction of these films will be discussed in the
next section on electrical characterization and electrical properties of TCOs.As it was
noted in the section on evaporation technique, ion beams can be used in conjunction
with an evaporation source. The evaporation of the target material is done by thermal
means (in a heated crucible) or by an electron beam, in a controlled environment
[230-233]. If inert Ar ions are used to bombard the growing substrate [230] reactive
gas must be present to provide for the oxygen atoms. If on the other hand oxygen (O)
ions are emitted from the ion source, the deposition can take place in vacuum [231-
232]. Usually, the energy, angle of incidence, flux of ions,[231-232] and the pressure
of the reactive gas are varied to control the properties of the film. Crystallographic
showed that the (222) orientation becomes prominent as the energy of oxygen ions is
increased [232]. (222) has the lowest intensity when the material is simply evaporated
with no ions present. At the same time the resistivity does not show much change
from its evaporated value for ions up to 60 eV. However, the evaporated films were
unsuitable for transparent conductors, as their transparency was only 40%. Films
deposited by ion assistance reached 80% with concomitant improvement of surface
roughness and increase in (400) orientation. Arch discharge ion plating was used by
Suzuki Y et al [234] to deposit very good TCOs on glass. Unfortunately we could not
find more information about this technique which was probably invented in Japan
[235]. Typical ion plating deposition of ZnO:Al is presented in [236].The following
98
table summarizes the results discussed so far for the ion assisted deposition
techniques.
TABLE 4
TCO Substrate
Temperature
C
Rate
A/min
Resistivity
cm
Transmission
%
Remarks Ref.
In
2
O
3
100 60 5x10
-4
80 O cluster 218
In
2
O
3
RT 60 5x10
-4
90 Amorphous 224
ITO 80 200 5.5x10
-4
80 Amorphous 222
ITO RT 36 5.2x10
-4
90 Amorphous 232
ITO RT 60-210 4.4x10
-4
90 Ar bombardement 231
ITO 200 ------ 1.2x10
-4
85 Arc discharg ion
plat
234
ZnO:Al 300 ------ 1x10
-3
------- Ion plating 236
Spray pyrolysis
Spray pyrolysis is one of the relatively simple and cheap methods and can easily be
adopted for mass production of large area coatings. It is based on the pyrolytic
decomposition of a metallic compound dissolved in a liquid mixture when it is
sprayed onto a preheated substrate. For the deposition of TCOs a metal chloride is
hydrolised when in conduct with the heated substrate with the production of the metal
oxide and hydrochloric acid. A spray nozzle is used to spray the carrier gas and the
solution onto the substrate that is held at constant temperature by a control circuit. The
pressure and the flow rate of the atomised solution are kept constant. This method can
be easily used for spraying large area substrates by scanning the nozzle over the
intended area.
In general substrate temperatures greater than 400C should be used so polycrystalline
film should be formed. As we mentioned above partial oxidation of the metals lead to
the increased conductivity of the oxides. So, it is necessary to include in the atomized
solution a reducing agent such as propanol, ethyl alcohol or pyroganoll. The
decomposition products of these organic materials lead to the reduction of the TCO
resulting in conductivity enhancing vacancies.
Although spray pyrolysis is the cheapest method for the production of TCOs and has
given among the lowest of conductivities, it suffers from poor reproducibility, poor
homogeneity and quick deterioration of the films.
Attempts have been made to rectify these problems by making the size of the droplets
in the atomised solution more uniform, since this size is a critical parameter in
deciding the homogeneity of the films.
More control over the properties of the films is achieved by employing an ultrasonic
vaporizer, so the variation in the diameter of the droplets is easily controlled just by
varying the ultrasonic frequency. According to a general formula the diameter is
inversely proportional to the frequency.
For large area coatings a complex electromechanical system for controlling the flow
rate, the temperature of the substrate and the movements of the nozzle and the
substrate. Unfortunately the low deposition efficiency of the spray pyrolysis has an
adverse effect on the production costs. To enhance the deposition of the droplets an
electric field is used for electrophoretic transportation. A discharge arc is used to
charge the droplets.
99
Electroless chemical growth technique.
In this process, the substrate is immersed in an aqueous solution of metal chloride.
Solid phases of metal chloride or metal hydrous oxide are formed, which on heating
yield the metal oxide. The important parameters, which control the deposition
process, are the composition of the initial solution and its pH value. The pH value of
the solution controls the ultimate thickness in the films, the lower the pH value, the
higher is the film thickness.
Sol-gel technique
In this technique the substrates are inserted into a solution containing hydrolysable
organometallic compounds and then pulled out at a constant speed into an atmosphere
containing water vapour. In this atmosphere, hydrolysis and condensation processes
take place. Water and carbon groups are removed by baking at temperatures of 500C
and TCO films are thus obtained.
The conductivity of these films is generally low (1-10 cm) but the production cost is
low.
Laser-assisted deposition techniques
When high radiation energy flux is absorbed by the target material part of the surface
vaporises and a plume of particulates of the target material is formed which
propagates towards the substrate where it gets deposited. There are three types of
absorption: (i) below the bandgap (ii) free electron and (iii) plume absorption. The
first type is characteristic of dielectric materials and the second mainly occurs in
metals whwere there are more free electrons than the dielectrics. Ultraviolet laser
light is used which is pulsed to the effect that there is not forcible and incongruent
evaporation of the material,or splashing, as it is generally called. The solid-light
interaction in this enviroment is very complex and a definitive model there is not as
yet developed. . The ablation can take place in reactive or inert gas enviroment or
even in vacuum.
The main advantage of this method is that it can be used to grow highly oriented films
at low substrate temperatures. Typical values of resistivity are around 10
-3
ohm cm
when the substrate is kept at room temperature. The ejected particles have energies
more than 1000 eV that makes the structure of the film well oriented.
At the moment this method is only used for experimental purposes and it has not been
applied to industry yet. The presence of splashing which introduces particulates in the
films has been a major problem for the large-scale introduction of pulsed laser
deposition.
As in the other techniques described before there are deferent variants of laser
ablation that use mixed methods. For example in ion-beam assisted laser deposition
the substrate is biased to enhance the energy of the impending ions or decelerate
unwanted ionic species. Additionally, a filament or an ion source can be employed as
external sources of electrons or ions.
Alternatively to a single laser beam an extra laser source can be used either to
selectively separate the heavy particulates from the light ion evaporants that get
deposited, or to vaporise them when are in flight.
100
Anodisation
This is a simple and efficient method for converting metals into their oxides. However
partial success has been achieved for tin and indium oxides. The metal to be oxydised
is used as an anode dipped into an electrolyte. When a field is applied across oxygen
atoms are attracted towards the anode where they react with the metal to form an
oxide. The rate of film growth depends on the temperature and the kind of the
electrolyte used. It should be mentioned that it is not possible to grow films of large
thickness using this technique.
Commercially Available Sources of TCOs
The following web addresses give some manufactures of transparent conductive
oxides worldwide (up to 31 Dec. 2000).
http://mfgshop.sandia.gov/1400_ext/1400_ext_Coatings.htm
http://www.the-infoshop.com/study/ti3328_conductive_polymers.html
http://www.thomasregister.com/olc/evapcoatings/trdata3.htm
http://www.ocioptics.com/ito.html
http://www.thinfilm-coating.com/English/Capabilities.html
http://www.sierratherm.com/prod5500.htm
http://www.matsci.com/SpecialtyFilm.htm
Concluding Remarks
Various deposition techniques that can be employed to grow TCOs have been
described above. The properties of the resultant films depend markedly on the
deposition parameters and the intrinsic characteristics of each technique. A broad
comparison of the different techniques is summarized in the following table[240]. The
particular characteristics of the TCO films, which are produced by each technique and
by different research groups, have been discussed in the presenting text in some detail.
TABLE 5
deposition
technique
substrate
temperature
Growth
rate
uniformity reproducibility Cost conductivity transmission
CVD High High High High moderate Moderate-
Excellent
Moderate-
Excellent
Spray High High Poor Moderate Low Moderate-
Excellent
Moderate-
Excellent
Sputtering Low Low Excellent Excellent High Excellent Excellent
Ion plating RT Low Excellent Excellent High Excellent Excellent
evaporation High High Moderate Moderate Moderate Moderate-
Excellent
Moderate
Spray pyrolysis is used for mass production of low-cost films where uniformity is
not important
The ion assisted techniques are used to deposit on plastic substrates where the
deposition temperature cannot be high
CVD and sputtering have been used extensively for mass production of films in
different variations when reproducibility is a requirement. Sputtering, although
more complex and more expensive, is preferred as it permits better control of
composition and thickness
101
The other techniques like, evaporation, laser deposition, dip coating are used
mainly by research groups for academic purposes only.
Among the different TCOs that have been described ITO has received a lot of
attention and a lot of research have been contacted in order to get the best possible
material. Recent trends suggest that ZnO:Al is of equal value to ITO and can be used
as alternative to ITO in the future. It can achieve equal conductivity and at better
transparency. Recently SnO
2
:F is gaining a lot of attention which is considered a
difficult material to produce on wide surfaces. However, it has to be added SnO
2
is
severely sensitive to the crystallinity and the stoichiometry of the film, which depends
highly on deposition techniques and post-treatment.
Electrical Properties
In the absence of an electric field, the electrons in a semiconductor, or the electron gas
as it is commonly called, are in a equilibrium state, which is established as the result
of interaction of electrons with the lattice defects. Such defects are lattice
imperfections, thermal vibrations of the atoms of the lattice and impurrity atoms.
When an electric field is applied the electrons flow in the direction of J according to
Ohms law,
E j
(1)
where c is the electrical conductivity of the material. is the reciprocal of c and is
known as the resistivity.
For a rectangular shaped sample the resistance R is given by:
)] bt /( l [ R
(2)
where l is the length, b is the width and t is the thickness of the sample. For l=b we
have:
s
R t / R
(3)
The quantity R
s
is known as the sheet resistance and it is the resistance of one square
of the film and is independent of the size of the square. It is expressed in ohms/square.
The most commonly used method for measuring the sheet resistance is the four-point
probe method. In this method, four probes are touching the material in four places
aligned next to each other. A current is made to pass through the first and last probes
and the voltage drop between the two middle probes is measured with a multi-meter.
When the probes are placed on a material of semi-infinite volume at equal distances
apart, the resistivity is given by:
I / ) dV ( 2
(4)
If the material is in the form of an infinitely thin film resting on an insulating support
this equation becomes:
102
I / V . R t /
s
53 4
(5)
Under the influence of an electric field, the electrons begin to move in a specific
direction, and this movement is called drift. The average velocity of the electron gas is
known as the drift velocity (v
d
).
If N is the number density of electrons, the current density is given by:
d
Nev J
(6)
where e is the electron charge.
Combining eq 1 and 6 we get for the drift velocity:
E Ne v
d
) / (
(7)
Here the proportionality factor is called the mobility of charge carriers and is equal
to:
Ne /
(8)
The mobility of the electrons is related to the effective mass of the charge carriers
(m
eff
)

and the relaxation time (), which is the average time the electron is moving
before its velocity is changed by a collision, according to:
eff
m e /
(9)
The average distance that the electron travels, between scattering events, in time is
called the mean free path ().
It is often necessary to determine whether the sample is n-type or p-type. The
conductivity measurement does not give this information since it cannot distinguish
between hole and electron conduction. A Hall effect study is usually required to
distinguish between the two types of carriers. It also allows determination of the
density of charge carriers.
When a current is passed through a slab of material in the presence of a transverse
magnetic field, a small potential difference, known as the Hall voltage, is developed
in a direction perpendicular to both the current and the magnetic field. Mathematically
this voltage is given by:
) / ( t B I R V
H H

(10)
Where V
H
is the Hall voltage, B is the magnetic field and I is the current through the
sample. R
H
is the Hall coefficient and is related to the carrier density according to the
relation:
) / 1 ( Ne r R
H H

(11)
103
where r
H
is the Hall scattering factor. The value of r
H
depends on the geometry of the
scattering surface and the mechanism by which the carriers are scattered. In general,
though, r
H
does not depart much from unity.
For an n-type semiconductor R
H
is negative, and for a p-type semiconductor is
positive. The mobility of the carries in a semiconductor can be calculated from
conductivity and Hall effect measurements.
From equations 9 and 11 we get:

H
R
The value of mobility determined with the previous method is called the Hall mobility
(
H
).
In the case of thin films, the conductivity is greatly influenced by the thickness of the
films. The surface
Of a thin film affects the conduction of the carriers by interrupting the transit along
their mean free path.
After a collision, they might loose all or part of their energy so they will diffuse
without memory of their previous velocity, or they might change momentum with
their energy been unaffected. In the first case they are diffusely scattered and in the
second they are reflected. Any surface that can cause diffusion will result in decrease
in the conductivity of the films.
In addition to size effects, the different lattice impurities and the enormous number of
structural defects in films also affect the conductivity. The mobility, relaxation time,
drift velocity and the mean free path, all depend on the mechanisms by which the
carriers are scattered.
These are in brief:
Lattice scattering
In addition to the various stationary (surface) imperfections, lattice vibrations also
distort the perfect periodicity of the lattice. The degree of distortion is a strong
function of temperature. There are two kinds of lattice vibrations, acoustical and
optical. Lattice scattering in general is discussed in terms of deformation potentials.
When an acoustic wave propagates in a crystal lattice, the atoms oscillate about their
equilibrium position. The equilibrium position is attained at absolute zero. These
oscillations are the cause of scattering of the charge carriers. The mobility for this
type of scattering is proportional to the density of the material, the sound velocity in
the material and inversely proportional to the temperature (T
3/2
).
The scattering, by the lattice may also be due to the strains produced by the lattice
vibrations. This is more pronounced when a semiconductor crystal consists of
dissimilar atoms where the bonds are partly ionic.
Th mobility in this occasion is proportional to the dielectric constant of the material
and inversely proportional to temperature (T
1/2
).
In the vibrations, which are associated with optical phonons, the neighbouring atoms
in the crystal vibrate in an opposite phase. These vibrations may produce strain called
the optical strain, which is measured in terms of the displacement of the sub-lattice of
one type of atom with respect to the sub-lattice containing the other type of atom. This
optical phonon scattering will be important when the lattice temperature is higher than
the Debye temperature (
D
).
Neutral impurity scattering
104
The scattering of carriers by a neutral impurity atom in the crystal lattice is similar to
the scattering of low energy electrons in a gas. In this case the mobility is inversely
proportional to the concentration of neutral impurities and the dielectric constant.
Ionised impurity scattering
Of all the impurities that may be present in the crystal, the ionised impurities produce
the greatest effect on the scattering of the carriers. This is because the electrostatic
field due to such impurities remains effective even at great distance. In the case of
degenerate semiconductors, as all TCOs are, the contribution of ionised scattering is
given by:
3 / 2 3 / 1
)
3
(
4

N
h
e
(12)
Where N is the concentration of ionised impurities. For non-degenerate
semiconductors the mobility is given by a more complicated equation
Electron-electron scattering
Electron-electron scattering has little influence on mobility because in this process the
total momentum of the electron gas is not changed. However, it is always combined
with another scattering mechanism, which is influenced by it. Typically, for a non-
degenerate semiconductor dominated by ionised impurity scattering, the mobility is
reduced by 60%, whereas in the case of degenerate semiconductors, there is no
reduction.
In addition to the scattering mechanisms discussed above, grain boundary scattering is
another important scattering mechanism in polycrystalline semiconductors. In
polycrystalline thin films, the conduction mechanism is dominated by the inherent
inter-crystalline boundaries (grain boundaries) rather than the intra-crystalline
characteristics. These boundaries generally contain fairly high densities of interface
states which trap free carriers from the bulk of the grain and scatter free carriers by
virtue of defects and trapped charges. Due to this space charge region band bending
occurs and charge barriers are created that impede the charge transport. The most
commonly used model is that of Petritz [237]. According to his model, the current
density is given by the relation:
E )}
kT
e
exp( e { J
b
0
(13)
Where
0
=(M/n
c
kT),
b
is the height of the potential barrier, n
c
is the number of
crystallites per unit length along the film, and M is a factor that is barrier dependent.
The grain boundary potential barrier
b
is related to N
1
and N
2
, the number of carriers
in the grain and grain boundary, respectively, by:
)
N
N
( kT
b
2
1

(14)
105
The quantity in the bracket in Petritz equation is the conductivity of charge carriers
dominated by grain boundaries (
g
). Thus the grain boundary limited mobility can be
written as:
)
kT
e
exp(
b
g

0
(15)
Seto [238] modified the pre-exponential term in equation (15) on the assumption that
(i) the current flows between the grains by thermionic emission and (ii) conduction in
the grains is much higher than through the grain boundaries. He came up with the
following equation:

)
kT
e
exp( ) kT m ( el
b / eff '
g

2 1
2
(16)
When an applied voltage across a grain is distributed between the neutral bulk grain
and the space charge region created by the grain boundaries, the mobility is the sum
of contributions from bulk as well as grain boundaries:
g bulk H

1 1 1
+
(17)
The grain boundary mechanism generally dominates in polycrystalline films with
small crystallite size.
In amorphous materials like the TCOs produced at room temperature, the hopping
process is the most dominant conduction mechanism. Conduction by hopping results
in conductivity of the form:
] )
T
T
( exp[
T
x
/
'
0
2 1
0

(18)
where the value of x depends on the nature of the hopping process. When conduction
is three dimensional, variable range hopping gives x=0.25 for a constant density of
states and x=0.5 for a parabolic density of states. In amorphous materials variable
range hopping conduction occurs at temperatures at which the phonons do not have
sufficient energy for transfer to a nearest neighbour atom. The charge carriers hop
from a neutral atom to another neutral atom situated at the same energy level, which
can be many interatomic distances away.
The principle common features of the electrical properties of the TCOs are:
All transparent conductive films are n-type semiconductors. Recently, a new kind
of transparent conductive oxide has been developed that behaves like a p-type
semiconductor.
The substrate temperature has a significant effect on the electrical properties of all
oxide films. By increasing the temperature more oxygen vacancies are created and
hence increased conductivity.
The electrical properties are influenced by the thickness variation of the oxide
films as it is expected. This may be due to increased grain size, improved
crystallinity and the presence of oxygen on the surface layer.
106
Doping of transparent conducting oxide films with suitable impurities improves
the electrical properties of these oxide films considerably. It results, generally, in
increase in carrier density and mobility. However, the upper limit of electron
density is determined by the solubility of the dopants. If excessive impurities are
added they tend to form clusters of oxides of the impurities and distort the lattice.
In addition they produce extra scattering centers
In the films that have carrier concentrations more than 10
20
cm
-3
, both the mobility
and the carrier concentration are almost independent of temperature, indicating
that the TCO is degenerate. In general when the carrier concentration is less than
10
18
cm
-3
, the conduction is always limited by grain boundary scattering. If the
carrier concentration is greater than 10
20
cm
-3
, ionised impurity scattering is the
dominant mechanism.
The properties of the films are influenced by te process of diffusion of oxygen
either into the film or out of it.
Optical Properties
If the thickness of a film is t, and its reflectance R and transmittance T measured at
normal incudence are known, it is possible to derive the optical constants i.e.
refractive index n and extinction coefficient k of the complex refractive index n
*
=n-ik.
There are different formulas for absorbing, weakly absorbing and transparent films.
Most of the TCOs fall into the second category.
For very weakly absorbing films, the measurement of transmission of light through
the film in the region of tgransparency is suffucient to determine the real and
imaginery parts of the complex refractive index n
*
=n-jk. There are a nimber of
methods developed to calculate these constatnts. Among them Manifaciers [239]
method is the most simpler to use with less computations. For an incident light of unit
amplitude the transmitted wave would have an amplitude of:

) / t in exp( r r
) t in exp( t t
A
*
*

4 1
2
2 1
2 1
+
(19)
where t
1
, t
2,
r
1
, and r
2
are the transmission and reflection coefficients of the front and
rear surfaces and are given by:
n n
n
t
+
0
0
1
2

1
2
n n
n 2
t
+
(20)
n n
n n
r
+
0
0
1
1
1
2
n n
n n
r
+
(21)
The transmission of the layer is given by:
2
0
1
A
n
n
T
(22)
In the case of weak absorption, k
2
<<(n-n
0
)
2
and k
2
<<(n-n
1
)
2
so that K is given by:
107
) / nt cos( a C C a C C
a n n n
T
4 2
16
2 1
2 2
2
2
1
2
1 0
+ +
(23)
where C
1
=(n+n
0
)(n
1
+n), C
2
=(n-n
0
)(n
1
-n), and
kt
exp a
4
(24)
The maxima and minima of T in the above equation occur for:
m
nt
4
(25)
where m is the order number in the appearance of the peaks or troughs. At these
points the extreme values are given by the following equations:
2
2 1
2
1 0
16
) a C C (
a n n n
T
max
+

2
2 1
2
1 0
16
) a C C (
a n n n
T
min
(26)
From the above equations we have for n:
2 / 1 2 / 1 2
1
2
0
2
] ) n n N ( N [ n +
(27)
where N is given by the equation:
min max
min max
1 0
2
1
2
0
T T
T T
n n 2
2
n n
N

+
+
(28)
Equation 27 shows that n is explicitly determined from T
max
, T
min
, n
1
and n
0
, measured
at the same wavelenght. Knowing n one can find the thickness of the film from the
equation, using the position of two minima or two maxima:
] ) ( n ) ( n [ 2
M
t
1 2 2 1
2 1

(29)
Where M is the number of oscillations between the two extrema. is given by the
equation:
] ) T / T ( 1 [ C
) T / T ( 1 [ C
a
2 / 1
min max 2
2 / 1
min max 1
+
(30)
Experimental and comparative results:
In evaluating transparent conducting films both the transparency and conductivity
should be taken into account. Different equations have been devised that take into
account simultaneously the performance of the TCO as a conductor and as a
transparent material. Any particular equation gives a number which is consider as a
figure of merit for the particular TCO. The following equation defined by Haacke
108
[241] is widely used for comparing different TCOs. This figure of merit is a strong
function of thickness.
S
TC
R
T
10

(31)
where T is the transmission and R
S
is the sheet resistance.
REFERENCES
[1] Muranoi T, Furukoshi M. Properties of stannic oxide thin films produced from
the SnCl
4
H
2
O and SnCl
4
H
2
O
2
reaction systems, THIN SOLID FILMS, vol.48,
no.3, pp.309-18, 1978.
[2] Grosse P, Schmitte FJ, Frank G, et al."Preparation and growth of SNO2 thin-
films and their optical and electrical-properties", THIN SOLID FILMS, vol. 90,
no. 3, pp. 309-315, 1982.
[3] Kane J, Schweizer HP, Kern W. Chemical vapor deposition of transparent,
electrically conductive tin oxide films formed from dibutyl tin diacetate, J. OF
THE ELECTROCHEMICAL SOCIETY, vol.122, no.8, 1975, pp.1144-9.
[4] Upadhyay JP, Vishwakarma SR, Prasad HC, "Studies of electrical and optical-
properties of SNO2-P films", THIN SOLID FILMS, vol. 169, no. 2, pp. 195-204,
1989.
[5] Proscia J, Gordon RG, "Properties of fluorine-doped tin oxide-films produced
by atmospheric-pressure chemical vapor-deposition from tetramethyltin,
bromotrifluoromethane and oxygen", THIN SOLID FILMS, vol. 214, no. 2, pp.
175-187, 1992.
[6] Mayer B, "Highly conductive and transparent films of tin and fluorine doped
indium oxide produced by APCVD", THIN SOLID FILMS, vol. 221, no. 1-2, pp.
166-182, 1992.
[7] Hu JH, Gordon RG, "Textured aluminum-doped zinc-oxide thin-films from
atmospheric-pressure chemical-vapor deposition", J APPL PHYS, vol. 71, no. 2,
pp. 880-890, 1992.
[8] Ataev BM, Bagamadova AM, Mamedov VV, et al, "Thermally stable, highly
conductive, and transparent ZnO layers prepared in situ by chemical vapor
deposition", MAT SCI ENG B-SOLID, vol. 65, no. 3, pp. 159-163, 1999.
[9] Wenas WW, Yamada A, Takahashi K, et al. "Electrical and optical-properties
of boron-doped ZnO thin-films for solar-cells grown by metalorganic chemical
vapor-deposition". J APPL PHYS, vol. 70, no. 11, pp. 7119-7123, 1991.
[10] Maruyama T, Fukui K, "Indium-tin oxide thin-films prepared by chemical
vapor-deposition", J APPL PHYS, vol. 70, no. 7, pp. 3848-3851, 1991.
[11] Nishino J, Kawarada T, Ohshio S, et al, "Conductive indium-doped zinc oxide
films prepared by atmospheric-pressure chemical vapour deposition", J MATER
SCI LETT vol. 16, no. 8, pp. 629-631, 1997.
[12] Gordon R, "Chemical vapor deposition of coatings on glass", J NON-CRYST
SOLIDS, vol. 218, pp. 81-91, 1997.
[13] Manifacier JC, De Murcia M, Fillard JP, Vicario E. Optical and electrical
properties of SnO
2
thin films in relation to their stoichiometric deviation and their
crystalline structure, THIN SOLID FILMS, vol.41, no.2, 1977, pp.127-35.
109
[14] Geurts J, Rau S, Richter W, et al, "SNO films and their oxidation to SNO
2
raman-scattering, ir reflectivity and x-ray-diffraction studies", THIN SOLID
FILMS, vol. 121, no. 3, pp. 217-225, 1984.
[15] Qazi IA, Akhter P, Mufti A, "On angle-dependent growth of electron-beam
vacuum-evaporated tin oxide-films", J PHYS D APPL PHYS. vol.24, no. 1, pp.
81-82, 1991.
[16] Feng T, Ghosh AK, Fishman C. Angle-of-incidence effects in electron-beam-
deposited SnO
2
Si solar cells, APPL PHYS LETT, vol.34, no.3, 1 Feb. 1979,
pp.198-9.
[17] Casey V, Stephenson MI, "A study of undoped and molybdenum doped,
polycrystalline, tin oxide thin-films produced by a simple reactive evaporation
technique", J PHYS D APPL PHYS, vol. 23, no. 9, pp. 1212-1215, 1990.
[18] Parkansky N, Berman RL, Goldsmith S, et al, "Improvement of thin-film
semiconductor conductivities using a transverse current during deposition", SURF
COAT TECH, vol. 68, pp. 320-324, 1994.
[19] Pan CA, MA TP, "Highly transparent conductive films of thermally
evaporated IN2O3", J ELECTRON MATER, vol. 10, no. 1, pp. 43-57, 1981.
[20] Pan CA, Ma TP. High-quality transparent conductive indium oxide films
prepared by thermal evaporation, APPL PHYS LETT, vol.37, no.2, 15 July 1980,
pp.163-5.
[21] Lau WS, Fonash SJ, "Highly conducting transparent undoped indium oxide-
films deposited below 100-degrees-c by activated reactive evaporation", J
ELECTRON MATER, vol. 15, no. 3, pp. 117-123, 1986.
[22] Laser D, "Properties of indium oxide-films prepared by the reactive
evaporation of indium", THIN SOLID FILMS, vol. 90, no. 3, pp. 317-321, 1982.
[23] Golan A, Bregman J, Shapira Y, et al, "Novel indium oxide n-gaas diodes",
APPL PHYS LETT, vol. 57, no. 21, pp. 2205-2207, 1990.
[24] Muranaka S, "Crystallization of amorphous in2o3 films during film growth",
JPN J APPL PHYS, vol. 230, no. 12a, pp. L2062-L2064, 1991.
[25] Lee CH, Kuo CV, Lee CL, "Effects of heat-treatment and ion doping of
indium oxide", THIN SOLID FILMS, vol. 173, no. 1, pp. 59-66, 1989.
[26] Nath P, Bunshah RF. Preparation of In
2
O
3
and tin-doped In
2
O
3
films by a
novel activated reactiveevaporation technique, THIN SOLID FILMS, vol.69,
no.1, 2 June 1980, pp.63-8.
[27] Christian KDJ, Shatynski SR, "Thin-film passive solar windows produced by
reactive evaporation of IN-SN", THIN SOLID FILMS, vol. 108, no. 3, pp. 319-
324, 1983.
[28] Yao JL, Hao S, Wilkinson JS, "Indium tin oxide-films by sequential
evaporation", THIN SOLID FILMS, vol. 189, no. 2, pp. 227-233, 1990.
[29] Agnihotry SA, Saini KK, Saxena TK, et al, "Studies on e-beam deposited
transparent conductive films of IN2O3 - SN at moderate substrate temperatures", J
PHYS D APPL PHYS, vol. 18, no. 10, pp. 2087-2096, 1985.
[30] Patel NG, Lashkari BH, "Conducting transparent indium tin oxide-films by
postdeposition annealing in different humidity environments", J MATER SCI, vol.
27, no. 11, pp. 3026-3031, 1992.
[31] Habermeier HU, "Properties of indium tin oxide thin-films prepared by
reactive evaporation", THIN SOLID FILMS, vol. 80, no. 1-3, pp. 157-160, 1981.
[32] Nath P, Bunshah RF, Basol BM, Staffsud OM. Electrical and optical
properties of In
2
O
3
:Sn films prepared byactivated reactive evaporation, THIN
SOLID FILMS, vol.72, no.3, 1980, pp.463-8.
110
[33] Krokoszinski HJ, Oesterlein R, "Postdeposition annealing effects in electron-
beam-evaporated indium tin oxide thin-films", THIN SOLID FILMS, vol. 187,
no. 1, pp. 179-186, 1990.
[34] Hjortsberg A, Hamberg I, Granqvist CG, "Transparent and heat-reflecting
indium tin oxide-films prepared by reactive electron-beam evaporation", THIN
SOLID FILMS, vol. 90, no. 3, pp. 323-326, 1982.
[35] Lee WK, Machino T, Sugihara T, "Low-pressure and temperature deposition
of transparent conductive indium tin oxide (ITO) films by the face target
sputtering (FTS) process", THIN SOLID FILMS, vol. 224, no. 1, pp. 105-111,
1993.
[36] Shigesato Y, Hayashi Y, Haranoh T, "Doping mechanisms of tin-doped
indium oxide-films", APPL PHYS LETT, vol. 61, no.1, pp. 73-75, 1992.
[37] Paine DC, Whitson T, Janiac D, et al, "A study of low temperature
crystallization of amorphous thin film indium-tin-oxide", J APPL PHYS, vol. 85,
no. 12, pp. 8445-8450, 1999.
[38] Salehi A, "The effects of deposition rate and substrate temperature of ito thin
films on electrical and optical properties", THIN SOLID FILMS, vol. 324, no. 1-
2, pp. 214-218, 1998.
[39] Ma J, Li SY, Zhao JQ, et al, "Preparation and properties of indium tin oxide
films deposited on polyester substrates by reactive evaporation", THIN SOLID
FILMS, vol. 307, no. 1-2, pp. 200-202, 1997.
[40] Thilakan P, Kumar J, "Investigations on the annealing effects on reactively
deposited ito thin films", PHYS STATUS SOLIDI A, vol. 160, no. 1, pp. 97-104,
1997.
[41] Penza M, Cozzi S, Tagliente MA, et al, "Characterization of transparent and
conductive electrodes of indium tin oxide thin films by sequential reactive
evaporation", THIN SOLID FILMS, vol. 349, no. 1-2, pp. 71-77, 1999.
[42] Taga N, Odaka H, Shigesato Y, et al, "Electrical properties of heteroepitaxial
grown tin-doped indium oxide films", J APPL PHYS, vol. 80, no.2, pp. 978-984,
1996.
[43] Alterkop B, Parkansky N, Boxman RL, et al, "Influence of a parallel electric
field on the conductivity of a growing indium oxide film", THIN SOLID FILMS,
vol. 291, pp. 10-12, 1996.
[44] Mizuhashi M. "Electrical properties of vacuum-deposited indium oxide and
indium tin oxide films", THIN SOLID FILMS, vol.70, no.1, 15 July 1980, pp.91-
100.
[45] Oyama T, Hashimoto N, Shimizu J, et al, "Low resistance indium tin oxide-
films on large-scale glass substrate", J VAC SCI TECHNOL A, vol. 10, no. 4, pp.
1682-1686, 1992.
[46] Swamy HG, Reddy PJ, "Preparation of zno films by activated reactive
evaporation", SEMICOND SCI TECH, vol. 5, no. 9, pp. 980-981, 1990.
[47] Ranson R. et al to be published.
[48] Bhagwat S, Howson RP, "Use of the magnetron-sputtering technique for the
control of the properties of indium tin oxide thin films", SURF COAT TECH, vol.
111, no. 2-3, pp. 163-171, 1999.
[49] Thin film processes, ed. Vossen JL, Kern W, Academic Press, 1978.
[50] Handbook of Thin Film technology, ed. Maissel LI, Lang RG, McGrawhill,
1970.
111
[51] Yeom GY, Thornton JA, Kushner MJ, "Cylindrical magnetron discharges .2.
the formation of dc bias in rf-driven discharge sources", J APPL PHYS, vol. 65,
no. 10, pp. 3825-3832, 1989.
[52] Ishibashi K, Hirata K, Hosokawa N, "Mass-spectrometric ion analysis in the
sputtering of oxide targets", J VAC SCI TECHNOL A, vol. 10, no. 4, pp. 1718-
1722, 1992.
[53] Tominaga K, Yuasa T, Kume M, et al, "Influence of energetic oxygen
bombardment on conductive zno films", JPN J APPL PHYS 1, vol. 24, no. 8, pp.
944-949, 1985.
[54] Tominaga K, Kataoka M, Ueda T, et al, "Preparation of conductive zno-al
films by a facing target system with a strong magnetic-field", THIN SOLID
FILMS, vol. 253, no. 1-2, pp. 9-13, 1994.
[55] Tominaga K, Kuroda K, Tada O, "Radiation effect due to energetic oxygen-
atoms on conductive al-doped zno films", JPN J APPL PHYS 1, vol. 27, no 7, pp.
1176-1180, 1988.
[56] Ellmer K, Cebulla R, Wendt R, "Characterization of a magnetron sputtering
discharge with simultaneous rf- and dc-excitation of the plasma for the deposition
of transparent and conductive zno : al-films", SURF COAT TECH, vol. 98, no. 1-
3, pp. 1251-1256, 1998.
[57] Glow discharge processes, Chapman BJ, Wiley, 1980.
[58] Brauer G, Szczyrbowski J, Teschner G, "New approaches for reactive
sputtering of dielectric materials n large scale substrates", J NON-CRYST
SOLIDS, vol. 218, pp. 19-24, 1997.
[59] Tsiogas CD, Avaritsiotis JN, "Modeling reactive sputtering process in
symmetrical planar direct-current magnetron systems", J APPL PHYS, vol. 71,
no. 10, pp. 5173-5182, 1992.
[60] Safi I, "Recent aspects concerning dc reactive magnetron sputtering of thin
films: a review", SURF COAT TECH, vol. 127, no. 2-3, pp. 203-219, 2000.
[61] Czternastek H, Brudnik A, Jachimowski M, et al, "Voltage-controlled dc
reactive magnetron sputtering of indium-doped zinc-oxide films", J PHYS D
APPL PHYS, vol. 25, no. 5, pp. 865-870, 1992.
[62] Schiller S, Beister G, Sieber W, "Reactive high-rate dc sputtering - deposition
rate, stoichiometry and features of tiox and tinx films with respect to the target
mode", THIN SOLID FILMS, vol. 111, no. 3, pp. 259-268, 1984.
[63] Maniv S, Westwood WD. "Surface oxidation kinetics of sputtering targets",
Surface Science, vol.100, 1980, pp.108-18.
[64] Berg S, Blom HO, Moradi M, et al, "Process modeling of reactive sputtering",
J VAC SCI TECHNOL A, vol. 7, no. 3, pp. 1225-1229, 1989.
[65] Maniv S, Westwood WD. Discharge characteristics for magnetron sputtering
of Al in Ar and ArO
2
mixtures, J. OF VACUUM SCIENCE & TECHNOLOGY,
vol.17, no.3, 1980, pp.743-51.
[66] Scholl RA, "Power systems for reactive sputtering of insulating films", SURF
COAT TECH, vol. 93, no. 1, pp. 7-13, 1997.
[67] Rettich T, Wiedemuth P, "High power generators for medium frequency
sputtering applications", J NON-CRYST SOLIDS, vol. 218, pp. 50-53, 1997.
[68] May C, Strumpfel J, "ITO coating by reactive magnetron sputtering-
comparison of properties from dc and mf processing", THIN SOLID FILMS, vol.
351, no. 1-2, pp. 48-52, 1999.
112
[69] Wallace G, "Design considerations for the ac/dc -magnetron deposition source
and power supply system", THIN SOLID FILMS, vol. 351, no. 1-2, pp. 21-26,
1999.
[70] Szczyrbowski J, Brauer G, Teschner G, et al, "Antireflective coatings on large
scale substrates produced by reactive twin-magnetron sputtering", J NON-CRYST
SOLIDS, vol. 218, no.25-29, 1997.
[71] Howson RP, Danson N, Safi I, "High rate reactive sputtering using gas
pulsing: a technique for the creation of films onto large, fat substrates", THIN
SOLID FILMS, vol. 351, no. 1-2, pp. 32-36, 1999.
[72] Danson N, Safi I, Hall GW, et al, "Techniques for the sputtering of optimum
indium-tin oxide films on to room-temperature substrates", SURF COAT TECH,
vol. 99, no. 1-2, pp. 147-160, 1998.
[73] Howson RP, Spencer AG, Oka K, et al, "The formation and control of direct-
current magnetron discharges for the high-rate reactive processing of thin-films", J
VAC SCI TECHNOL A, vol. 7, no.3, pp. 1230-1234, 1989.
[74] Shin SH, Shin JH, Park KJ, et al, "Low resistivity indium tin oxide films
deposited by unbalanced dc magnetron sputtering", THIN SOLID FILMS, vol.
341, no. 1-2, pp. 225-229, 1999.
[75] Asmussen J, "Electron-cyclotron resonance microwave discharges for etching
and thin-film deposition", J VAC SCI TECHNOL A, vol. 7, no. 3, pp. 883-893,
1989.
[76] Burke RR, Pomot C, "Microwave multipolar plasma for etching and
deposition", SOLID STATE TECHNOL, vol. 31, no. 2, pp. 67-71, 1988.
[77] Pichot M, Durandet A, Pelletier J, et al, "Microwave multipolar plasmas
excited by distributed electron-cyclotron resonance - concept and performance",
REV SCI INSTRUM, vol. 59, no. 7, pp. 1072-1075, 1988.
[78] Matsuoka M, Ono K, "New high-rate sputtering-type electron-cyclotron
resonance microwave plasma using an electric mirror", APPL PHYS LETT, vol.
54, no. 17, pp. 1645-1647, 1989.
[79] Kubota E, Shigesato Y, Igarashi M, et al, "Effects of magnetic-field gradient
on crystallographic properties in tin-doped indium oxide-films deposited by
electron-cyclotron-resonance plasma sputtering", JPN J APPL PHYS 1, vol. 33,
no. 9a, pp. 4997-5004, 1994.
[80] Latz R, Daube C, Haranou T, et al, "Microwave plasma assisted sputtering", J
NON-CRYST SOLIDS, vol. 218, pp. 329-334, 1997.
[81] Yang ZW, Han SH, Yang TL, et al, "Bias voltage dependence of properties
for depositing transparent conducting ito films on flexible substrate", THIN
[82] Hoshi Y, Ohki R, "Low energy rf sputtering system for the deposition of ito
thin films", ELECTROCHIM ACTA, vol. 44, no. 21-22, pp. 3927-3932, 1999.
[83] Matsuoka M, Hoshi Y, Naoe M, "Reactive synthesis of well-oriented zinc-
oxide films by means of the facing targets sputtering method", J APPL PHYS, vol.
63, no. 6, pp. 2098-2103, 1988.
[84] Lee DH, Moss RW, Vuong KD, et al, "Transparent-conductive indium tin
oxide films fabricated by atmospheric rf plasma deposition technique", THIN
SOLID FILMS, vol. 291, pp. 6-9, 1996.
[85] Williams JA, Lee DH, et al, SPIE PROC. OPT. MATER. TECHNOL., vol
2531, p333, 1995.
[86] Shen CQ, Vuong KD, et al, ADV. SYNTH. PROCCES. COMP. ADV.
CERAM., vol 56, p 315, 1995.
113
[87] Hosokawa N, "Large area deposition: sputtering- and pcvd-systems and
techniques for lcd", THIN SOLID FILMS, vol. 282, no. 1-2, pp. 136-142, 1996.
[88] Ishibashi K, Watabe K, Hosokawa N, "Large area deposition of ito films by
cluster type sputtering system", THIN SOLID FILMS, vol. 282, no. 1-2, pp. 198-
201, 1996.
[89] Ishibashi K, Watabe K, Sakurai T, et al, "Large area deposition of ito films by
cluster type sputtering system", J NON-CRYST SOLIDS, vol. 218, pp. 354-359,
1997.
[90] Odaka H, Iwata S, Taga N, et al, "Study on electronic structure and
optoelectronic properties of indium oxide by first-principles calculations", JPN J
APPL PHYS 1, vol. 36, no. 9a, pp. 5551-5554, 1997.
[91] Strumpel J, Kammer M et al in: Bakish R (Ed), PROC. 11
TH
CONF.
VACUUM WEB. COAT., p 279, 1997.
[92] De Bosscher W, Lievens H, "Advances in magnetron sputter sources", THIN
[93] Heister U, Krempel-Hesse J, Szczyrbowski J, et al, "Twinmag (tm) ii:
attempts to improve an excellent sputter tool", THIN SOLID FILMS, vol. 351, no.
1-2, pp. 27-31, 1999.
[94] De A, Ray S, "A study of the structural and electronic-properties of magnetron
sputtered tin oxide-films", J PHYS D APPL PHYS, vol. 24, no. 5, pp. 719-726,
1991.
[95] Croitoru N, Seidman A, Yassin K. "Effect of composition and structure
modification of SnO/sub x/ films on the electron secondary emission THIN
SOLID FILMS, vol.116, no.4, 1984, pp.327-39
[96] Croitoru N, Seidman A, Yassin K. "Physical properties of SnO
x
films" J. OF
APPL PHYS, vol.57, no.1, 1 Jan. 1985, pp.102-4.
[97] Hecq M, Portier E. "Chemical aspects of oxide film formation by reactive
sputtering" THIN SOLID FILMS, vol.9, no.3, 1972, pp.341-55.
[98] Tohda T, Wasa K, Hayakawa S. "The crystallographic site of cosputtered Eu
in RF-sputtered SnO
2
film", J. OF THE ELECTROCHEMICAL SOCIETY,
vol.123, no.11, 1976, pp.1719-20.
[99] Ruske M, Brauer G, Pistner J, et al, "Properties of sno2 films prepared by dc
and mf reactive sputtering", THIN SOLID FILMS, vol. 351, no. 1-2, pp. 146-150,
1999.
[100] Vaynshteyn VM, SOV. J. OPT. TECHNOL., vol 34, 1967, p 45
[101] Lehmann HW, Widmer R. "Preparation and properties of reactively co-
sputtered transparent conducting films" THIN SOLID FILMS, vol.27, no.2, 1975,
pp.359-68.
[102] Vossen JL. "Contamination in films sputtered from hot-pressed targets" J. OF
VACUUM SCIENCE & TECHNOLOGY, vol.8, no.6, 1971, pp.751-2.
[103] Sabnis AG, Moldovan AG. "Correspondence between the antimony contents
of the sputtered films and the targets", APPL PHYS LETT, vol.33, no.10, 15 Nov.
1978, pp.885-6.
[104] Suzuki K, Mizuhashi M, "Structural, electrical and optical-properties of rf-
magnetron-sputtered sno2-sb film", THIN SOLID FILMS, vol. 97, no. 2, pp. 119-
127, 1982.
[105] Vossen JL, Poliniak ES. "The properties of very thin r.f. sputtered transparent
conducting films of SnO
2
Sb and In
2
O
3
:Sn" THIN SOLID FILMS, vol.13, no.2, 15
1972, pp.281-4.
114
[106] Sabnis AG, Kuang-Yeh Chang. "Effect of substrate temperature on DC-
sputtered antimony-doped tin-dioxide films" ELECTRONICS LETTERS, vol.13,
no.4, 1977, pp.113-14.
[107] Stjerna B, Granqvist CG, "Optical and electrical-properties of snox thin-films
made by reactive rf magnetron sputtering", THIN SOLID FILMS, vol. 193, no. 1-
2, pp. 704-711, 1990.
[108] Kaganovich EB, Ovsjannikov VD, Svechnikov SV. Determination of optimal
reactive sputtering conditions for the preparation of conductive transparent indium
oxide films. THIN SOLID FILMS, vol.60, no.3, 1979, pp.335-40.
[109] Wickersham CE, Greene JE. The effect of substrate bias on the electrical and
optical properties of In
2
O
3
films grown by RF sputtering, PHYSICA STATUS
SOLIDI A, vol.47, no.1, 1978, pp.329-37
[110] Morris JE, Bishop CA, Ridge MI, Howson RP. Structural determination of
indium oxide thin films on polyester substrates by transmission electron
microscopy, THIN SOLID FILMS, vol.62, no.1, 1979, pp.19-23.
[111] Howson RP, Avaratsiotis JN, Ridge MI, Bishop CA. Properties of conducting
transparent oxide films produced by ion plating onto room-temperature
substrates, APPL PHYS LETT, vol.35, no.2, 1979, pp.161-2.
[112] Fraser DB, Cook HD. "High conductive, transparent films of sputtered In
2-
x
Sn
x
O
3-y
", .J. OF THE ELECTROCHEMICAL SOCIETY, vol.119, no.10, 1972,
pp.1368-74.
[113] Mukherjee A, "The deposition of transparent conductive oxide thin-films onto
large sheets of glass, acrylic and polycarbonate", VACUUM, vol. 39, no. 6, pp.
537-540, 1989.
[114] Bawa SS, Sharma SS, Agnihotry SA, et al, "Deposition of transparent
conducting indium tin oxide-films by dc sputtering", P SOC PHOTO-OPT INST,
vol. 428, pp. 22-28. 1983.
[115] Szczyrbowski J, Dietrich A, Hoffmann H, "Optical-properties of rf-sputtered
indium oxide-films", PHYS STATUS SOLIDI A, vol. 69, no. 1, pp. 217-226,
1982.
[116] Itoyama K. "Properties of Sn-doped indium oxide prepared by high rate and
low temperature RF sputtering", JPN J OF APPL PHYS, vol.17, no.7, 1978,
pp.1191-6.
[117] Jachimowski M, Brudnik A, Czternastek H, "Modified procedure for
deposition of ito films by dc sputtering", J PHYS D APPL PHYS, vol. 18, no. 8,
pp. L145-L148, 1985.
[118] Howson RP, Avaritsiotis JN, Ridge MI, Bishop CA. "Reactive plating of
metal oxides onto insulating substrates", THIN SOLID FILMS, vol.58, no.2,
1979, pp.379-84.
[119] Ganzorig C, Fujihira M, "Improved drive voltages of organic
electroluminescent devices with an efficient p-type aromatic diamine hole-
injection layer", APPL PHYS LETT, vol. 77, no. 25, pp. 4211-4213, 2000.
[120] Li M, Yu J, Chen ZJ, et al, "New red electroluminescent devices using tris(2,2
'-bipyridine) ruthenium (ii) hexafluorophosphate as emitter", JPN J APPL PHYS
2, vol. 39, no. 11b, pp. L1171-L1173, 2000.
[121] Sheng Z, Gan LB, Huang CH, "Photoelectric response of pyrrolidinofullerene
and bis-pyrrolidinofullerene lb films", CHEM PHYS LETT, vol. 331, no. 2-4, pp.
143-148, 2000.
115
[122] Feng W, Fujii A, Lee S, et al, "Broad spectral sensitization of organic
photovoltaic heterojunction device by perylene and c-60", J APPL PHYS, vol. 88,
no. 12, pp. 7120-7123, 2000.
[123] Lee JH, Yu HS, Kim W, et al, "Synthesis and characterization of a new green-
emitting poly(phenylenevinylene) derivative containing alkylsilylphenyl pendant",
J POLYM SCI POL CHEM, vol. 38, no. 23, pp. 4185-4193, 2000.
[124] De Morais TD, Chaput F, Boilot JP, et al, "Two-layer light emitting diodes
prepared by the sol-gel route", CR ACAD SCI IV-PHYS, vol. 1, no. 4, pp. 479-
491, 2000.
[125] ara K, Horiguchi T, Kinoshita T, et al, "Highly efficient photon-to-electron
conversion with mercurochrome-sensitized nanoporous oxide semiconductor solar
cells", SOL ENERG MAT SOL C, vol. 64, no. 2, pp. 115-134, 2000.
[126] Delahoy AE, Ruppert A, Contreras M, "Charging and discharging of defect
states in cigs/zno junctions", THIN SOLID FILMS, vol. 361, pp. 140-144, 2000.
[127] Shimizu S, Komaru T, Okawa K, et al, "Fabrication of solar cells having
sih2cl2 based i-layer materials", JPN J APPL PHYS, vol. 138, no. 12a, pp. 6617-
6623, 1999.
[128] Aperathitis E, Hatzopoulos Z, Androulidaki M, et al, "RF sputtered indium-
tin-oxide as antireflective coating for gaas solar cells", SOL ENERG MAT SOL
C, vol. 45, no. 2, pp. 161-168, 1997.
[129] Hamberg I, Hjortsberg A, Granqvist CG, "High-quality transparent heat
reflectors of reactively evaporated indium tin oxide", APPL PHYS LETT, vol. 40,
no. 5, pp. 362-364, 1982.
[130] Hjortsberg A, Hamberg I, Granqvist CG, "Transparent and heat-reflecting
indium tin oxide-films prepared by reactive electron-beam evaporation", THIN
[131] Frank G, Kauer E, Kostlin H, "Transparent heat-reflecting coatings based on
highly doped semiconductors", THIN SOLID FILMS, vol. 77, no. 1-3, pp.107-
117, 1981.
[132] Kumar CVRV, Mansingh A, "Effect of target-substrate distance on the growth
and properties of rf-sputtered indium tin oxide-films", J APPL PHYS, vol. 65, no.
3, pp. 1270-1280, 1989.
[133] Westwood WD. Calculation of deposition rates in diode sputtering systems,
Journal of Vacuum Science & Technology, vol.15, no.1, 1978, pp.1-9.
[134] Nyaiesh AR, "Target profile change during magnetron sputtering",
VACUUM, vol. 36, no. 6, pp. 307-309, 1986.
[135] Song PK, Shigesato Y, Kamei M, et al, "Electrical and structural properties of
tin-doped indium oxide films deposited by dc sputtering at room temperature",
JPN J APPL PHYS, vol. 138, no. 5a, pp. 2921-2927, 1999.
[136] Meyer k, Schuller IK, Falco CM, "Thermalization of sputtered atoms", J
APPL PHYS, vol. 52, no. 9, pp. 5803-5805, 1981.
[137] Song PK, Shigesato Y, Yasui I, et al, "Study on crystallinity of tin-doped
indium oxide films deposited by dc magnetron sputtering", JPN J APPL PHYS,
vol. 137, no. 4a, pp. 1870-1876, 1998.
[138] Shigesato Y, Takaki S, Haranoh T, "Electrical and structural-properties of low
resistivity tin-doped indium oxide-films", J APPL PHYS, vol. 71, no. 7, pp. 3356-
3364, 1992.
[139] Kamei M, Shigesato Y, Takaki S, "origin of characteristic grain-subgrain
structure of tin-doped indium oxide-films", THIN SOLID FILMS, vol. 259, no. 1,
pp. 38-45, 1995.
116
[140] Higuchi M, Sawada M, Kuronuma Y, "Microstructure and electrical
characteristics of sputtered indium tin oxide-films", J ELECTROCHEM SOC, vol.
140, no. 6, pp. 1773-1775, 1993.
[141] Rottmann M, Heckner KH, "Electrical and structural-properties of indium tin
oxide-films deposited by reactive dc sputtering", J PHYS D APPL PHYS, vol. 28,
no. 7, pp. 1448-1453, 1995.
[142] Shigesato Y, Paine DC, "A microstructural study of low-resistivity tin-doped
indium oxide prepared by dc magnetron sputtering", THIN SOLID FILMS, vol.
238, no. 1, pp. 44-50, 1994.
[143] Higuchi M, Uekusa S, Nakano R, et al, "Micrograin structure influence on
electrical characteristics of sputtered indium tin oxide-films", J APPL PHYS, vol.
74, no. 11, pp. 6710-6713, 1993.
[144] Na JG, Cho YR, Kim YH, et al, "Effects of annealing temperature on
microstructure and electrical and optical-properties of radio-frequency-sputtered
tin-doped indium oxide-films", J AM CERAM SOC, vol. 72, no. 4, pp. 698-701,
1989.
[145] Morikawa H, Fujita M, "Crystallization and electrical property change on the
annealing of amorphous indium-oxide and indium-tin-oxide thin films", THIN
[146] Wu WF, Chiou BS, "Effect of annealing on electrical and optical-properties of
rf magnetron-sputtered indium tin oxide-films", APPL SURF SCI, vol. 68, no. 4,
pp. 497-504, 1993.
[147] Yasui H, Tsuda Y, "ITO thin-films prepared by magnetron sputtering method
using ito target - (effects of plasma conditions and substrate-temperature on ito
film properties)", JSME INT J B-FLUID T, vol. 38, no. 1, pp. 108-113, 1995.
[148] Latz R, Michael K, Scherer M, "High conducting large area indium tin oxide
electrodes for displays prepared by dc magnetron sputtering", JPN J APPL PHYS,
vol. 230, no. 2a, pp. l149-l151, 1991.
[149] Kawada A, "Indium-tin oxide deposition by dc reactive sputtering on a low
softening point material", THIN SOLID FILMS, vol. 191, no. 2, pp. 297-303,
1990.
[150] Larsson T, Blom HO, Nender C, et al, "A physical model for eliminating
instabilities in reactive sputtering", J VAC SCI TECHNOL, vol. a6, no. 3, pp.
1832-1836, 1988.
[151] Howson RP, Ridge MI, "Deposition of transparent heat-reflecting coatings of
metal-oxides using reactive planar magnetron sputtering of a metal and-or alloy",
THIN SOLID FILMS, vol. 77, no. 1-3, pp. 119-125, 1981.
[152] Bhagwat S, Howson RP, "Use of the magnetron-sputtering technique for the
control of the properties of indium tin oxide thin films", SURF COAT TECH, vol.
111, no. 2-3, pp. 163-171, 1999.
[153] Banerjee R, Ray S, Barua AK, "Thickness dependence of the properties of
magnetron sputtered indium tin oxide-films", J MATER SCI LETT, vol. 6, no. 10,
pp. 1203-1204, 1987.
[154] Shigesato Y, Takaki S, Haranou T, "Crystallinity and electrical-properties of
tin-doped indium oxide-films deposited by dc magnetron sputtering", APPL
SURF SCI, vol. 48-9, pp. 269-275, 1991.
[155] Vossen, Poliniak ES, Thin Solid Films, vol 13, p 281, 1972.
[156] Ishibashi S, Higuchi Y, Ota Y, et al, "Low resistivity indium tin oxide
transparent conductive films .2. effect of sputtering voltage on electrical property
of films", J VAC SCI TECHNOL, vol. a8, no. 3, pp. 1403-1406, 1990.
117
[157] Huang TC, Lim G, Parmigiani F, et al, "Effect of ion-bombardment during
deposition on the x-ray microstructure of thin silver films", J VAC SCI
TECHNOL, vol. a3, no. 6, pp. 2161-2166, 1985.
[158] Matsuda Y, Yamori Y, Muta M, et al, "Relation between plasma parameters
and film properties in dc reactive magnetron sputtering of indium-tin-oxide", JPN
J APPL PHYS, vol.136, no. 7b, pp. 4922-4927, 1997.
[159] Honda S, Chihara K, Watamori M, et al, "Depth profiling of oxygen content
of indium tin oxide fabricated by bias sputtering", APPL SURF SCI, vol. 114, pp.
408-411, 1997.
[160] Ma GH, Nathan A, "Room-temperature sputter deposition of polycrystalline
indium-tin oxide", ELECTROCHEM SOLID ST, vol. 2, no. 10, pp.542-543,
1999.
[161] Sun XW, Wang LD, Kwok HS, "Improved ito thin films with a thin zno buffer
layer by sputtering", THIN SOLID FILMS, vol. 360, no. 1-2, pp. 75-81, 2000.
[162] Meng L, Santos MP, THIN SOLID FILMS, vol 322, p 56, 1998.
[163] Kamei M, Yagami T, Takaki S, et al, "Heteroepitaxial growth of tin-doped
indium oxide-films on single-crystalline yttria-stabilized zirconia substrates",
APPL PHYS LETT, vol. 64, no. 20, pp. 2712-2714, 1994.
[164] Kamei M, Shigesato Y, Takaki S, et al, "Electron-microscopic and ion-
scattering studies of heteroepitaxial tin-doped indium oxide-films", APPL PHYS
LETT, vol. 65, no. 5, pp. 546-548, 1994.
[165] Ishibashi S, Higuchi Y, Ota Y, et al, "Low resistivity indium tin oxide
transparent conductive films .1. effect of introducing h2o gas of h2 gas during
direct-current magnetron sputtering", J VAC SCI TECHNOL, vol. a8, no. 3, pp.
1399-1402, 1990.
[166] Harding GL, Window B, "DC magnetron reactively sputtered indium-tin-
oxide films produced using argon-oxygen-hydrogen mixtures", SOL ENERG
MATER, vol. 20, no. 5-6, pp. 367-379, 1990.
[167] Rottmann M, Hennig H, Ziemer B, Kalahne R, Heckner KH. "Variations in
microstructure and composition of indium tin oxide films with the deposition
technique", J MATER SCI, vol.31, no.24, 1996,pp.6495-500.
[168] Zhang K, Zhu F, Huan CHA, Wee ATS. "Effect of hydrogen partial pressure
on optoelectronic properties of indium tin oxide thin films deposited by radio
frequency magnetron sputtering method", J APPL PHYS,vol.86, no.2, 1999,
pp.974-80
[169] Suzuki T, Yamazaki T, Oda H, "Effects of composition and thickness on the
electrical-properties of indium oxide tin oxide multilayered films", J MATER SCI,
vol. 24, no. 4, pp. 1383-1388, 1989.
[170] Suzuki T, Yamazaki T, Takizawa M, et al, "Thickness dependence of
electrical-properties in thin-films of undoped indium oxide prepared by ion-beam
sputtering", J MATER SCI, vol. 24, no. 1, pp. 187-191, 1989.
[171] Jan SW, Lee SC, "Preparation and characterization of indium-tin-oxide
deposited by direct thermal evaporation of metal indium and tin", J
ELECTROCHEM SOC, vol. 134, no. 8a, pp. 2056-2061, 1987.
[172] Nanto H, Minami T, Orito S, et al, "Electrical and optical-properties of indium
tin oxide thin-films prepared on low-temperature substrates by rf magnetron
sputtering under an applied external magnetic-field", J APPL PHYS, vol. 63, no.
8, pp. 2711-2716, 1988.
118
[173] Mukherjee A, "The deposition of transparent conductive oxide thin-films onto
large sheets of glass, acrylic and polycarbonate", VACUUM, vol.39, no. 6, pp.
537-540, 1989.
[174] Baia I, Quintela M, Mendes L, et al, "Performances exhibited by large area ito
layers produced by rf magnetron sputtering", THIN SOLID FILMS. vol. 337, no.
1-2, pp. 171-175, 1999.
[175] Morgan DV, Aliyu YH, Bunce RW, et al, "Annealing effects on opto-
electronic properties of sputtered and thermally evaporated indium-tin-oxide
films", THIN SOLID FILMS, vol. 312, no. 1-2, pp. 268-272, 1998.
[176] Kusano E, Kawaguchi J, Enjouji K, "Thermal-stability of heat-reflective films
consisting of oxide-ag-oxide deposited by dc magnetron sputtering", J VAC SCI
TECHNOL, vol. a4, no. 6, pp. 2907-2910, 1986.
[177] Choi KH, Kim JY, Lee YS, et al, "ito/ag/ito multilayer films for the
application of a very low resistance transparent electrode", THIN SOLID FILMS,
vol. 341, no. 1-2, pp. 152-155, 1999.
[178] Kloppel A, Kriegseis W, Meyer BK, et al, "Dependence of the electrical and
optical behaviour of ito-silver-ito multilayers on the silver properties", THIN
[179] Bender M, Seelig W, Daube C, et al, "Dependence of oxygen flow on optical
and electrical properties of dc-magnetron sputtered ito films", THIN SOLID
FILMS, vol. 326, no. 1-2, pp. 72-77, 1998.
[180] Geoffroy C, Campet G, Portier J, et al, "Preparation and characterization of
fluorinated indium tin oxide-films prepared by rf-sputtering", THIN SOLID
FILMS, vol. 202, no. 1, pp. 77-82, 1991.
[181] Suzuki M, Maeda Y, Sawada Y, "Enhanced electrical conductivity of indium
tin oxide films by ag addition", JPN J APPL PHYS, vol. 137, no. 1, pp. 34-38,
1998.
[182] Utsumi K, Matsunaga O, Takahata T, "Low resistivity ito film prepared using
the ultra high density ito target", THIN SOLID FILMS, vol. 334, no. 1-2, pp. 30-
34, 1998.
[183] Echigoya J, Kato S, Enoki H, "Optical and electrical-properties of laser-
irradiated in2o3-4mol-percent sno2", J MATER SCI-MATER EL, vol. 3, no. 3,
pp. 168-171, 1992.
[184] Cranton W private communication.
[185] Dutta J, Ray S, "Variations in structural and electrical-properties of
magnetron-sputtered indium tin oxide-films with deposition parameters", THIN
[186] Karasawa T, Miyata Y, "Electrical and optical-properties of indium tin oxide
thin-films deposited on unheated substrates by dc reactive sputtering", THIN
[187] Nadaud N, Kim DY, Boch P, "Titania as a sintering additive in indium oxide
ceramics", J AM CERAM SOC, vol. 80, no. 5, pp. 1208-1212, 1997.
[188] Szyszka B, Jager S, "Optical and electrical properties of doped zinc oxide
films prepared by ac reactive magnetron sputtering", J NON-CRYST SOLIDS,
vol.218, pp. 74-80, 1997.
[189] Ellmer K, Kudella F, Mientus R, et al, "Influence of discharge parameters on
the layer properties of reactive magnetron-sputtered zno-al films", THIN SOLID
FILMS, vol. 247, no. 1, pp. 15-23, 1994.
119
[190] Hu JH, Gordon RG, "Textured fluorine-doped zno films by atmospheric-
pressure chemical vapor-deposition and their use in amorphous-silicon solar-
cells", SOL CELLS, vol. 30, no. 1-4, pp. 437-450 1991.
[191] Vandepol FCM, Blom FR, Popma TJA, "RF planar magnetron sputtered zno
films .1. structural-properties", THIN SOLID FILMS, vol. 204, no. 2, pp. 349-
364, 1991.
[192] Polycrystalline Semiconductors, eds. Werner JH, Moller HJ, Strunk HP,
Springer, 1989.
[193] Tsurumi T, Nishizawa S, Ohashi N, et al, "Electric properties of zinc oxide
epitaxial films grown by ion-beam sputtering with oxygen-radical irradiation",
JPN J APPL PHYS, vol. 138, no. 6a, pp 3682-3688, 1999.
[194] Igasaki Y, Saito H, "The effects of deposition rate on the structural and
electrical-properties of zno-al films deposited on (1120) oriented sapphire
substrates", J APPL PHYS, vol. 70, no. 7, pp. 3613-3619 1991.
[195] Ellmer K, Wendt R, "dc and rf (reactive) magnetron sputtering of zno:al films
from metallic and ceramic targets: a comparative study", SURF COAT TECH,
vol. 93, no. 1, pp. 21-26, 1997.
[196] Tominaga K, Kuroda K, Tada O, "Radiation effect due to energetic oxygen-
atoms on conductive al-doped zno films", JPN J APPL PHYS, vol.127, no. 7, pp.
1176-1180, 1988.
[197] Bose S, Ray S, Barua AK, "Textured aluminium-doped zno thin films
prepared by magnetron sputtering", J PHYS D APPL PHYS, vol. 29, no. 7, pp.
1873-1877, 1996.
[198] Ellmer K Cebulla R, Wendt R, "Transparent and conducting zno(: al) films
deposited by simultaneous rf- and dc-excitation of a magnetron", THIN SOLID
FILMS, vol. 317, no. 1-2, pp. 413-416, 1998.
[199] Tsuji T, Hirohashi M, "Influence of oxygen partial pressure on transparency
and conductivity of rf sputtered al-doped zno thin films", APPL SURF SCI, vol.
157, no. 1-2, pp. 47-51, 2000.
[200] Ellmer K, "Magnetron sputtering of transparent conductive zinc oxide: relation
between the sputtering parameters and the electronic properties", J PHYS D APPL
PHYS, vol. 33, no. 4, pp. R17-R32, 2000.
[201] Wickramanayaka S, Matsumoto A, Nakanishi Y, et al, "Remote plasma sio2
deposition by tetraethoxysilane with chemically and energetically different atomic
species", JPN J APPL PHYS, vol. 133, no. 6a, pp. 3520-3527, 1994.
[202] Yoon KH, Choi JW, Lee DH, "Characteristics of zno thin films deposited onto
al/si substrates by rf magnetron sputtering", THIN SOLID FILMS, vol. 302, no. 1-
2, pp. 116-121, 1997.
[203] Sundaram KB, Khan A, "Characterization and optimization of zinc oxide films
by rf magnetron sputtering", THIN SOLID FILMS, vol. 295, no. 1-2, pp. 87-91,
1997.
[204] Han BM, Chang S, Kim SY, "Chopping effect on the crystallinity of zno films
prepared by a r.f. planar magnetron sputtering method", THIN SOLID FILMS,
vol. 338, no. 1-2, pp. 265-268, 1999.
[205] Tominaga K, Umezu N, Mori I, et al, "Effects of uv light irradiation and
excess zn addition on zno : al film properties in sputtering process", THIN SOLID
FILMS, vol. 316, no. 1-2, pp. 85-88, 1998.
[206] Jager S, Szyszka B, Szczyrbowski J, et al, "Comparison of transparent
conductive oxide thin films prepared by a.c. and d.c. reactive magnetron
sputtering", SURF COAT TECH, vol. 98, no. 1-3, pp. 1304-1314, 1998.
120
[207] Menner R, Schaffler R et al, PROC. 2
ND
WORLD CONF. EXHIB.
PHOTOVOL. SOL. ENERGY, Vienna, 1998, p 660
[208] Cebulla R, Wendt R, Ellmer K, "Al-doped zinc oxide films deposited by
simultaneous rf and dc excitation of a magnetron plasma: relationships between
plasma parameters and structural and electrical film properties", J APPL PHYS,
vol. 83, no. 2, pp. 1087-1095, 1998.
[209] Kluth O, Rech B et al, PROC. 2
ND
INT. CON. COAT. GLASS, Saarbrucken,
Germany.
[210] Tominaga K, Umezu N, Mori I, et al, "Transparent conductive zno film
preparation by alternating sputtering of zno : al and zn or al targets", THIN
[211] Park KC, Ma DY, Kim KH, "The physical properties of al-doped zinc oxide
films prepared by rf magnetron sputtering", THIN SOLID FILMS, vol. 305, no. 1-
2, pp. 201-209, 1997.
[212] Minami T, Yamamoto T, Miyata T, "Highly transparent and conductive rare
earth-doped zno thin films prepared by magnetron sputtering", THIN SOLID
FILMS, vol. 366, no. 1-2, pp. 63-68, 2000.
[213] Zhang K, Zhu F, Huan CHA, Wee ATS, "Osipowicz T. Indium-doped zinc
oxide films prepared by simultaneous r.f.and d.c. magnetron sputtering", Wiley.
SURFACE & INTERFACE ANALYSIS, vol.28, no.1, 1999, pp.271-4.
[214] Minami T, Sonohara H, Kakumu T, et al, "Highly transparent and conductive
zn2in2o5 thin-films prepared by rf magnetron sputtering", JPN J APPL PHYS,
vol. 234, no. 8a, pp. l971-l974, 1995.
[215] Choe YS, Chung JH, Kim DS, et al, "Synthesis of tin oxide films by dual ion
beam sputtering using sn target and oxygen ion beam", SURF COAT TECH, vol.
112, no. 1-3, pp. 267-270, 1999.
[216] 216.
[217] Choe YS, Chung JH, Kim DS, et al, "Ion beam sputtering of sno2 with low
energy oxygen ion beams", THIN SOLID FILMS, vol. 341, no. 1-2, pp. 230-233,
1999.
[218] Qin W, Howson RP, Akizuki M, et al, "Indium oxide film formation by o-2
cluster ion-assisted deposition", MATER CHEM PHYS, vol. 54, no. 1-3, pp. 258-
261, 1998.
[219] Akizuki M, Matsuo J, Ogasawara S, et al, "Low-temperature oxidation of
silicon by o-2 cluster ion beams", JPN J APPL PHYS, vol. 135, no. 2b, pp. 1450-
1453, 1996.
[220] Akizuki M, Matsuo J, Yamada I, et al, "SIO2 film formation at room
temperature by gas cluster ion beam oxidation", NUCL INSTRUM METH B, vol.
112, no. 1-4, pp. 83-85, 1996.
[221] Akizuki M, Matsuo J, Harada M, et al, "Gneration of O
2
and metalorganic
cluster ion beams and its application to low-temperature thin oxide film
formation", MAT SCI ENG A-STRUCT, vol. 217, pp. 78-81, 1996.
[222] Fan JCC. Preparation of Sn-doped In/sub 2/O/sub 3/ (ITO) films at low
deposition temperatures by ion-beam sputtering, APPL PHYS LETT, vol.34,
no.8, 1979, pp.515-17.
[223] Gessert TA, Williamson DL, Coutts TJ, et al, "The dependence of the
electrical-properties of ion-beam sputtered indium tin oxide on its composition
and structure", J VAC SCI TECHNOL A, vol. 5, no. 4, pp. 1314-1315, 1987.
121
[224] Bellingham JR, Phillips WA, Adkins CJ, "Electrical and optical-properties of
amorphous indium oxide", J PHYS-CONDENS MAT, vol. 2, no. 28, pp. 6207-
6221, 1990.
[225] Bellingham JR, Phillips WA, Adkins CJ, "Amorphous indium oxide", THIN
[226] Bellingham JR, Graham M, Adkins CJ, et al, "Temperature-dependence of the
resistivity of amorphous indium oxide", J NON-CRYST SOLIDS, vol. 137,
pp.519-522, 1991.
[227] Bellingham JR, Mackenzie AP, Phillips WA, "Precise measurements of
oxygen-content - oxygen vacancies in transparent conducting indium oxide-
films", APPL PHYS LETT, vol. 58, no. 22, pp. 2506-2508, 1991.
[228] Bellingham JR, Phillips WA, Adkins CJ, "Intrinsic performance limits in
transparent conducting oxides", J MATER SCI LETT, vol. 11, no. 5, pp. 263-265,
1992.
[229] Graham MR, Bellingham JR, Adkins CJ, "Hopping conduction near the metal-
insulator-transition in amorphous indium oxide", PHILOS MAG B, vol. 65, no. 4,
pp. 669-673, 1992.
[230] Pongratz S, Zoller A, "Plasma ion-assisted deposition - a promising technique
for optical coatings", J VAC SCI TECHNOL, vol. a10, no. 4, pp. 1897-1904,
1992.
[231] Laux S, Kaiser N, Zoller A, et al, "Room-temperature deposition of indium tin
oxide thin films with plasma ion-assisted evaporation", THIN SOLID FILMS, vol.
335, no. 1-2, pp. 1-5, 1998.
[232] Cho JS, Koh SK, Yoon KH, "Microstructure and electrical properties of
indium oxide thin films prepared by direct oxygen ion-assisted deposition", J
ELECTROCHEM SOC, vol.147, no. 3, pp. 1065-1070, 2000.
[233] Bae JW, Kim HJ, Kim JS, et al, "Effects of oxygen ion beam plasma
conditions on the properties of indium tin oxide thin films", VACUUM, vol. 56,
no. 1, pp. 77-81, 2000.
[234] Suzuki Y, Niino F, Katoh K, "Low-resistivity ito films by dc arc discharge ion
plating for high duty lcds", J NON-CRYST SOLIDS, vol.218, pp. 30-34, 1997.
[235] Uramoto J, Research Report Inst. Plasma Physics, Nagogya Univ., Nagoya
Univ., Nagoya, Japan, IPPJ237, 1975.
[236] Kuroyanagi A, "Crystallographic characteristics and electrical-properties of al-
doped zno thin-films prepared by ionized deposition", J APPL PHYS, vol. 66, no.
11, pp. 5492-5497, 1989.
[237] Petritz RL, PHYS. REVIEW, vol 104, p 1508, 1956.
[238] Seto JYW. The electrical properties of polycrystalline silicon films, J. OF
APPLIED PHYSICS, vol.46, no.12, 1975, pp.5247-54
[239] Manifacier JC, Gasiot J, Fillard JP. A simple method for the determination of
the optical constants n, k and the thickness of a weakly absorbing thin film,
Journal of Physics e - Scientific Instruments, vol.9, no.11, 1976, pp.1002-4.
[240] Semiconducting Transparent thin Films, Hartnagel HL, Dawar AL, Jain AK,
Jagadish C, Institute of physics publishing, 1995.
[241] Haacke G, J. APPL. PHYS., Vol 47, p 4086, 1976.
[242] Ritala M, Asikainen T, Leskela M,Enhanced growth rate in atomic layer
epitaxy of indium oxide and indium tin oxide thin films, ELECTROCHEMICAL
AND SOLID STATE LETTERS, Vol 1, pp156-157, 1998.
Section 8: Highly conductive ITO frequency selective structures Frequency Selective Windows
122
Section 8: Highly conductive ITO frequency selective
structures
Introduction
The ITO fabricated at NTU was employed to fabricate a frequency selective structure
with a bandstop frequency at around 28 GHz. The performance of the ITO FSS is
compared with those made of copper and transparent thin-film gold.
In order for a comparison in terms of shielding performance to be possible the same
FSS pattern was replicated on each of the three different materials. A triangular lattice
with ring elements was chosen as the particular type of FSS for all the materials. The
structure is shown in Figure 1. The period, D, of the FSS is equal to 0.45 mm and the
mean diameter, r, of the ring element is equal to 0.15mm.
The thin film gold is commercial and is obtained from CPFilms, Portsmouth, UK.
Details of the etching procedure were presented in section 8. The surface resistance of
the gold film is 1-2 /. The film is about 20-35% transparent in the visual spectrum.
The uniformity of the gold film across the polymer substrate was very good.
For the copper FSS structure a thin sheet of copper was used which was attached to a
standard glass after the FSS pattern had been etched.
A number of optically transparent FSS patterns made with ITO, produced at NTU,
were measured independently by the Radiocommunication Agency [1].
In-House Fabrication And Characteristics Of The ITO
The in-house ITO was grown on glass wafers 100 mm in diameter and 2 mm in
thickness, by using RF magnetron sputtering at 280C and 5 mTorr sputtering gas
pressure, for 50 min. The RF power was kept at 200 Watt in order to get optimum
quality ITO films. The sputtering gas consisted of 2% oxygen in argon. A 13.56 MHz
RF power supply was used. More details of the growth and the development systems
are presented in Section 8. A commercially available ITO ceramic target was
employed instead of a metallic indium and tin target.
The thin film ITO employed to generate the FSS had a surface resistance of around
1.6 /. Its optical transparency was around 90% and its thickness was 8000 . The
value of the resistivity was calculated to be 1.28x10
-4
cm. This film has not
undergone post-annealing treatment. It was slightly stressed but it showed excellent
adherence to the glass, good stability and good performance with varying
environmental factors.
This resistivity is among the lowest reported to date [2,3]. An elevated deposition
temperature was used because the ITO resistivity is abruptly increasing below 250C.
The reproducibility also of the films is affected adversely with the age of the ITO
target.
We are currently involved in optimising the deposition conditions, growing ITO at
lower temperatures without affecting the achieved conductivity and using different
techniques for improving further the conductivity without compromising the optical
transparency. There are indications that the conductivity can be improved further
without affecting much the high optical transparency [4,5].
The sheet resistance of our films was measured with a four-point probe station. There
was less than 10% variation of sheet resistance across the substrate with the values
becoming higher towards the edge. The resistivity is estimated by multiplying the
sheet resistance at the centre by the thickness of the film. The thickness is measured
by a Dectak-Sloan profilometer over an edge of the etched film. The transparency in
123
the visual spectrum is measured with the aid of a spectro-photometer. It is calculated
as the ratio of the transmitted light intensity through the film to the transmitted light
intensity through the glass substrate only. A standard incandescent source is used to
provide the incident white light. The comparison in terms of transparency between the
thin gold film and the ITO sample can be seen in Figure 2.
Experimental Procedure and Results
The FSS structures were mounted onto a square metal plate (280 280mm), which
was covered with absorbers (600 490mm) for protection against any diffraction
phenomena as seen in Fig 3. The metal plate has a hole of 100 mm in the middle in
order to accommodate the sample. The whole structure has the capability of rotational
motion. The structures have two different interfaces, glass and air as shown in Fig.1.
An open-ended K
A
band rectangular waveguide was used for the production of the
incident plane wave, and it was positioned at 463 mm away from the structure. A horn
antenna was used as the receiver, and was position 214 mm away from the back of the
FSS. The transmission coefficient (S
21
parameter) was obtained with the aid of a HP
8722D vector network analyser. Figure 4 presents the co-polarisation transmission
results of the triangular lattice FSS made different conducting materials. It can be seen
that the copper structure has the best performance as expected, while the ITO is
visibly superior to the gold film of comparable surface resistance. The copper FSS has
a resonant frequency at almost 32 GHz with an attenuation of 30 dB. This has been
confirmed by independent measurements at the Radiocommunications Agency and at
The Nottingham Trent University [1]. The gold FSS has a resonance frequency
greater than the copper and an attenuation of 16 dB. In contrast to both of these
materials the ITO FSS has a resonant frequency at 29 GHz and an attenuation of 25
dB. We believe that this shift can be attributed to the finite size of our aperture and
can be eliminated if more ring elements are used. Further investigation is being
carried out to clarify this matter. It was further established that the orientation of the
FSS structures did not affect the experimental results at normal incidence. Fig. 5
shows how the angle of plane wave incidence affects the performance of the co-
polarisation transmission of the ITO structure. It can be seen that the resonance
frequency does not change significantly with the angle of incidence. This stable
behaviour is attributed to the particular FSS structure that has been selected for this
work. Figure 6 shows how the performance of ITO compares with that of copper at
30 plane wave incidence. The attenuation around 35 and 37 GHz is caused by the
particular orientation of the structure. This was verified by measuring the response of
a substrate of larger dimensions (270mm 200mm) with copper based FSS.
Conclusions
We have showed that in order to have good screening performance (better than -
20db) the transparent conducting material should be around 1-2 /. We believe that
lower surface resistance is achievable and future investigation will determine how low
its value can be. Using more FSS layers is expected to improve considerably the
shielding performance of the structure.
References
[1] M. Dudhia, Optically transparent RF absorbing structures, RTCG project report
566, August 2000.
124
[2] Hamberg, C. G. Granvist, Evaporated Sn-doped In
2
O
3
films:Basic optical
properties and applications to energy efficient windows, J. Appl. Phys., vol 60,
1983, pp. R123-R159
[3] A.L. Dawar, J.C. Joshi, Review Semiconducting transparent thin films:their
properties and applications, J. Mater. Sci., vol 19, 1984, pp.1-23
[4] J.R. Bellingham, W.A. Phillips, C.J. Adkins. Intrinsic performance limits in
transparent conducting oxides, J Mater. Sci. Lett., vol 11, 1992, pp. 263-265
[5] S. Ray, R. Banerjee, N. Basu, A.K. Batabyal, A.K. Barua, Properties of tin doped
indium oxide thin films prepared by magnetron sputtering, J. Appl. Phys., vol 54,
1983, pp. 3497-3501
Figure 1: Top and side view of the FSS structure that has been used with D = 0.45
mm.
and r = 0.15 mm
450 500 550 600 650 700 750
0
10
20
30
40
50
60
70
80
90
100
WAVELENGTH nm
T
R
A
N
S
P
A
R
E
N
C
Y

%
air
D
r
glass
125
Figure 2:The optical transparencies of the in-house ITO (o) and the commercially
available gold thin film (*).
Figure 3: The dimensions of the set up used in this experiments. The width of the
absorber block is W= 600 mm.
2.6 2.8 3 3.2 3.4 3.6 3.8 4
x 10
10
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
A
T
T
E
N
U
A
T
I
O
N

d
B
Top
view
Transmitting
antenna
214mm
463mm
Side
view
305mm
100mm
90mm
Rotational stand
Transmitting
antenna
126
Figure 4: Co-polarisation transmission graphs graphs of Copper FSS (), ITO FSS
(O) and thin Gold film FSS ().
Figure 5: Co-polarisation transmission graphs of ITO FSS at different angles of plane
wave incidence: =0 (), =15 (), =30 ().
Figure 6: Co-polarisation transmission graphs for Copper () and ITO (O) at =30
of plane wave incidence.
2.6 2.8 3 3.2 3.4 3.6 3.8 4
x 10
10
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
A
T
T
E
N
U
A
T
I
O
N

d
B
2.6 2.8 3 3.2 3.4 3.6 3.8 4
x 10
10
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
A
T
T
E
N
U
A
T
I
O
N

d
B
Section 9: FSS box and Microwave Oven measurements Frequency Selective Windows
127
Section 9: FSS box and Microwave Oven measurements
Introduction
The aim is to create a frequency selective surface box (an igloo type enlcosure)
which, when a microwave oven is inserted in it, will be able to significantly attenuate
microwave radiation centre around the operating frequency of the microwave oven
(2.45 GHz). Hexagonal element frequency selective surfaces were employed to shield
the microwave oven emissions. To avoid multipath propagation which results in
deterioration of the FSS box performance, pyramidal absorbers were inserted within
the enclosure.
Enclosure Structure
The box structure must allow flexibility in testing a variety of FSS. The box structure
was constructed using a proprietary system [1] consisting of slotted extruded
aluminium supports connected by cast aluminium knuckle joints at the corners. The
slots allowed structures of up to 10mm in thickness to be used, these being optionally
held in place by rubber wedges. The initial structure is 600mm high, 900 mm deep,
and 900mm wide as shown in Figure 1, the internal knuckle corner detail is shown in
Figure 2 below. The larger the structure the more the number of periods on the FSS
window.
Solid 4mm thick aluminium sheets were used on the floor and ceiling of the
enclosure.
By using suitably cut glass window frames, different thickness of dielectric substrates
and multiple layer FSS structures can easily be employed as walls.
To accommodate for coaxial or power cables when placing an antenna (biconical) or
the microwave oven respectively within the box, a hole was drilled on the boxs floor.
Hexagonal element FSS
A number of hexagonal structures were considered for the construction of the FSS
box. The FSS box must block microwave radiation at around 2.45GHz. The
dimensions of the hexagonal element of the preferred hexagonal FSS were identified
empirically from the various experiments.
In order to determine the effect of separation distance on the FSS performance (for the
preferred element), two types of element spacing were used. These are shown in
Figure 1 Figure 2
128
9999Figures 3 and 4 and are termed as close and distant coupling. The
geometrical dimensions are also shown.
The array does not posses the same symmetry along the x and y axis. Therefore, the
FSS performance for normal plane wave incidence with the electric field oriented
along the x and y axis is examined.
Single and double FSS layers are considered. In the case of double layer FSS, both air
and glass spacing are considered. The hexagons are produced using high conductivity
silver ink. They are printed on a polyester film which is subsequently sandwiched
between glass substrates.
The effect of electric field polarisation on a single layer structure orientation is shown
in figure 5. This figure shows the FSS filter response with the hexagons in a vertical
and horizontal position. This position is identified in figure 5. It can be seen, that the
FSS response for the two orientations of the electric field is practically identical. The
results in Figure 5 are for the close coupled hexagons. The centre frequency of of
around 2.5GHz is constant in both cases with a maximum attenuation of 26dB. Note
however, that the measurements were performed using an absorbing stand and not
isolated enclosures in order to accelerate the measurement process. Thus, the results
presented may deviate from those obtained using ideal measurements conditions. For
example, the fluctuations at low frequencies were reduced by placing absorbing
material around the transmitting horn antenna and by increasing the amount of
absorbers around the measurement stand.
Figure 3. Close coupling.
x
y
y
x
t=1.44 mm
a=1.15 cm
d=
1.1mm
Figure 4. Distant coupling
t=1.44 mm
a=1.15 cm
d=
4.1 mm
129
The response of single and double layer FSS is presented in figure 6. The single layer
FSS consists of printed closed couple hexagonal elements sandwiched between two
4mm glass substrates. The double layer FSS consists of two single layer FSS
separated by a 4mm-thick layer of glass and also sandwiched between two 4mm glass
substrates. The hexagons are aligned vertically (see figure 6). We observe that the
bandstop characteristic of the double layer FSS is more abrupt. The centre frequency
of the two structures is similar. There is also a slight decrease in attenuation by the
double layer.
The effect of cascading two FSS layers with identical or orthogonal hexagon
orientations is also examined (see figure 7). Significant increase in the attenuation
level (40dB) at the centre frequency of around 2.5GHz is observed for the orthogonal
orientations relative to the aligned orientations (22dB). The two FSS layers were
separated by a 4mm-thick glass slab.
Figure 6
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-30
-25
-20
-15
-10
-5
0
5
Single and Double Hexagons FSS
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
Single
Double
(Hz)
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-30
-25
-20
-15
-10
-5
0
Hexagon Orientation
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
Horizontal
Vertical
E
E
(Hz)
Figure 5.
130
In two layer FSS, the effect of varying the separation distance between the layers is
illustrated in figure 8. The two layers consist of vertically aligned hexagons. Three
separation thickness were considered: 4, 6 and 8mm. It can be seen that the centre
frequency drifts slightly towards lower values and the level of attenuation increases as
the glass thickness increases.
The effect of air instead of glass between two close coupled vertically oriented
hexagon FSS layers is shown in figure 9. The FSS combination was sandwiched
between 4mm-thick glass substrates. It can be seen that the attenuation level is
slightly improved bandwidth increases as the air gap thickness increases.
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-45
-40
-35
-30
-25
-20
-15
-10
-5
0
5
Orthogonal Hexagon Double FSS
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
Aligned
Orthogonal
Figure 7
(Hz)
Figure 8
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
5
Double Hexagonal
Frequency
Tr
an
sm
itt
an
4mm glass
6mm glass
8mm glass
(Hz)
Figure 9
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
5
Double Hexagon FSS air gap spacing
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
AIR GAP:
0mm
9mm
54mm
(Hz)
131
The 54 mm air gap double-layer close coupled hexagons with aligned orientation are
compared with an orthogonal orientation double-layer FSS structure with also a
54mm air gap. The spectral response of the two filters is almost identical (figure 10).
In figure 11, the performance of two single layer FSS with closed and distant coupled
hexagonal elements respectively is investigated. In each FSS structure, the elements
are sandwiched between two 4mm-thick glass substrates. The results reconfirm an
earlier observation that by changing the lattice spacing the bandstop frequency also
changes.
The closed coupled element FSS has, at normal incidence, the required, for the
project, spectral response. Hence its performance at different angles of plane wave
incidence and incident electric field polarisation (with respect to element orientation)
is examined below.
The following two figures (figures 12 and 13) show the co-polarisation transmittance
response at two different angles of plane wave incidence, at 0 (blue and red lines)
and 45 (cyan, magenta, yellow and green lines), and for the two different element
orientations, vertical (blue, cyan, green), horizontal (red, magenta, yellow). The
yellow and green lines show the measurements acquired with both antennas polarised
horizontally. The rest four coloured lines represent the measurements when both
antennas are vertically polarised.
In figure 12 the transmittance response is shown of a single layer FSS sandwiched
between two similar layers of glass of 4 mm in thickness. The common minimum is
also shown in the same figure and for the frequency at interest (2.45 GHz) has a value
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-30
-25
-20
-15
-10
-5
0
5
Far and near coupled hexagons
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
(Hz)
Close coupled
Distant coupled
Figure 11
Figure 10
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
5
Orthogonal Double Hexagon with air gap
Frequency
T
r
a
n
s
m
i
t
t
a
n
c
e
Aligned
Orthogonal
(Hz)
132
of about 17.5 dB. This means that a wave at 2.45 GHz that is incident on the structure
at any angle between 0 and 45 has at least 17.5 dB attenuation.
In figure 13 the co-polarisation transmittance response is shown for the double layer
FSS. This structure is composed by two single FSS layers separated by a single layer
of glass, 6 mm in thickness, and the whole structure is sandwhiched between two
similar layers of glass 4 mm in thickness. The common minimum for 2.45 GHz is
found to be at about 22 dB.
In conclusion, when designing an FSS structure the following factors (a) element
orientation between layers; (b) distance between elements; (c) substrate material and
thickness in addition to (d) element geometry, affect the FSS filter parameters
(bandstop frequency, bandwidth and attenuation). Hence, in finely tuning the desired
frequency response of an FSS structure, considerable numerical and/or experimental
work must be made. Here, through an extended series of experiments, we have
achieved the aim of designing an FSS with a bandstop frequency at around 2.5 GHz.
Microwave Oven Measurements
The following results show the investigations made at Nottingham Trent University
on the performance of an FSS box enclosing a microwave oven. Multipath
phenomena within the box suggested that absorbers should be placed within the box
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
T
R
A
N
S
M
IT
T
A
N
C
E
Common minimum
Figure 13
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
5
FREQUENCY Hz
T
R
A
N
S
M
IT
T
A
N
C
E
Common minimum
Figure 12
133
to improve the boxs shielding effectiveness. This can also be done by removing a
side of the box. During the measurements, steam was generated within the box. The
effect of the steam was not analysed.
It was also observed that by completely shielding the box and using a biconical
antenna as the transmitter, the reflection coefficient of the antenna system (i.e.
antenna + metallic box) was increased. This observation agrees with the calculations
of the input impedance of a cavity. The latter impedance is shown to increase in value
as the losses of the cavity walls reduce.
The results that follow show comparisons between the calibration results (which are
direct measurements without the presence of frequency selective structures) and FSS
results. The letters (E,W,S,N) and phrases (top plate, bottom plate) indicating the
orientation of the horn antenna in respect to the box, the presence or not of absorbers,
metal plates etc. are clarified in the following figure. The presence or not of absorbers
is presented some times with the letter A (presence) or E (absence or empty) in front
of the letter that denotes a particular side (E,W,S,N). The horn antenna was vertically
polarised and was placed at 50 cm away from the front surface of the box (S side).
In every result that follows, apart from the plots there is a figure indicating the setup
employed.
The following types of FSS were employed on the south side:
4mmFSS4mm: single layer hexagonal element FSS sandwiched between two
4mm thick glass windows.
4mmFSS6mmFSS4mm: two layer hexagonal element FSS sandwiched between
4mm, 6mm and 4mm thick glass windows.
The height (H) of the receiving antenna is either 102 cm (Figure 1 antenna at the
same height as the microwave oven) or 117 cm (Figure 3 antenna at the middle of
the FSS window).
In the experiments, a microwave oven, a biconical antenna and a broadband horn were
employed.
Top view Side View
It is our conclusion that an optically transparent FSS box can block the emitted
radiation from a microwave oven. However, future work is required in dealing with
the multipath reflection issue and in identifying FSS structures with an even more
improved performance. We believe that the latter can be achieved using a more
conductive paint.
South
Side (S)
East
Side (E)
North Side (N)
West
Side (W)
Top metal plate
Bottom metal plate
134
Figure. 14.
Red= absorbers N,E,W, empty S, no top metal plate.
Blue= absorbers N,E,W, 4mmFSS4mm S, no top metal plate
Horn antenna at 102 cm.
H = 102cm
Top view Side view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

135
Figure. 15.
Blue= absorbers N,E,W, 4mmfss6mmfss4mm in S, no top metal plate
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

136
Figure. 16.
Red= absorbers N,E,W, empty S, no top metal plate, antenna at 117 cm.
Blue= absorbers N,E,W, 4mmfss6mmfss4mm S, no top metal plate, Horn antenna at 117 cm
H = 117cm
Top view Side view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

137
Figure. 17.
Blue= absorbers N,E,W, 4mmfss6mmfss4mm S, no top metal plate, Horn antenna at 102 cm,
microwave oven at 20 degrees angle.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

20
138
Figure. 18.
Blue= absorbers N,E,W, 4mmfss6mmfss4mm S, no top metal plate, Horn antenna at 102 cm,
microwave oven at 35 degrees angle.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

35
139
Figure. 19.
Red= metal plate E,W, empty S, top metal plate on, empty N.
Blue= metal plate E,W, 4mmfss6mmfss4mm S, top metal plate on, empty N
H = 102cm
Top view Side view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

140
Figure. 20.
Red= metal plate E,W, empty S, top metal plate on, empty N.
Blue= metal plate E,W, 4mmfss6mmfss4mm S, top metal plate on, empty N,Horn antenna 117cm
height
H = 127cm
Top view Side view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

141
Figure. 21.
Red= absorbers E,W, empty N, S, with top metal plate.
Blue= absorbers E,W, empty N, 4mmfss4mm S, with top metal plate
at angle 20 degrees, Horn antenna at 102 cm.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

20
142
Figure. 22.
Blue= absorbers E,W, empty N, 4mmfss6mmfss4mm S, with top metal plate
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

20
143
Figure. 23.
Red= absorbers E,W, empty N, empty S, with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

35
144
Figure. 24.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

35
145
Figure. 25.
at angle 35 degrees, Horn antenna at 117 cm Repeat of previous experiment for reproducibility
reasons.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

35
146
Figure. 26.
Blue= absorbers E,W, empty N, 4mmfss4mm S, with top metal plate.
Microwave oven at at angle 35 degrees. Horn antenna at 117 cm.
Top view
35
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

147
Figure. 27.
Blue= absorbers E,W, empty N, 4mmfss4mm S, with top metal plate
Microwave oven at angle 35 degrees. Horn antenna at 102 cm.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

35
148
Figure. 28.
Blue=4mmfss4mm N,E,W,S (all around), no top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

149
Figure. 29.
Red=absorbers N,E,W, empty S, no top metal plate.
Blue=4mmfss4mm N,E,W, S,(all around), no top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

150
Figure. 30.
Blue=4mmfss4mm N,E,W,S (all around), no top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

151
Figure. 31.
Red= absorbers N,E,W, empty S, with top metal plate.
Blue=4mmfss4mm N,E,W, S,(all around), with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

152
Figure. 32.
Red= absorbers N,E,W, empty S, with top metal plate.
Blue=4mmfss4mm N,E,W, S,(all around), with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

153
Figure. 33.
Blue=4mmfss4mm E,W,S, empty N, with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

154
Figure. 34.
Blue=4mmfss4mm E,W,S, empty N, with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

155
Figure. 35.
Magenta= absorbers E,W, empty N, S, with top metal plate
With cup of water placed at the centre
Cyan= absorbers E,W, empty N, S, with top metal plate.
Empty turntable, height 102 cm.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

156
Figure. 36.
Magenta= absorbers E,W, empty N, S, with top metal plate
With cup of water placed at the centre
Cyan= absorbers E,W, empty N, S, with top metal plate
Empty turntable. Horn antenna at 117 cm
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

157
Figure. 37.
Repeat twice of the same experiment for reproducibility reasons. Water at the very edge.
Horn antenna at height 117 cm. 4mmfss4mm E,W,S, empty N, with top metal plate.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

158
Figure. 38.
Magenta= absorbers E,W, empty N, S, with top metal plate.
Black= absorbers E,W, empty N, S, with top metal plate.
With cup of water placed at the edge.
Top view
2.35 2.4 2.45 2.5 2.55
x 10
9
-100
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

159
Figure 39:
Effect of 4mm glass FSS on the transmission of a biconical antenna placed inside the box.
Transmitting antenna is the biconical and receiving antenna is the horn with Vertical
polarisation. Red data are the raw data which result from subtraction of calibration with
absorber-NEW empty-S and top metal plate from the ones with 4mmfss all around with top
metal plate.
Blue line is the averaged red by every 10 points.
0.5m
Top view
1.5 2 2.5 3 3.5 4 4.5 5 5.5
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
5
10
15
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5 5.5
x 10
9
-20
-15
-10
-5
0
5
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

160
Figure 40:
Transmitting antenna is the horn with vertical polarisation and receiving antenna is the
biconical.Red data are the raw data which result from subtraction of calibration with absorber-
NEW empty-S and top metal plate from the ones with 4mmfss all around with top metal plate.
0.5m
Top view
1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-35
-30
-25
-20
-15
-10
-5
0
5
10
15
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-20
-15
-10
-5
0
5
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

161
Figure 41:
Transmitting antenna is the biconical and receiving antenna is the horn with vertical
polarisation. Measurements were taken around the dip with 1MHz step.
0.5m
Top view
2.4 2.6 2.8 3 3.2 3.4 3.6
x 10
9
-40
-30
-20
-10
0
10
20
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

2.4 2.6 2.8 3 3.2 3.4 3.6
x 10
9
-20
-15
-10
-5
0
5
10
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

162
Figure 42:
Transmitting antenna is the biconical at the centre of box and receiving antenna is the horn with
vertical polarisation placed at 2m away from the side of box. Red data are the raw data which
result from subtraction of calibration with absorber-NEW,empty-S and top metal plate from the
ones with 4mmfss all around with top metal plate.
2m
1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-40
-30
-20
-10
0
10
20
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-15
-10
-5
0
5
10
15
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

163
Figure 43:
Transmitting antenna is the biconical at the corner of the box between south and east, and
receiving antenna is the horn with vertical polarisation placed at 2m away from the side of box.
Red data are the raw data which result from subtraction of calibration with absorber-
NEW,empty-S and top metal plate from the ones with 4mmfss all around with top metal plate.
2m
1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-40
-30
-20
-10
0
10
20
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-15
-10
-5
0
5
10
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

164
Figure 44:
Transmitting antenna is the biconical and receiving antenna is the horn with Vertical
polarisation. Absorbers have been placed on opposite sides of FSS windows E, absorber-N with
top metal plate. Red data are the raw data which result from subtraction of calibration with
absorber NEW, empty-S and top metal plate from the ones with 4mmfss all around , absorber-
EN and with top metal plate.
0.5m
1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-40
-35
-30
-25
-20
-15
-10
-5
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-30
-25
-20
-15
-10
-5
0
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

165
Figure 45:
-
Transmitting antenna is the biconical in the centre and receiving antenna is the horn with
horizontal polarisation. Measurements with absorbers all around the three sides where
subtracted from measurements of the box with FSS and horn horizontally polarised.
Top view
1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-45
-40
-35
-30
-25
-20
-15
-10
-5
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

1.5 2 2.5 3 3.5 4 4.5 5
x 10
9
-30
-28
-26
-24
-22
-20
-18
-16
-14
-12
-10
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

166
Figure 46:
Red= raw data represents subtraction of data with Tx=horn Vp outside 50 cm away and with
Rx=biconical inside and absorber-NEW from same configuration but with absorbers gone and
replaced with 4mm fss N,E,W,S metal top.
Blue=red averaged by every 10 points
0.5m
Top view
2.4 2.6 2.8 3 3.2 3.4 3.6
x 10
9
-40
-30
-20
-10
0
10
20
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

2.4 2.6 2.8 3 3.2 3.4 3.6
x 10
9
-25
-20
-15
-10
-5
0
5
10
Frequency (GHz)
A
t
t
e
n
u
a
t
i
o
n

(
d
B
)

167

Frequency Selective Surface

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Department of Electrical and

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