Backscattering Spectrometry

Younes Sina
The University of Tennessee, Knoxville
ion-solid interactions
Interaction with:
Electrons
Nuclei
Such interaction will result in:
Ionization the electron is ejected from its atomic orbit
Excitation the electron is raised to an outer orbit
The interaction of an ion with an atomic electron is purely
Coulomb (i.e. interaction governed by the Coulombs law).
An ionized/excited atom will eventually return to its ground state,
accompanied by the emission of one or more x-rays/photons.
The interaction of an ion with an atomic nucleus can be
Rutherford scattering is also sometimes referred to as
Coulomb scattering because it relies only upon static
electric (Coulomb) forces, and the minimal distance
between particles is set only by this potential.
Elastic Backscattering Spectrometry (EBS)
(non-Rutherford) is used when the incident particle is
going so fast that it exceeds the Coulomb barrier" of
the target nucleus, which therefore cannot be treated
by Rutherfords approximation of a point charge. In
this case Schrdinger's equation should be solved to
obtain the scattering cross-section.
Ion Beam Analysis Techniques
TECHNIQUE ION BEAM
ENERG
Y
(MeV)
PIXE H
+
1 - 4
RBS
4
He
+
, H
+
s 2
ERDA
35
Cl+,
20
Ne+
2 - 40
NRA H+, D+ 0.4 - 3
Comparison of RBS,PIXE, and NRA methods
For Best choice Example
Channeling studies of crystal perfection
RBS
Surface studies involving some elements
that are difficult for RBS
Combination of
RBS and NRA
Surface coverage of O using
the
16
O(d,p)
17
Oreaction
Lattice location of impurities
(the impurity mass>>host atom mass)
RBS Lattice position of
As in Si, Ag in Zr
Light impurity element in a heavy-
element host lattice
NRA and
characteristic X-ray
H to S in a heavier lattice
Intermediate mass impurities in heavy
host lattice
Characteristic X-ray
Channeling studies
With single crystal targets, the effect of channeling also allows the investigation of the
crystalline perfection of the sample








S
c
a
t
t
e
r
i
n
g

y
i
e
l
d

(
c
o
u
n
t
s
)

Alignment of a Si (110) crystal for channeling
RBS spectra for a randomly oriented crystal and aligned crystal
random
aligned
Schematic diagrams for
(a) an amorphous layer
(b) random polycrystalline layers
(c) <2 off axis polycrystalline layers
Schematic diagrams for comparison
of align and random RBS
(a) sample
(b) spectrum
RBS makes it possible to investigate elemental content, composition
and element depth profiles of thin films.
The technique is quantitative since the following are well known:
K= (1680/2000)= 0.84
Mass Resolution
M
2
=(15/2000)(470) 4
M
2
=(15/2000)(210) 2
Energy
| | x S E = A
| | x N E . c = A
100 200 300 400 500 600 700
0
500
1000
1500
2000


Y
i
e
l
d
channel
<0001>
random
Sample 14-15
Zr
Al
O
7.9x10
15
Zr
+
/cm
2
E(keV)=2.61 keV/ch * ch + 123 keV
calibration

=
E
N
2

3
~
30

nm


| | x N E . c = A
Rutherford Cross Section
Unit: barn/ sr
1 b(barn)=10
-24
cm
2
Au
Si
The scattering cross section for a given Z
2
is Rutherford at energies below the line.
C Si
Non Rutherford
Rutherford
E0.2514+0.4=3.9
Summary
Examples
c N
dx
dE
=
For a compound of A
m
B
n
:

AB
=m
A
+n
B

B
AB
B
A
AB
A
AB AB
AB
N N N
dx
dE
c c
c
+ = =
|
.
|

\
|
Effects of energy loss of ions in solids
Atomic density
Stopping cross section
Molecular density
Atomic density
stopping power
Example:

Al
= 44x10
-15
eVcm
2

O
= 35x10
-15
eVcm
2

Al
2
O
3
=(2x44+3x35)x10
-15
=193x10
-15
eVcm
2
3
3 2
22
23
3
0
cm
molecules O Al
10 35 . 2
mol
g
102
mol
molecules
10 6
cm
g
4
3 2
=

= =
M
N
N
O Al
A
eV
46 10 193 10 35 . 2
0
15 22
3 2 3 2
3 2
= = =

|
.
|

\
|
c
O Al O Al
O Al
N
dx
dE
3
O Al
Al
cm
atoms Al
N
22 22
3 2
10 7 . 4 10 35 . 2 2 = =
3
22 22
3 2
cm
atoms O
10 1 . 7 10 35 . 2 3 = =
N
O Al
O
Calculate the stopping cross section and stopping power of
2 MeV
4
He
+
in Al
2
O
3
using Bragg rule
From appendix 3:
For a compound of A
m
B
n
:

AB
=m
A
+n
B

A
eV
46 10 193 10 35 . 2
0
15 22
3 2 3 2
3 2
= = =

|
.
|

\
|
c
O Al O Al
O Al
N
dx
dE
A
eV
46
eV
10 46 10 35 10 1 . 7 10 44 10 7 . 4
0
8 15 22 15 22
=
= + =

cm
}
= A
x
dx dx dE E
0
) / (
Example:
B
AB
B
A
AB
A
AB AB
AB
N N N
dx
dE
c c
c
+ = =
|
.
|

\
|
Depth scale
| | x S E = A
| |
(

|
.
|

\
|
+
|
.
|

\
|
=
2 1 cos
1
cos
1
u u
out in
dx
dE
dx
dE
K S
| | x N E . c = A
| |
|
.
|

\
|
+ =
2 1 cos
1
cos
1
u
c
u
c c
out in
K
x N E
AB
AB
A
A
c
= A
|
.
|

\
|
+ =
2
,
1 cos
1
cos
1
u u
c c c
AB
A out
AB
in
A
AB
A
K
}
= A
x
dx dx dE E
0
) / (
Energy loss factor
Stopping cross section factor
Depth resolution
Example
Calculate the depth- scattered ion energy differences
for 2 MeV
4
He
+
in Al
2
O
3

1
=0and
2
=10
K factor for
4
He on Al=0.5525
K factor for
4
He on O=0.3625
0
KE E =
1
MeV
E
Al
105 . 1 2 5525 . 0
1
= =
MeV
E
O
725 . 0 2 3625 . 0
1
= =
Using the surface-energy approximation
2 15 15 15
10 193 10 35 3 10 44 2 3 2
3 2
eVcm
O
in
Al
in
O Al
in

= + = + =
c c c
2 15 15 15
, , ,
10 240 10 46 3 10 51 2 3 2
3 2
eVcm
O
Al out
Al
Al out
O Al
Al out

= + = + =
c c c
2 15 15 15
, , ,
10 252 10 48 3 10 54 2 3 2
3 2
eVcm
O
O out
Al
O out
O Al
O out

= + = + =
c c c

AB
=m
A
+n
B

at E
0,surface
at E
1
|
.
|

\
|
+ =
2
,
1
0
cos
1
cos
1 3 2 3 2
3 2
] [
u u
c c
c
O Al
Al out
O Al
in
Al
O Al
Al
K
We can now calculate the stopping cross section factors
2 15 15 15
0
3 2
10 350 015 . 1 10 240 10 193 5525 . 0
] [
eVcm
O Al
Al

= + =
c
|
.
|

\
|
+ =
2
,
1
0
cos
1
cos
1 3 2 3 2
3 2
] [
u u
c c
c
O Al
O out
O Al
in
O
O Al
O
K
2 15 15 15
0
3 2
10 326 015 . 1 10 252 10 193 3625 . 0
] [
eVcm
O Al
O

= + =
c
Using the molecular density N
Al
2
O
3
=2.35x10
22
molecules/cm
3
we find:

| |
x x
N E
O Al
O Al
Al
Al

|
|
|
.
|

\
|
= = A
A
eV
0
3 . 82
3 2
3 2
0
c
| |
x x
N E
O Al
O Al
O
O

|
|
|
.
|

\
|
= = A
A
eV
0
6 . 76
3 2
3 2
0
c
Example
Surface spectrum height
1
0
0
cos ] [
) (
u
o
c
E Q E
H
O
=
Surface height of the two elemental peaks in the compound A
m
B
n
are given by
| |
1
0
0 ,
cos
0
m ) (
u
o
c
AB
A
A
A
Q E
H
E O
=
| |
2
0
0 ,
cos
0
n ) (
u
o
c
AB
B
B
B
Q E
H
E O
=
Energy width per channel
stopping cross section factors
Mean energy in thin films
) (
) (
1
0
Nt
E E
SEA
i
r
i
i SEA
in

A
=
=
c
Mean energy of the ions in the film ,
(1)
2
0
) 1 (
E
SEA
in
E E
A
=
) (
0
) , (
cos
Nt
N
t
SEA
i
E E
i
i i
i
E Q
A
=
O
=
=
u o
u
Surface Energy Approximation
E
0
E
1
E
2
For the second iteration, the values of (Nt)
i
(1)
should

be calculated using with

E=
(1)
then E
i
(1)
and
(2)

) , (
cos
u o
u
E Q
A
i
i i
i
N
t
O
=
) (
) 1 (
) 1 (
1
) 1 (
Nt
E
i
r
i
i
in
E

A
=
=
c
2
) 1 (
0
) 2 (
E
in
E E
A
=
Mean energy in thin films
E
0
E
1
E
2
Example
Calculate surface height for 2 MeV
4
He
+
on Al
2
O
3
:
=10
-3
sr
E=1

keV/channel
Q=6.24x10
13
incident particles (10C charge)

1
=0,
2
=10 (scattering angle=170)
From appendix 6:
R
Al
=0.2128x10
-24
&
R
O
=0.0741x10
-24
From previous example:
2 15
0
3 2
10 326
] [
eVcm
O Al
O

=
c
2 15
0
3 2
10 350
] [
eVcm
O Al
Al

=
c
| |
1
0
0 ,
cos
0
) (
u
o
c
AB
A
A
A
E Qm E
H
O
=
| |
cnt
E Q
O Al
Al
Al
Al H
76
10 350
10 2 10 24 . 6 10 10 2128 . 0
0
2
15
3 3 3 24
3 2 0 ,
=

=
O
=

c
o
| |
cnt
E Q
O Al
O
O
O H
43
10 326
10 3 10 24 . 6 10 10 0741 . 0
0
3
15
3 3 3 24
3 2 0 ,
=

=
O
=

c
o
For not too thick film
) ( ) (
0
) (
2
) (
Nt
E
E
Nt
SEA
i
f
i
f
|
|
.
|

\
|
=
E=
(f)
E
0
E
1
E
2
Sample analysis
Experimental Parameter Units Values
Analysis ion energy MeV 1.0-5.0
Beam cross section mm x mm 1.5x1.5
Beam current nA 10-200
Integrated charge C 5-100
Detector energy resolution for
4
He ions keV 15
Data acquisition time min 5-10
Vacuum Torr 2x10
-6
Pump-down time min 15
Typical experimental operating conditions and parameter ranges used during
acquisition of backscattering spectra
U
n
i
t

c
o
n
v
e
r
s
i
o
n
s

Multiply units by For units Example
MeV

MeV/amu 4 MeV
4
He ~ 1 MeV/amu


v/v
o
(MeV/amu)
1/2
v/v
o
=1~0.025 MeV/amu
1
H


(MeV/amu)
1/2
m/s 2 MeV
4
He ~ v
HE
=9.82x 10
6
m/s





10
15
atoms/cm
2

nm 10
18
Atoms/cm
2
For Au~170nm

g/cm
2

nm 100

g/cm
2
For C~258 nm

g/cm
2

10
15
atoms/cm
2
100 g/cm
2
For Au~305x10
15
atoms/cm
2
eV cm
2
/10
15
atoms

MeV/(mg/cm
2
) 100 eV cm
2
/10
15
atoms for
Al
2
O
3
~2.95 MeV cm
2
/mg
[M
2
= (2M
Al
+ 3 M
O
)/5; M
Al
=26.98,
M
O
=16.00]

eV cm
2
/10
15
atoms

keV/m 30eV cm
2
/10
15
atoms for Si~150
keV/m
] [ 1
1
amu M
] 3 / [
] [
10
661 . 1 2
2
cm g
amu M

] / [
10
3
cm
g
] [ 661 . 1
10
1
3
amu M
1581 . 0
10
389 . 1
7

] [ 661 . 1
1
2 amu M
] [ 661 . 1
] / [
10
2
3 2
amu M
cm
g
Thin-film analysis
The peak integration method
i
R
i
R
Bi i
E Q
DTR e C A
i Nt
) )( , ( '
cos
) (
1
o
o
u
u
o
O

=
Integrated peak counts
That can be accurately determined
from the spectrum
Non Rutherford correction factor
Correction factor
Dead time ratio
Integrated charge deposited
on the sample during the run
solid angle subtended by
the detector at the target
an application of the peak integration method of analysis of the two-element
thin film
E
0
=3776 keV
=170

1
=0

2
=10
=0.78 msr
C
Bi
=(0.990.03)
E=(3.7420.005)keV/channel
=(83) keV
K
Fe
=(170)=0.7520
K
Gd
=(170)=0.90390
E
1
= nE+
Example
Energy intercept
sr
cm
E
Fe
R
2
24 24
2
0
10 2469 . 0 10
776 . 3
521 . 3
) 170 , (

= =

o
sr
cm
E
Gd
R
2
24 24
2
0
10 510 . 1 10
776 . 3
53 . 21
) 170 , (

= =

o
998 . 0
3776
) 26 )( 2 )( 049 . 0 (
1
3 / 4
= =
|
.
|

\
|
Fe
R o
o
993 . 0
3776
) 64 )( 2 )( 049 . 0 (
1
3 / 4
= =
|
.
|

\
|
Gd
R o
o
From appendix 6
E
Z Z
CM
R
2 1
3 / 4
049 . 0
1 =
o
o
From
Example
Center-of-mass energy
From Trim 1985:
2 15
10 4 . 51 ) 3776 ( eVcm keV
Fe
= c
2 15
10 2 . 52 ) 3676 ( eVcm keV
Fe
= c
2 15
10 3 . 86 ) 3776 ( eVcm keV
Gd
= c
2 15
10 5 . 87 ) 3676 ( eVcm keV
Gd
= c
Example
008 . 1
) 20 1020 (
) 1 660 ( '
) 1 757 (
01 . 20 '
0 ,
=
=
=
=
=
DTR
cts
nB
nB
C Q
H
AB
A

cts
nA
nA
H
AB
B
) 20 640 (
) 1 812 ( '
) 1 910 (
0 ,
=
=
=
Integrated counts in spectral regions of interest (initial
and final channel numbers are listed:
Channels (789-918)=103978 cts; (920-960)=49 cts
Channels (640-767)=64957 cts; (768-788)=79 cts
Example
From: E
1
= nE+ and K
i
=E
i
1
/E
0
:
keV E n
B
B
E
) 6 2841 ( ) 3 8 ( ) 005 . 0 742 . 3 )( 1 757 ( '
1
= + = + = E
keV E n
A
A
E
) 7 3413 ( ) 3 8 ( ) 005 . 0 742 . 3 )( 1 910 ( '
1
= + = + = E
002 . 0 752 . 0
) 5 3776 (
) 6 2841 (
0
1
=

= =
E
E
K
B
B
002 . 0 904 . 0
) 5 3776 (
) 7 3413 (
0
1
=

= =
E
E
K
A
A
Therefore, element A and B are Gd and Fe, respectively. Note that element A
could also be Tb, because K
Tb
=0.9048
Example
Energy intercept
Calculation of elemental areal densities,(Nt)
Values of A
i
are calculated from the integrated counts in the
regions of interests
cts A
Fe
) 261 64475 ( ) 128 (
21
79
64957 = =
cts A
Gd
) 323 103823 ( ) 130 (
41
49
103978 = =
In this case, the background correction is almost negligible
Example
The areal densities in the surface-energy approximation,(Nt)
SEA

i

using E=E
0
2
24 3 6
19
) 998 . 0 )( 10 2469 . 0 )( 10 78 . 0 )( 10 01 . 20 (
) 10 602 . 1 )( 03 . 0 99 . 0 )( 008 . 1 )( 261 64475 (
) (
cm
atoms
Nt
SEA
Fe

=
2
18
10 ) 021 . 0 709 . 0 (
) (
cm
atoms
Nt
SEA
Gd
=
2
18
10 ) 08 . 0 68 . 2 (
cm
atoms
=
i
R
i
R
Bi i
E Q
DTR e C A
i Nt
) )( , ( '
cos
) (
1
o
o
u
u
o
O

=
DTR C
Bi
A
i
1
Q
0.998

e
Example
The mean energy of the
4
He ion in the film,
(1)
, is calculated (to first order)
using the following equation
) (
) (
1
0
Nt
E E
SEA
i
r
i
i SEA
in

A
=
=
c
For the first-order energy loss, E
SEA
in
,of the ions in the film:
2
0
) 1 (
E
SEA
in
E E
A
=
keV
eV
E E
Nt Nt
E
SEA
Gd
Gd
SEA
Fe
Fe SEA
in
199
) 10 709 . 0 )( 10 3 . 86 ( ) 10 68 . 2 )( 10 4 . 51 (
) ( ) (
18 15 18 15
0 0
) ( ) (
=
+ =
+ =

A c c
keV E 3676
2
199
3776
) 1 (
= =
Example
From the following Eq. we can calculate the areal densities:
) ( ) (
0
) (
2
) (
N
E
E
Nt
SEA
i
f
i
f
|
|
.
|

\
|
=
2 18
2
) 1 (
/ 10 54 . 2
) (
3776
3676
) (
cm atoms
N Nt
SEA
Fe Fe
= =
|
.
|

\
|
2 18
) 1 (
/ 10 672 . 0
) (
cm atoms
Nt
Gd
=
Example
Results of an additional iteration of this procedure using the
following equations we have: (Note that c
Fe
and c
Gd
are
evaluated at
(1)
)
eV eV
Ein
191 ) 10 672 . 0 )( 10 5 . 87 ( ) 10 54 . 2 )( 10 2 . 52 (
18 15 18 15
) 1 (
= + =

A
) (
) 1 (
) 1 (
1
) 1 (
Nt
E
i
r
i
i
in
E

A
=
=
c
2
) 1 (
0
) 2 (
Ein
E E
A
=
) ( ) (
0
) (
2
) (
Nt
E
E
Nt
SEA
i
f
i
f
|
|
.
|

\
|
=
eV
Ein
3681
2
192
3776
) 2 (
= =
A
2 18
2
) 2 (
/ 10 ) 08 . 0 55 . 2 (
) (
3776
3681
) (
cm atoms
Nt Nt
SEA
Fe Fe
= =
|
.
|

\
|
2 18
) 2 (
/ 10 ) 021 . 0 674 . 0 (
) (
cm atoms
Nt
Gd
=
Example
The average stoichiometric ratio for this film using the following Eq.:
) , (
) , (
.
u o
u o
E
E
A
A
N
N
m
n
B
A
A
B
A
B
= =
( )
( )
02 . 0 78 . 3
998 . 0
993 . 0
.
521 . 3
53 . 21
.
323 103823
) 261 64475 (
.
) 170 , (
) 170 , (
/
/
0
0
=

=
=
R
R
E
E
A
A
N
N
Fe
Gd
Fe
R
Gd
R
Gd
Fe
Gd
Fe
o o
o o
o
o

Example
If the molecular formula for the film is
written as Gd
m
Fe
n
, then:


m=0.2090.001 and n=0.7910.001
n+m=1
Example
The value of the physical film thickness:
nm cm t
Fe
302
10 44 . 8
10 55 . 2
22
18
=

=
E
l
e
m
e
n
t
a
l

b
u
l
k

d
e
n
s
i
t
y

3 22
0
/ 10 44 . 8 cm atoms
M
N
N
Fe
Fe
Fe
= =

3 22
0
/ 10 02 . 3 cm atoms
M
N
N
Gd
Gd
Gd
= =

nm cm t
Gd
223
10 02 . 3
10 674 . 0
22
18
=

=
nm t
GdFe
525 ~
Example
N N
AB
B
B
AB
A
A Nt Nt
t
) ( ) (
= =
) , (
cos
u o
u
E Q
A
i
i i
i
N
t
O
=
Areal density, Nt, as atoms per unit area
Detector solid angle
Integrated peak count
Incident ions
Cross section
Areal density
) , (
) , (
.
u o
u o
E
E
A
A
N
N
m
n
B
A
A
B
A
B
= =
The average stoichiometric ratio for the compound film A
m
B
n
Ratio of measured
integrated peak count
Cross section ratio
AB
AB
M
N m
N
AB
A
0
=
AB
AB
M
N n
N
AB
B
0
=
AB
AB
M
N m
N
AB
A
0
=
AB
AB
M
N n
N
AB
B
0
=
N N
AB
B
B
AB
A
A Nt Nt
t
) ( ) (
= =
B A AB nM mM M + =
n mB A
Physical film thickness