International Journal of Emerging Technologies and Engineering (IJETE)

Volume 1 Issue 9, October 2014, ISSN 2348 8050

CHARACTERIZATION OF ZNO NANOSTRUCTURE BASED METHANOL SENSOR

PREPARED BY SOL-GEL AND CHEMICAL BATH DEPOSITION
Sudhakar Rattan1, Vijay Kumar Anand2
1
M.Tech Scholar, ECE Department, ACE, Devsthali
2
Senior Assistant Professor, ECE Department, ACE, Devsthali

ABSTRACT
A ZnO nanostructure based methanol sensor prepared by
sol gel having average length of 599nm is reported in
this paper. A low temperature chemical bath deposition
technique is employed using zinc nitrate hexahydrate
and hexamethylenetetramineprecursor at 1000C on SiO2
substrate having sol gel grown seed layer. After
structural characterization (XRD, SEM) three types of
sensor structure designed using Aluminum electrode
.The .1M concentration sample shows better magnitude
response at 2500 C .While other sensor shows that at low
temperature less than 1500 C the sensor operates. The
possible sensing mechanism also discussed briefly.
Keywords CBD, Methanol Sensing, Sol Gel, ZnO
Nanostructure.

1. Introduction
The different gases for thin film sensitivity are discussed
by [13] so that there is a change in the grain boundary
resistance. [7] Shows the effect of number of coating on
seed layer and their effect on film thickness. Results
show that thickness increases linearly with number of
coating. The effect of heating, spinning speed, fume
exhaust and precise control of concentration of reactants
[5] strongly effects the crystallographic orientation. The
synthesis of nano composities using ferric nitrate and
ethylene glycol as precursor via sol gel method and the
effect of annealing temperature was studied. The
crystallite size increased with annealing temperature.
The effect of calcinations temperature was affected the
quantum size of ZnO crystal [3]. The nanocrystalline
thin film prepared by dip coating method was studied
[2].Of these methods CBD provides a low temperature,
fast, versatile and easily controllable method for the
synthesis of various ZnO nanostructures on a variety of
substrates [1]. The advantage of this method also
includes the possibility of large-scale production of such
structures and the low energy requirement. Though there
have been some reports regarding methane sensing with
sol-gel grown or electrodeposited ZnO thin films,

however methane sensing with CBD grown ZnO

nanostructure still remains somewhat less explored.
1.1 Problem Formulation
A number of opportunities in chemical gas sensor by
using different methodology. Firstly the application of
various classes of nanostructures that were synthesized
on a range of substrates by chemical bath technique
remains an area of great interest. Most of the gas sensors
are made up of gold electrode and different gases used
also the sensitization is required to improve sensitivity.
Further many sensors are made through spray pyrolysis
and different methods which are very costly. Most of the
sensor works at high temperature and finally
Semiconductor oxide based methanol gas sensor is very
less.
1.2 Objectives
To design and fabricate a sensor using Al electrode
and achieve the same sensitivity.
To design and fabricate a sensor using cost effective
technique.
To design and fabricate semiconductor oxide based
methanol gas sensor.
To design and fabricate a sensor which can be
operated at low temperature.

2. Experimental Procedure
The overall growth mechanism of ZnO nanostructure
was similar to that reported elaborately by Banerjee et. al
,[1]. The base seed layer of ZnO nanostructure is formed
by sol-gel technique by reacting Zinc Acetate dehydrate
(3gm) and 2-propanol(25ml) on SiO2 / p-Si<100>
substrate, 3ml diethaloamine was also added drop by
drop to get crystal clear solution. The samples were spin
coated a(3000 r.p.m) for 30 sec and put in annealing
furnance at 5000C for 1hr in nitrogen ambient and
subsequently ZnO seed layer was formed by thermal
decomposition of Zinc Acetate Dihydrates. To prepare
ZnO nanostructure, a 50ml solution was prepared by
mixing Zinc nitrate hexahydrate and
HMTA in
deionised water in different molar ration i.e. .1M,.0
204

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International Journal of Emerging Technologies and Engineering (IJETE)

Volume 1 Issue 9, October 2014, ISSN 2348 8050

1M,1M resp. The Substrate was immersed into the

solution for 3hr at 950C. Samples were allowed to rinsed
slowly with water, The length of nanostructure formed
in range of 599nm.

3. Sensor Fabrication
Three types of sensor structures were fabricated for
sensing methanol vapor. The details of sensor structures
are summarized in Table I.

Sample
S-1
S-2
S-3

Table 1
Nomenclature of Samples
Concentration
No.of Coatings
.1M
Single
.01M
Single
1M
Single

Figure 1 XRD Spectrum

4. Gas Measurement Study

For the purpose of testing the response of the
sensor, we used a vapor sensor setup.The setup consist
of conical flask in which methanol is deposited. The
carrier gas N2 is passed through methanol so that the
saturated methanol vapor was achieved. And the outlet
goes to mixing chamber where another N2 carrier gas is
directly inserted.Both the outlets are mixed in the mixing
chambr and the outlet from the mixing chamber is the
gas which should be passed on to the surface of sample.
The sensor was tested on different temperature and the
readings. should be observed through RISH Multi14S
multimeter. The resistance is measured both in air and
the gas passes on to the surface.

5. Result and Discussion

This shows improvement in Crystallinity of the films on

silicon substrate. In addition the value of full width half
maxima (FWHM) also suggesting betterment of
Crystallinity [1] with solution used to make seed layer
on silicon substrate.
5.2 Scanning Electron Microscopy
The surface topography of thin film is very important
tool to investigate microstructure of the films. Scanning
Electron Microscopy (SEM) micrograph of ZnO thin
film is shown in Fig 2 with presence of tightly packed
grains. The nanocrystals are regularly distributed on the
silicon substrate and crystallite size is approximately 4691nm. It can be seen that the small grains made a smooth
and transparent surface similar to those observed by
other author [5].It is observed that the nanostructure is
uniformly distributed over the ZnO film. The average
diameter of the nanorods absorbs ~ 599 nm and having
hexagonal cross section. Fig 2 shows the ZnO nanorods
arrays over film annealed at 500C.

5.1 Diffraction Peaks and FWHM

The (101) diffraction peak appeared at 36.24 for
sample S-1, while (002) peak located at 34.42, 34.67
was the most intensive respectively for sample S-1 , S-2
as shown intable 5.1,indicating that samples S-1, S-2
were oriented along c-axis perpendicular to the substrate
surface All the dominating peaks were matched with the
results available in literature [4,29]. FWHM value (Table
5.1) corresponding to dominating peaks are lower for
different solution used for making seed layer.
s.no
1
2
3

peak
101
002
100

2theta(0)
36.2409
34.4279
31.7834

FWHM(0)
0.1673
0.2175
0.1171

Figure 2 SEM Micrograph of Sample S3

[1M] (edge view)
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International Journal of Emerging Technologies and Engineering (IJETE)

Volume 1 Issue 9, October 2014, ISSN 2348 8050

The average diameter of the nanorods absorbs ~ 599 nm

and having hexagonal crosssection. Fig 2 Shows the
ZnO nanorods arrays over film annealed at 500C
5.3 Response Magnitude Curve
It can be investigated that at room temperature none of
the sensor shows the response magnitude. While all the
sensor shows some response magnitude from 1000C
temperature. From graph it is clear that the optimum
temperature for different samples is obtained at different
temperatures. Sample S-1 get its optimum temperature at
2500C with response magnitude 67.89.After that its
response magnitude gets decreases continuously. Sample
S-2 gets its optimum operating point obtained on
temperature at 3000C.After that its response magnitude
gets decreases. Its response magnitude obtained is 48.30
80

Response Magnitude (%)

70
60

50
40

S-1

30

S-2
S-3

20
10

concentration with a moderate response magnitude with

a rather slow response time.
But our results shows that from 1500C temperature the
sensor S-3 shows response magnitude of 48.30 which is
better than Al doped ZnO thin film response magnitude
at temperature 2750C.

6. Conclusion
It is concluded that the ZnO nanostructure based
methanol sensor using Al electrode and prepared by the
cost effective technique shows some improvement as
compared to the gold electrode used by [1]. So it is
better to design and fabricate a sensor using Al electrode
and cost effective technique i.e. sol gel is better for
Practical applications. The chemical bath deposition of
ZnO thin films and the effect of different molar
concentrations of the mixtures on the morphologies are
analyzed.The structural characterization of prepared
films has been done. The lattice constants are lies in the
range as per standard values .The maximum grain size of
the film matched with the proposed grainsize. Crystal
structure obtained is hexagonal and plane orientation is
obtained at <002> . Results obtained from scanning
electron microscopy for molar ratio of mixtures shows
the length of nanostructure and the testing result is
comparable with the proposed results. By using Al
electrodes a semiconductor oxides based methanol gas
sensor is fabricated and have a comparable sensitivity as
per proposed criteria.

References
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100
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250
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Tempreature (0c)

Figure 2 Response Magnitude Vs temperature

Also when the ZnO structure is exposed to the methanol
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temperature of excess of 2000C for different

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International Journal of Emerging Technologies and Engineering (IJETE)

Volume 1 Issue 9, October 2014, ISSN 2348 8050

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