Pd Doped TiO2 – CuO Mixed Metal Oxide Thin

Film Sensor for H2 Sensing Application

Bikram Biswas* Anup Dey Subhashis Roy
Department of E.T.C.E Department of E.T.C.E Department fo E.T.C.E
Jadavpur University Jadavpur University Jadavpur University
Kolkata, India Kolkata, India Kolkata, India
*bikram94biswas@gmail.com *anupetce@gmail.com subhashisaec@gmail.com
Subir Kumar Sarkar
Department of E.T.C.E
Jadavpur University
Kolkata, India
su_sircir@yahoo.co.in

Abstract— In this present work, high response Pd modified efficient by virtue of being low cost, room temperature
TiO2-CuO thin film hydrogen sensors have been prepared by using operation and simplicity.
sol-gel process. Prepared thin film was characterized by field
emission scanning electron microscope (FESEM). Sensitivity of In this proposed work, TiO2-CuO mixed metal oxide thin
hydrogen sensors was observed at operating temperature 500C- film has been prepared by the use of sol-gel technique. To
2500C and different gas concentrations (3000 ppm). It has been enhance the sensitivity of mixed metal oxides we
observed that Pd-doped thin film sensors have better responsivity incorporated PdCl2 solution on the top of thin film sensors.
in comparison with the un-doped thin film sensors. We found that, Pd/ TiO2-CuO thin film sensors obtained
better sensitivity in comparison with the undoped thin film
Keywords— Sol-gel-process, TiO2-CuO thin film, Pd- sensors. At operating temperature 1500C, proposed Pd-doped
modification, Surface morphology, H2 sensing. thin film sensors gets high sensitivity as compared to the
undoped prepared samples.
I. INTRODUCTION
Over the years, the fabrications of low size devices and II. EXPERIMENTAL DETAILS
reliable gas sensors with reduced power consumption have Sensitivity of the thin film sensor has been measured by the
attracted considerable attention [1-3]. In this substance, equation 1.
several studies have been discussed on hydrogen detection
due to safety reasons as an illustration, gas detection in Rn  Rg
industries, gas detection in food industries, environmental S (%)  100 (1)
gas detection, gas detection in biomedical and space Rn
applications. Hydrogen is an odorless, colorless, non-toxic,
Where, Rn is the resistance of the sensor in carrier gas (N2)
non-metallic, highly combustible diatomic and explosive gas.
and Rg is the resistance in the presence of hydrogen gas.
So, it is a major challenge to detect gas efficiently.
The experimental setup is shown in Fig. 1. and the device
Over the last few decades, the concentration
structure is shown in Fig. 3 Nitrogen has been used as a
measurement and detection of hydrogen gas leakage has
carrier gas with a mass flow controller (MFC) which controls
been done and various approaches proposed to realize
the gas flow and hydrogen as the target gas with a mass flow
hydrogen sensor with effective performance [4-6]. However,
meter (MFM) which controls the gas flow. Hydrogen and
the presently used H2 sensors have some drawbacks like low
nitrogen are mixed in the mixing chamber. The electrical
response time, recovery time and poor longevity. So there is
behaviour of the thin film sensors in presence of H2 and
a requirement of high performance H2 sensor for different
absence of H2 are measured by using agilent multimeter
industries.
(U1252A). Temperature of the measurement chamber is
Different metal oxides have been used for sensing controlled by the temperature controller.
material like ZnO, WO3, CuO, TiO2, Cr2O3, Mn2O3, Co3O4,
NiO, Ta2O5, La2O3, CeO2, Nd2O3 ,SrO, In2O3, V2O3, Fe2O3,
GeO2, Nb2O5, MoO3, [7]. Now-a-days, mixed metal oxides
are used for better sensing application. Some nobel metal are
used like (Pd, Pt, Au, Ag) to modified the surface of the
metal oxides for better sensitivity[8-10].These metal oxides
are useful for the detection of toxic gases like H2, CO, NO2,
CO2 etc.
Mixed metal oxide based sensor have been widely used
for gas detection. Various processes are available for
deposition of TiO2 -CuO mixed metal thin film, such as sol
gel process, RF sputtering, pulse laser deposition (PLD),
molecular beam epitaxy (MBE), metal organic chemical
vapor deposition (MOCVD) etc. Sol gel process is very
Fig. 1. Experimental Setup.

978-1-5386-6722-4/19/$31.00 ©2019 IEEE

 III. FABRICATION STEPS IV. DEVICE STRUCTURES

Fig. 3. (a) TiO2-CuO/p-Si (b)Pd/TiO2-CuO/p-Si

V. FESEM
Surface morphology (Field Emission Scanning Electron
Microscopy) of prepared thin film sensors are shown in the
Fig. 4 FESEM suggests that sol-gel grown metal oxides have
different polycrystalline size (78 nm-92nm). FESEM
characteristics also found that deposited Pd-doped TiO2-CuO
thin have sharper grain size in comparison with the
unmodified TiO2-CuO thin film allowing better adsorption
H2 in the letter case.

(a)

Fig. 2. Fabrication steps of prepared thin film sensor.

Fabrication steps of Pd modified thin film sensor for

detection of hydrogen is shown in the Fig. 2 In step (1), p-Si (b)
substrate is taken and cleaned. Afetr cleaning in step (2),
by using dip-coating meathod, prepared TiO2-CuO thin film
is deposited on the p-Si substrate. In step (3), PdCl2 solution
is prepared and deposited on the top of TiO2-CuO layer by
spin coating meathod (1200 rpm and 25 sec). Al metal
electrodes is formed in the step (4). In step (5), copper wire
is taken for connectivity of the prepared thin film devices.

Fig. 4. FESEM image of (a) undoped and (b) Pd-doped TiO2-CuO thin
film sensor.

Fig. 5. XRD pattern of Pd modified TiO2-CuO thin film sensor.
Fig. 5 shows the XRD peaks of Pd modified TiO2-CuO thin
film sensors at operating temperature 1500C. Prepared
sample clearly indicates that deposited nano film is available
in the sample which different peaks obtained at different
angles (2θ= 29.20-75.10).
VI. RESULT AND DISCUSSION
The variation of sensitivity w.r.t gas concentration changes is
shown in Fig. 6 With the increase in gas concentration the
sensitivity also increases and after 1100 ppm of
concentration the sensor shows highest sensitivity. After that
the sensitivity saturate because hydrogen gas molecules are
desorbed by the high conductive Pd/TiO2-CuO surface.
Fig. 6. Sensitivity vs gas concentration
How sensitivity has changed with operating temperature of
the sensor is shown in the Fig. 7 It has been observed that
the sensor has shown the highest sensitivity at the
temperature of 1500C. Pd modified TiO2-CuO sensor has
given the highest sensitivity compared to unmodified TiO 2-
CuO sensor.
Fig. 7. Sensitivity vs temperature.
VII. CONCLUSION
This work, TiO2-CuO thin film has been prepared by the
use of sol-gel synthesis technique. Surface morphology of
the prepared sample was characterized by FESEM. The
experimental result shows that hydrogen sensors huge affect
on prepared thin film TiO2-CuO samples. It also shows that
at Pd doped mixed thin film sensors obtained better
sensitivity (78%) in comparison to the undoped thin film. In
addition, we found that prepared mixed metal oxide thin film
sensors in the environmental monitoring had a huge impact
towards high sensitivity hydrogen sensing application. The
experimental results shows that TiO2-CuO based mixed
metal oxide thin film sensors are highly sensitive to
variations in H2 concentration and are hence sensible for H2
sensors.
ACKNOWLEDGMENT
The authors thankfully acknowledge the UGC UPE phase
II project Ref. No. R-11/183/17 fund for the financial support
and also acknowledge IC Design and Fabrication Centre and
School of Material Science and Nanotechnology, Jadavpur
University for providing infrustructure facilities to conduct
the present work.
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