Journal of Applied Science and Engineering, Vol. 17, No. 1, pp.

31-38 (2014)

DOI: 10.6180/jase.2014.17.1.05

A Comparison Study on Hydrogen Sensing

Performance of MoO3 Nanoplatelets Coated with a
Thin Layer of Ta2O5 or La2O3
J. Yu*, Y. Liu, F. X. Cai, M. Shafiei, G. Chen, N. Motta, W. Wlodarski,
K. Kalantar-zadeh and P. T. Lai
1

Department of Electrical and Electronic Engineering, The University of Hong Kong,

Hong Kong, SAR
2
School of Chemistry, Physics and Mechanical Engineering, Institute of Future Environments,
Queensland University of Technology, Australia
3
School of Electrical and Computer Engineering, RMIT University, Australia

Abstract
There has been significant interest in developing metal oxide films with high surface
area-to-volume ratio nanostructures particularly in substantially increasing the performance of
Pt/oxide/semiconductor Schottky-diode gas sensors. While retaining the surface morphology of these
devices, they can be further improved by modifying their nanostructured surface with a thin metal
oxide layer. In this work, we analyse and compare the electrical and hydrogen-sensing properties of
MoO3 nanoplatelets coated with a 4 nm layer of tantalum oxide (Ta2O5) or lanthanum oxide (La2O3).
We explain in our study, that the presence of numerous defect traps at the surface (and the bulk) of the
thin high-k layer causes a substantial trapping of charge during hydrogen adsorption. As a result, the
interface between the Pt electrode and the thin oxide layer becomes highly polarised. Measurement
results also show that the nanoplatelets coated with Ta2O5 can enable the device to be more sensitive (a
larger voltage shift under hydrogen exposure) than those coated with La2O3.
Key Words: Hydrogen, Gas Sensor, Metal Oxide, Heterostructure

1. Introduction
The rise of nanotechnology and the ability to organise and restructure matter at the nanoscale, have
brought forth the development of cheap, low-power,
miniaturized sensors with enhanced performance. As
such, hydrogen sensors are important and have become a
core component in clean and renewable energy related
instruments. Devices which convert hydrogen gas to energy, such as internal-combustion engines, turbines and
fuel cells, all require high-performance and responsive
sensors, due to the highly volatile nature of hydrogen
gas, especially when applied as a fuel [2].
*Corresponding author. E-mail: jcwyu@hku.hk, yu.jerrycw@gmail.com

Sensors based on Pt/metal oxide/semiconductor

Schottky diode have arisen as one of the most favourable
choices for industrial applications due to their simplicity,
lightweight and portability. They have demonstrated
many innovative advantages such as sizable down-scaling and also adaptability and compatibility with existing
electronic based technologies [3]. The performance of
sensors that have implemented nanostructured metal oxide materials have been shown to excel far beyond those
with bulk-based materials in terms of sensitivity and response time [4,5].
In terms of sensing performance, as we continue to
scale the dimensions of a sensor down to incredibly
smaller size, it would inevitably assign a decrease in the
surface area available for interaction with a gas. Thus,

32

J. Yu et al.

the main advantage in implementing a nanostructured

thin film for sensing applications comes from addition of
a metal oxide layer which the first necessary step that can
be used to increase the surface area-to-volume ratio of
the morphological surface. Whilst preserving the surface
morphology, we can apply a second step by the modification of the surface quality by adding an ultrathin metal
oxide layer to maximise the effectiveness of the materials surface.
In this work, the authors designate two high-k metal
oxides (Ta2O5 and La2O3) to be deposited as an ultra-thin
layer on MoO3 nanoplatelets. By adding this thin layer,
the resulting structure of the sensor resembles that of
thin-film devices based on quantum heterostructures [6].
A high-k layer is commonly implemented in many highperformance electronic devices to suppress the problematic leakage current. However, in this work, we aim to
make use of the defects in the high-k metal oxide for effectively trapping the hydrogen adsorbate charge to induce a stronger polarisation at the interface between the
Pt electrode and the metal oxide layer. In addition, this
can provide a new method for low-temperature (or RT)
sensor and thus save power.

2. Experimental
2.1 Preparation of Substrates
The nanoplatelet MoO3 films were grown by thermal
evaporation on 6H-SiC n-type substrates (Tankeblue Co.),
the motivations behind the choice of our deposition parameters are explained in our previous work [7,8]. The native SiO2 layer was removed by etching the wafers in 10%
HF + H2O and an electrode of Ti and Pt, with thicknesses
of 40 and 100 nm, respectively were deposited on the
backside of the wafers using electron beam evaporation.
The wafers were diced into 5 5 mm2 substrates and annealed at 500 C to form the ohmic contact. A second
cleaning process was performed using the same HF process to remove the SiO2 layer from the polished side of the
substrate, which is formed during the annealing process.
Subsequently, the prepared substrates were cleansed in
acetone, isopropanol, DI water and blown dry with N2 gas.
2.2 Growth of Nanoplatelets Films
The source was prepared by weighing 10 mg of MoO3

powder (China Rare Metal Material) on an alumina boat,

placing it at the centre of a (18 mm inner diameter and 680
mm length) quartz tube furnace. The SiC substrates were
placed on another alumina boat at a distance of 16 cm from
the source. A flow of gas with 10% O2 in Ar at 800 sccm
was initiated and the thermal deposition was performed
by heating to 770 C for 30 min at a rate of 2 C/min. The
cooling process was controlled at the same rate.

2.3 Deposition of Thin Sensing Layer

The fabrication of Ta2O5 and La2O3 thin film layers
were performed by RF sputtering deposition in a Denton
vacuum discovery sputtering system as per our works
referenced in [9,10]. The thickness of the Ta2O5 and
La2O3 high-k layers were calibrated by depositing at a
power of 15W RF separately for 350 sec approximately
on dummy wafers. The thickness achieved was approximated as 3.7 nm (with a mean square error of 0.623) as
measured by a VB400 Spectroscopic Ellipsometer software (Cauchy model). Deposition of the high-k layers
were then repeated for the nanoplatelet films.
2.4 Material Characterisation
The surface morphology of the deposited MoO3
nanostructures was characterised by scanning electron
microscopy (SEM) via a FEI Nova NanoSEM. X-ray diffraction (XRD) analysis was conducted using a Brucker D8
Advance to determine the difference in crystallographic
structure for the uncoated MoO3 films, and those coated
with Ta2O5 and La2O3. Transmission electron microscopy (TEM) was performed via a JEOL 1010 determine
the thickness of the RF sputtered high-k layer.
2.5 Formation of Schottky Contact and Testing
Methodology
Using a shadow mask, a circular pad of Pt with diameter of 1 mm was deposited by the PECS sputter, via
a lift-off process. The deposited thickness was 30 nm as
determined by a calibrated built-in quartz crystal thickness monitor.
In this work, the configuration of the developed sensors is of the form Pt/high-k thin film/MoO3 nanoplatelets on SiC. Electrical and hydrogen-sensing tests
were performed in a multi-channel gas testing system as
explained in our previous work [7-10].

A Comparison Study on Hydrogen Sensing Performance of MoO3 Nanoplatelets Coated with a Thin Layer of Ta2O5 or La2O3

3. Results and Discussion

3.1 Surface Morphology and Crystallographic
Structure
Analysis of the surface morphology of the as-deposited MoO3 nanoplatelets conducted by SEM is
shown in Figure 2. The insets of the figure illustrate the
TEM analysis of the selected area of the MoO3 nanoplatelets subsequent to the RF sputtering of Ta2O5 or
La2O3 (Figure 2).
The arrows in the micrograph indicate the thickness
of the deposited layer to be approximately 4 nm, verifying the modelling estimate as measured by ellipsometry.
The crystallographic structure of the MoO3 nanoplatelets, with Ta2O5 and La2O3 as measured by XRD is

Figure 1. SEM of the MoO3 nanoplatelets deposited onto SiC

by thermal evaporation (insets shows TEM of the 4
nm RF sputtered Ta2O5 and La2O3 thin film).

Figure 2. XRD diffractograms of the MoO3 nanoplatelets [1]

deposited onto SiC by thermal evaporation with the
presence of Ta2O5 (as indicated by hollow squares)
and La2O3 (as indicated by the filled circles).

33

shown in Figure 3. The results from the XRD also show

that the original MoO3 crystal structure is preserved [1,8]
with the exception of additional peaks of Ta2O5 for the
sputtered Ta2O5 layer. Similar observations can be made
for the MoO3 nanoplatelets with sputtered La2O3 layer.
These characterisation results indicate that the sputtered
Ta2O5 and La2O3 layers can be deposited onto the MoO3
nanoplatelets as a thin layer while preserving the surface
morphology.

3.2 Electrical and Static Hydrogen Sensing Properties

The measured current-voltage (I-V) characteristics
of the developed hydrogen sensors as exposed to synthetic air and dilute hydrogen ambience at various temperatures are shown in Figure 3.
The hydrogen sensing mechanism is based on the
catalytic dissociation of hydrogen and the hydrogen adsorption mechanism as per described in literature [11].
Hydrogen atoms that adsorb into the Pt catalyst metal
polarise and induce a dipolar charge layer at the interface
between the Pt electrode and the surface of the metal
oxide. We will subsequently characterise the build-up of
this dipolar charge in terms of barrier height lowering at
the interface and also change in the dielectric constant of
the metal oxide in the next section.
To simply characterise the static performance of the
sensors developed in this work, we calculate the sensitivity parameter (SF) under forward-bias mode of op-

Figure 3. Current-voltage characteristics of the pure MoO3

nanoplatelets, La2O3 and Ta2O5 coated nanoplatelets based hydrogen sensor as exposed to an air and
diluted hydrogen ambience at (a) 25 C; (b) 140 C;
(c) 220 C; (d) 300 C.

34

J. Yu et al.

eration. SF is defined as [12]:

(1)
where IH2 and Iair are the forward current measured in a
hydrogen ambience and in air ambience, respectively.
The value for SF as determined by Equation (1), and
voltage shift (DV) under a 100 mA constant current
mode of operation, are shown in Table 1. The results indicate that the Ta2O5 coating can give the device significantly higher hydrogen sensitivity than the La2O3 coating. We will further analyse the electrical properties in
terms of two different conduction mechanisms.

3.3 Change in Barrier Height and Dielectric Constant

In further analysis on the electrical properties of
these sensors, we assume that the current density (J) can
be modeled by the Schottky diode theory. Therefore, based
on the thermionic emission (TE) conduction mechanism,
charge carriers flow by climbing over an energy barrier
(the barrier height) at the interface according to the forward J-V equation as given by [13]:

height and the change in barrier height (df) with respect

to the exposure to hydrogen gas (1% concentration in
air) for different temperatures were calculated from the
J-V data in Figure 3. The low-field region between 0.1 V
and 0.3 V was selected for these calculations at 100 mA,
in order to increase the accuracy of the results. The calculated values for the above parameters and are plotted
in Figure 4.
From the results in Figure 4, we anticipated that the
change in barrier height would increase with respect to
increasing temperature. However, it appears that in Figure 5, the results (not shown) increasingly diverage and
exceed the values that have been considered reasonable
in the literature [10,14]. Therefore, to explain this discrepancy, we assume that there is an additional conduction mechanism other than TE. By calculating the ideality factor (as presented in Table 2) from the J-V data (Figure 3) using Equation 2, we observe that the nanoplatelets with either Ta2O5 or La2O3 coating exhibit a far stronger non-ideal behaviour than the pure MoO3 nanoplatelets. This indicates that there could likely be surface

(2)
where A** is the effective Richardson constant; T is the
absolute temperature; q is the electron charge; fB is the
effective barrier height; VF is the forward applied voltage; h is the ideality factor; and k is Boltzmanns constant.
Using Equation (2) from the TE model, the barrier
Table 1. The sensitivity (SF) and voltage change (DV) at
100 mA, exhibited from the MoO3, La2O3/MoO3
and Ta2O5/MoO3 nanoplatelets based MIS-type
sensor diodes exposed to air and 1% diluted
hydrogen ambience at different temperatures
MoO3 [1]
T (C)
25
140
220
300

La2O3/MoO3

Ta2O5/MoO3

SF

DV (V)

SF

DV (V)

SF

DV (V)

0.74
0.22
0.53
0.07

0.03
-

0.95
1.22
3.71
7.52

0.09
0.41
0.81
1.13

0.27
2.85
9.32
9.43

0.15
0.74
1.20
1.11

Figure 4. Effective barrier height fB (as denoted by the hollow circles) and dielectric constant k (as denoted by
the filled squares) for the MoO3 nanoplatelets, with
and without La2O3 and Ta2O5 coating at different
temperatures. The thermionic emission (TE) model
is found to be dominant allowing for an accurate
calculation of the effective barrier height, from 25
C to 350 C for the uncoated MoO3 and from 25 C
to 140 C for the MoO3 with the coatings. Thus,
from 180 C to 300 C, the Poole Frenkel (PF)
mechanism is dominant, allowing for the calculation of the dielectric constant for the nanoplatelets
with La2O3 and Ta2O5.

A Comparison Study on Hydrogen Sensing Performance of MoO3 Nanoplatelets Coated with a Thin Layer of Ta2O5 or La2O3

35

Table 2. The calculated values for the ideality factor h of

the MoO3, La2O3/MoO3 and Ta2O5/MoO3
nanoplatelets based sensor diodes
T (C)
25
140
180
220
260
300

Figure 5. Plot of the effective change barrier height dfB (as

denoted by the hollow circles) and effective change
in dielectric constant Dk (as denoted by the filled
squares) for MoO3 nanoplatelets, and Ta2O5 and
La2O3 coated MoO3 nanoplatelets.

and bulk traps in the thin coating layer which significantly influences the flow of current. Therefore, for simplicity we will consider these traps as defect traps and
examine the electrical properties in terms of the trap-assisted conduction mechanism (also known as Poole
Frenkel emission).
In classical mechanics, we presume that if numerous
defects are present in the thin high-k layer, charge carriers that flow in their proximity to these defects can
undergo trapping and de-trapping processes at the interface. In quantum mechanics, electrons have a probability
where they can exist inside the potential well (defect
trap) before tunneling through to the other side. With sufficient thermal energy, these traps can be thermally activated and provide carriers and alternative pathway to
flow through the energy barrier. Poole-Frenkel (PF)
emission models this behaviour quite effectively from a
classical viewpoint. In this model, the dielectric constant
(k) can be deduced from the slope of the forward bias
semi-log J-V1/2 characteristics using Equation (3) as
given by [15]:

La2O3/MoO3

Ta2O5/MoO3

1.77
1.20
1.12
1.15
1.06

5.22
4.42
3.97
4.03
3.93
3.43

5.92
4.40
4.24
4.19
4.26
4.26

In this work, we have selected a high-field region

between 1.5 V and 2.0 V to obtain a reasonable k-value,
as the PF model is suited for this region of data as plotted
in Figure 4.
Secondly, the TE mechanism that is present in these
coated nanoplatelets can overlap with the Poole Frenkel
(PF) emission due the traps in the RF sputtered high-k
layer. The forward bias condition was selected instead of
reverse bias as our previous investigations [7] and [10]
assumed pure TE to be present, however in this case, by
applying a high reverse bias voltage there can also be
contribution by Fowler-Nordheim tunnelling which can
often dominate over PF emission and therefore affect the
accuracy of our interpretation using the PF emission
model [16].
The significance of the values for the barrier height
and k-value of the sensors as calculated in Table 2 and
Table 3 tells us that at temperatures below 180 C, the
dominant conduction mechanism should be TE. Although
Table 3. Dielectric constant (k) and effective change in
dielectric constant (Dk) of La2O3/MoO3 and
Ta2O5/MoO3 nanoplatelets based sensors as they
are exposed to air and 1% diluted hydrogen
ambience at different temperatures. Values that
are highlighted with a * indicate a possible
overlap in conduction mechanism with
Thermionic Emission (TE)
T (C)

(3)
where C is a proportionality constant; WT is the activation energy of the traps; E is electric field across the thin
film; k and e0 are the dielectric constant of the thin film
and the permittivity of vacuum, respectively.

MoO3 [ref]

25
140
180
220
260
300

La2O3/MoO3

Ta2O5/MoO3

Dk

Dk

053.6*
035.7*
28.8
29.6
28.2
20.7

.-4.4*
.-0.6*
1.4
1.0
0.3
1.6

064.4*
035.3*
33.0
32.1
33.2
33.1

00.6*
00.8*
0.9
1.0
1.1
1.2

36

J. Yu et al.

the calculated change in effective barrier height gives a

reference to how much df in Figure 5 continues to increase with respect to temperature, it does not provide
enough information to conclusively speculate whether
these results are reasonable. However, from the PF results we can argue that there is evidence to suggest that at
temperatures roughly above 140 C, there is a clear transition of results making PF emission the dominant conduction mechanism. This is due to the activation of the
defect traps (assuming they are from the Ta5+ or La3+ atoms) at the surface (and bulk) of the high-k metal oxides,
and the results show consistency in the estimated k-value
as approximately 28 for La2O3 and 33 for Ta2O5 -coated
MoO3 nanoplatelets. We have displayed the results
which should be invalid below 180 C in the PF plot to
show the validity of this argument.

3.4 Dynamic Hydrogen Sensing Performance

In comparing the operating speed for hydrogen sensing applications, the dynamic response of the Ta2O5 and
La2O3 -coated MoO3 nanoplatelets is shown in Figure 6.
The sensors are operated below 300 C as the morphology of the nanoplatelets begin to deform above these
temperatures [8]. Thus, we chose to study and compared
the sensors at 220 C in terms of a potential difference
(voltage shift). This voltage shift is induced by the dipolar charge caused by the adsorption of hydrogen and
as compared to our previous work, the additional coating
layer increases the trapping of charge as per proposed in
this investigation [10,14].
From the dynamic response (as shown in Figure 6),
we can see that the voltage shift of the Ta2O5-based sensor is larger than that exhibited by the La2O3-based sensor. This implies that the Ta2O5 layer has a better capability to hold the adsorbate charge as compared to La2O3.
The implications of our results and principal advantage in modifying the metal oxide nanostructured surface
is to further increase the sensitivity (change in voltage),
which effectively also allows the resolution of the sensor
to be improved. Yet, in our previous work we observed
that there is clearly a trade-off between the above advantages and dynamic performance, in particular the
response and recovery time.
The aforementioned advantages are also dependent
on the operating temperature. As we have shown in this

work there is a transition from TE to PF emission and in

some instances, PF has undesirable effects, as it can
cause the consumption of applied potential difference in
order to maintain a constant current to flow across the
traps [17]. However in this case, as the PF emission is
clearly dominant at temperatures greater than 140 C and
thus, we have selected a temperature 220 C for the analysis of the sensing performance as at low temperatures
the sensitivity is very low. Our results also implies that
these traps will need to be thermally activated and thus
give the sensor an optimal operating temperature range.
We have calculated our voltage shift, response and
recovery time from Figure 6 as presented in Table 4.
We can deduce from the response and recovery time
results, that the La2O3 based sensor reaches saturation
quicker than the Ta2O5 based sensor across all hydrogen
concentrations. As the La2O3 sensor responds quicker,
the results suggest that the sensor based on this material
can accumulate charge at across the Pt/La2O3 interface
and the La2O3 layer at a greater rate than at the Pt/Ta2O5
interface. We also consider that when adsorbate charge is
accumulated at the Pt/oxide interface, it can also induce
an image force charge at the other side of the thin layer
[13] which increases the intensity of the overall change
in polarisation (or change in potential difference) over
the thin layer.
However, the results from the recovery time also
show that when the hydrogen source is removed, charge
is depleted from the Pt/La2O3 interface at a slower rate as
compared to that from Pt/Ta2O5 interface. These results

Figure 6. Dynamic hydrogen sensing performance of the

Ta2O5 and La2O3 coated MoO3 nanoplatelets as exposed to different concentrations of H2 gas for 5
min at 220 C, under 100 mA bias current.

A Comparison Study on Hydrogen Sensing Performance of MoO3 Nanoplatelets Coated with a Thin Layer of Ta2O5 or La2O3

37

Table 4. (a) Voltage shifts, (b) response and (c) recovery time for Ta2O5 and La2O3 coated MoO3 nanoplatelet sensors
towards hydrogen with different concentrations at 220 C under 100 mA bias current
Sensor

Parameter

H2 Concentration (ppm)
600

1250

2500

5000

10000

0.13
0.14

0.27
0.22

0.51
0.41

0.79
0.61

1.07
0.85

162
156

171
170

183
168

120
102

090
075

363
558

370
432

270
588

429
582

645
912

Voltage shift (V)

Ta2O5/MoO3
La2O3/MoO3
Response time (secs)
Ta2O5/MoO3
La2O3/MoO3
Recovery time (secs)
Ta2O5/MoO3
La2O3/MoO3

could signify that the traps in La2O3 are located deeper

than the traps in Ta2O5 and further work is required to investigate and understand the origin of this behaviour. In
terms of the response magnitude, the results indicate that
the Ta2O5 coating provides a stronger response which
signifies a better sensitivity and resolution for the sensor.

Ta2O5 layer provides better trapping of the adsorbate

charge than the La2O3 layer. As metal oxide based sensor
technologies will likely continue to employ high-k dielectrics in the future, it will be necessary to further our
control and understanding of defect traps in order to
further improve sensor functionality and performance.

3.5 Future Work

In this work, we have examined the effects of adding
a thin layer of Ta2O5 or La2O3 on MoO3 nanostructured
metal oxide. As we can see from the results, we can observe that there is a significant improvement in terms of
sensitivity, however dynamic response is still rather slow
(up to three minutes) as compared to other previous
works [7-9]. Therefore, there is a need to further improve sensors that employ a high-k metal oxide as its surface layer, by examining the effects of passivation methods on the defect traps or rather to dope the layer with
other materials to increase its overall conductivity. The
implications of such work can serve as a basis for future
studies in the fields of electronics and gas sensing.

Acknowledgements

4. Conclusions
In this work, we have presented how the addition of
Ta2O5 and La2O3 thin films substantially improves the
hydrogen sensing performance of MoO3 nanoplatelets.
By comparing their results, we establish that there is a
transition in the dominant conduction mechanism from
thermionic emission to Poole-Frenkel emission between
140 C and 180 C. By examining the changes in barrier
height and dielectric constant, we can conclude that the

The authors of this work would like to acknowledge

the CRCG Small Project Funding (201109176240) and
the University Development Fund (Nanotechnology Research Institute, 00600009) of The University of Hong
Kong.

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Manuscript Received: May 24, 2013

Accepted: Feb. 22, 2014