Copyright © 2014 by American Scientific Publishers

All rights reserved.

Printed in the United States of America
Science of Advanced Materials
Vol. 6, pp. 1–7, 2014
(www.aspbs.com/sam)

Low Operable Temperature Chemiresistive

Gas Sensing by Graphene-Zinc Oxide
Quantum Dots Composites
K. R. Nemade and S. A. Waghuley∗
Department of Physics, Sant Gadge Baba Amravati University, Amravati 444602, India

ABSTRACT
Chemiresistors based on graphene-ZnO QDs composite have been fabricated and tested for CO2 detection.
Structure and morphology of composites were analysed through X-ray diffraction, high resolution-transmission
electron microscopy, and Raman spectroscopy. The optical properties were studied through ultraviolet-visible
and fluorescence spectroscopy. The graphene-ZnO chemiresistor exhibits significant sensing response at low
operating temperature and it enhanced linearly with addition of graphene. The 80 wt.% graphene-ZnO chemire-
sistor exhibits the highest sensing response among all chemiresistors, low operating temperature, high selec-
tivity, good stability, and fast response and recovery time. The particle size effect and defects chemistry was

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employed to analyse the enhancement in sensing response with an increase in wt.% of graphene. Also, there
was excellent correlation observed between the defects density and sensing response as a function of wt.% of
graphene.
KEYWORDS: Chemiresistor, Sensing Response, Defect Density.

1. INTRODUCTION Graphene exhibits remarkably good gas sensing proper-

Rising carbon dioxide (CO2
levels in atmosphere is
mainly responsible for increased global warming. There
are many processes including industrial revolution, which
inevitably produce CO2 . As CO2 is an essential part of
earth atmosphere, it constantly being exchanged among the
atmosphere, sea, and soil surface. Ocean absorbing carbon
dioxide (CO2
from the atmosphere, this result in ocean
acidification and subsequently cause to climate change.1
Thus, there is much need of monitoring CO2 concentration
at low operating temperature and concentration. In the vast
area of chemical sensors, mostly sensors based on metal
oxide are known to be promising due to their fast response
than any other materials, but high operating temperature2 3
and poor stability4 are the serious problems. Also, the high
operating temperature results in enhancement of the opera-
tion cost. Therefore, development of low cost CO2 sensors
for an effective monitoring is required. Correspondingly,
the low level monitoring of CO2 is essential in a variety of
biology and chemistry experiments including biochemistry
of healthy respiration system. Hence, the present work
comprises a bold attempt to develop a chemiresistor based
upon graphene-ZnO composite as a sensing material.
∗
Author to whom correspondence should be addressed.
Email: sandeepwqghuley@sgbau.ac.in
Received: xx Xxxx xxxx
Accepted: xx Xxxx xxxx
ties due to fast adsorption process.5 6 Graphene decorated
with metal oxides can modify electronic properties and
materialize with potential results.7 Whereas, zinc oxide
(ZnO) is one of the most important material demon-
strated as a chemical sensors. Chu et al. reported the ace-
tone sensing properties of ZnO based chemi-senosrs.8 Bal
et al. explored the ammonia sensing characteristics of ZnO
based material.9 Wu et al. firstly reported the graphene-
ZnO nanocomposite synthesized through solvothermal
method.10 Chen et al. verified the electrochemical prop-
erties of ZnO/reduced graphene oxide.11 Chang et al.
demonstrated the gas sensing properties of SnO2 -reduced
graphene oxide composites towards the ethanol and H2 S.12
Singh et al. reported the remarkable room temperature gas
sensing of CO and NH3 and photoluminescence properties
of ZnO decorated graphene oxide sheets.13
In the light of above discussion, present work is
designed in view of the possibility of finding gas sens-
ing response in graphene-ZnO quantum dots (QDs) com-
posite. From literature survey, it is observed that few
reports are made on graphene-ZnO composites and this
is the first time, we investigate CO2 sensing properties
of graphene-ZnO QDs composite. The CO2 sensing prop-
erties of materials were studied at room temperature as
a function of concentration of gas as well as tempera-
tures. The chemiresistor shows the high sensing response,
low operating temperature, fast response, and recovery and

Sci. Adv. Mater. 2014, Vol. 6, No. 1 1947-2935/2014/6/001/007 doi:10.1166/sam.2014.1691 1

 Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites
good stability. The gas sensing mechanism for prepared
chemiresistors analysed by using defects chemistry. Our
experiment results; clearly shows that graphene-ZnO com-
posites chemiresistors operable at low temperature, this
reduced the operation cost significantly.
2. EXPERIMENTAL DETAILS
2.1. Synthesis of Graphene-ZnO QDs Composites
The analytical grade (SD Fine, India) chemicals were used
in this work. The ZnO QD was arrested by one pot chem-
ical route. The 1 M hexamethylenetetramine (HMT) was
dissolved in 10 ml distilled (DI) water separately. After
rigorous stirring, 1 M zinc nitrate was added into the solu-
tion. The reaction was stood for 2 h at room temperature.
The precipitate so obtained was vacuum filtered and fil-
trate was first dried at room temperature for 24 h and
sintered at 100  C for 3 h. The graphene samples used
in this study were prepared by a previously reported elec-
trochemical exfoliation method.14 The graphene-ZnO QDs
composite was prepared by changing the wt.% of graphene
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in constant 1 g ZnO QDs in organic media (acetone). The
solution was mixed by magnetic stirrer for 30 min at room
temperature. The obtained product was kept for over night
for evaporation of acetone. For complete evaporation of
acetone, composite was sintered at 373 K for 1 h. In this
way, four samples were prepared by varying the wt.% of
graphene from 20–80 wt.%.
2.2. Material Characterization
The structural analysis of prepared materials was done
through X-ray diffraction (XRD) (Bruker diffractome-
ter D8, Advance) analysis with CuK radiation ( =
15406 nm). The high resolution-transmission electron
microscopy (HR-TEM) (Philips Tecnai F-30107) was
employed to analyse the morphology. The Raman spectro-
scopic measurements were performed on BRUKER RFS
27: Raman Spectrometer using Nd: YAG laser source
of excitation 514 nm. Optical characterizations were
done using ultraviolet-visible (UV-VIS) spectrophotome-
ter (Perkin Elmer) and fluorescence Spectrophotometer
(Hitachi, F-7000).
2.3. Chemiresistor Fabrication and Gas
Sensing Response Measurements
The sensing response is measured in term of resistance
change. The chemiresistors were fabricated by screen-
printing on glass substrate of size 25 mm × 25 mm. Before
screen-printing, glass substrates were thoroughly washed
with DI water and acetone, and then dried under argon
atmosphere. For surface resistance measurements, high
conducting silver paint contacts were deposited on adja-
cent sides of the film. The ohmic contact was achieved by
2 Sci. Adv. Mater., 6, 1–7, 2014
Nemade and Waghuley
annealing the chemiresistors at 200  C for 5 min in argon.
The average thickness of screen-printed layer was about
8 m, as determined by Digimatic Outside Micrometer
(Series-293, Japan). The CO2 sensing properties of materi-
als were studied in a home build gas sensor assembly. The
resistance of the chemiresistor was measured by using a
voltage divider method.15 All experiments are carried out
using dry air as carrier gas having H2 O lower than 3 ppm.
Before each gas detection test, the chemiresistor was mea-
sured under air flow until a stable response is obtained
(set as the baseline resistance). The concentration inside
the chamber was maintained by injecting known volume
of the CO2 . The sensing response is defined as:15
Rg − Ra 
S= (1)
Ra
where, Ra is the baseline resistance of the chemiresistor in
dry air and Rg is the resistance of chemiresistor in gas. The
value of Rg measured at constant interval of time (15 s).
The response time was measured by injecting 100 ppm
CO2 gas into the chamber at the room temperature. The
time required to achieve 90% of its highest value was con-
sidered as response time. Similarly, the recovery time of
the chemiresistor was defined as the time required for its
resistance to be reduced by 90% from its highest value. To
assess the reproducibility of the results, each measurement
is repeated several times.
3. RESULTS AND DISCUSSION
3.1. XRD Analysis
Figure 1 shows the XRD patterns of the graphene (pre-
viously reported), ZnO QDs and (20–80 wt.%) graphene-
ZnO QDs composites. There are two prominent peaks
in the XRD pattern (Fig. 1(a)), (002) and (100) which
are characteristic peaks of graphene. The peak at 2 =
263 shows a highly organised structure with an inter-
layer spacing of 0.339 nm. The broad peak at 2 = 442
may be assigned for lower degree of crystallization.16
Likewise, the structural purity of ZnO QDs reflects in
Figure 1(b). The diffraction peaks for ZnO are in agree-
ment with the standard PDF card number 01-075-1533
(Fig. 2). The reflecting planes observed in graphene and
ZnO are appeared at the same 2 positions in compos-
ites Figures 1(c)–(f), this indicative of good coordination
between the graphene and ZnO. Besides that, the broad
width appeared in composites with an increasing wt.% of
graphene also shows the well interaction between the com-
ponents of composites that is graphene and ZnO. Debye–
Scherrer formula was used to calculate the crystallite size.
The crystallite size decreases with an increase in the wt.%
of graphene.
The average crystallite size of ZnO QDs was found to
be 4.17 nm and for composites, it was found to be ranges
Nemade and Waghuley Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites

Table I. Average crystallite sizes of all samples.

Sample Particle size (nm)

Graphene 56
ZnO QDs 417
20 wt.% 394
40 wt.% 380
60 wt.% 374
80 wt.% 368

3.2. TEM Analysis

Figure 3 shows the TEM images of ZnO QDs. The average

crystallite size of ZnO QDs estimated from XRD analy-
sis concurs with TEM investigation. However, the separate
ZnO QDs can be clearly distinguished in figure, which
meant the aggregation of ZnO was well barred.
Figure 4 shows the TEM image of the 80 wt.%
graphene-ZnO QDs composite. The TEM image presented
the graphene surface is densely decorated with ZnO QDs.
The inset of Figure 4 depicts the selected area electron
diffraction (SAED) image of composite. The good coor-

Fig. 1. XRD patterns of (a) graphene, (b) ZnO QDs along with
(c) 20 wt.%, (d) 40 wt.%, (e) 60 wt.% and (f) 80 wt.% of graphene-ZnO
QDs composite.
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dination between the graphene and ZnO QDs observed
through the broad rings in image. From magnified image
of the white section, hybridised structure of graphene and
ZnO QDs reflects. The ZnO QDs engaged surface and
edges of graphene. This has been directly visualised by
HR-TEM, shown in Figure 5.

between the 3.94–3.68 nm. The average crystallite values 3.3. UV-VIS and Fluorescence Measurements
for samples listed in Table I. The smallest crystallite size
was found to be 3.68 nm for 80 wt.% graphene-ZnO QDs Figure 6 shows the UV-VIS spectrum of graphene and
composite. ZnO QDs. The intense absorption at 268 nm assigned to

Actual Curve

Standard PDF card curve

(Card No. PDF 01-075-1533)

Fig. 2. Standard XRD card curve for ZnO.

Sci. Adv. Mater., 6, 1–7, 2014 3

 Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites
Fig. 3. TEM image of ZnO QDs.
the few layered two-dimensional graphene.17 The UV-VIS
spectrun of ZnO QDs shows intense absorption at 341 nm.
The value of particle size estimated from XRD analysis
and absorption in UV region confirms the presence of
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quantum confinment in ZnO QDs.18
The sensing properties are appreciably influence by
defects concentration on the sensing surface.19 20 So, deter-
mination of defects concentration on sensing surface is
important. Figure 7 shows the fluorescence spectrum of
(20–80 wt.%) graphene-ZnO QDs composites. From plot,
it is clearly observed that the intensity value of ultravio-
let (IUV
increases with an increase in wt.% of graphene.
This shows that the graphene surface becomes more defec-
tive in the presence of ZnO QDs. This may be due to
ZnO QDs create vacancies or dangling bonds on graphene
surface.21 Hence, as the defects density increases, inten-
sity also increases. The intensities ratio of the ultravio-
let (IUV
to visible deep levels (IDL
is direct measure of
defect density.19 The fluorescence spectroscopy is straight-
forward approach of measurements of defects density and
the ratio of fluorescence intensities of deep level and near
band edge emission is postulated to be an index of defect
density.20
Fig. 4. TEM image (left) of 80 wt.% graphene-ZnO QDs compos-
ite. Inset shows the selected area electron diffraction pattern. Magnified
image (right) of the white section, reflecting the hybridised structure of
graphene and ZnO QDs.
4 Sci. Adv. Mater., 6, 1–7, 2014
Nemade and Waghuley
Fig. 5. HR-TEM image of 80 wt.% graphene-ZnO QDs composite.
3.4. Gas Sensing Characteristics
To know about the selective behaviour of chemiresistors
towards the oxidizing and reducing species, its response to
CO2 (50 ppm) and LPG (50 ppm) at 423 K was studied,
respectively. It is well known that LPG is composition of
CH4 , C3 H8 , C4 H10 etc., hence this gas choose to study the
selective behaviour as a representative of reducing species.
The results are presented in Figure 8. It is notable that
selective behaviour of composites enhanced with wt.%
of graphene. The highest value of sensing response was
obtained for the 80 wt.% graphene. The reason may be
that CO2 has a higher redox activity compared to the LPG.
Furthermore, the sensing response of chemiresistors was
also measured as a function of concentration at room tem-
perature (Fig. 9). The chemiresistors exhibited an increase
in response as a function of CO2 concentration. Moreover,
the responses of 20–80 wt.% graphene-ZnO composites
chemiresistors have almost linear behaviour. From the plot,
it is analysed that composition with 80 wt.% graphene-
ZnO has the maximum sensing response. This may be due
the smaller crystallite size, which provides a larger surface
100
Graphene
268 nm
80
ZnO QDs
% Absorption
60
40
341 nm
20
0
260 300 340 380
Wavelength (nm)
Fig. 6. UV-VIS spectrum of graphene and ZnO QDs.
Nemade and Waghuley Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites

60 7
IUV 20 wt.% Graphene

40 wt.% 6 ZnO QDs

20 wt.%
Fluorescence Intensity

60 wt.%
40 5 40 wt.%
80 wt.%

Sensing Response
60 wt.%
4
80 wt.%

20 3

2
IDL
1
0
300 400 500 600 700
Wavelength (nm) 0
0 50 100 150 200
Fig. 7. Fluorescence spectrum of (20–80 wt.%) graphene-ZnO QDs Carbon Dioxide Concentration (ppm)
composites.
Fig. 9. Chemiresistor response as a function of concentration of CO2 .
22
to volume ratio for gas-solid interaction. Another rea-
son for enhancement in sensing response with wt.% of response related to defects density through the oxy-
graphene attributed to an increase in defects density. The gen vacancies, which can act as adsorption sites for
variation of IUV /IDL ratio and CO2 sensing response with atmospheric oxygen. Therefore, more number of defects

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the wt.% of graphene is shown in Figure 10. From the adsorbed more oxygen ions. This is one of the possible
plots, it is scrutinized that sensing response increases with reason for an increase in sensing response with increasing
defects density that is (IUV /IDL
ratio linearly as a function defects density and wt.% of graphene.
of wt.% graphene. This result is consistent well with the From Figure 9, it is demonstrated that the addition
observation made by previous reports.20 23 of graphene make composite to improve the gas sens-
In chemiresistors, the change in resistance is mainly ing properties. This may be due to ZnO is a readily
originated due to the adsorption atmospheric oxygen, electron donor and carbon based materials are compara-
forming ionic species such as24 tively good electron acceptors.25 Hence, ZnO QDs act as
O2 gas
→ O2 ads
(2) active sensing sites by damageing to the graphene sur-
face, which may create vacancies or dangling bonds on
O2 ads
+ e− → O−
2 ads
(3) graphene surface and subsequently, enhance defects den-
O− − − sity. Therefore, atmospheric oxygen more rapidly interacts
2 ads
+ e → 2O ads
(4)
with defects generated due to interaction between ZnO
This scheme hold good for semiconducting metal oxide QDs and graphene. This statement is supported by flu-
i.e., for ZnO QDs in chemiresistor. As gas sensing orescence spectroscopy. As displayed in Figure 7, under
excitation wavelength of 254 nm, a broad band at 330–
6 450 nm is detected in all samples, which is attributed to
the defects density. Another possible reason for increase
5
Carbon Dioxide
LPG
Sensing Response

0
Graphene ZnO QDs 20 wt.% 40 wt.% 60 wt.% 80 wt.%
graphene graphene graphene graphene

Fig. 8. Response of chemiresistors towards CO2 (50 ppm) and LPG Fig. 10. The variation of IUV /IDL ratio and CO2 sensing response with
(50 ppm) at 423 K. the wt.% of graphene.

Sci. Adv. Mater., 6, 1–7, 2014 5

 Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites
6
Graphene
ZnO QDs
5
20 wt.%
40 wt.%
Sensing Response
4 60 wt.%
80 wt.%
3
0
323 373 423
Temperature (K)
Fig. 11. Chemiresistor response as a function of operating temperature
to 30 ppm CO2 .
in sensing response is that at low graphene wt.%, electron
transfer mainly due to ZnO QDs and electrons are flow by
hopping between QDs. On the other hand, at high wt.%
ARTICLE
of graphene, it overlaps on to the ZnO QDs and the resis-
tance of graphene is lower than that of ZnO QDs. Hence,
the adsorption of CO2 increases with wt.% of graphene
and ZnO played important to make graphene sheets defec-
tive. Therefore, the synergistic effect between these two
materials would effectively increase gas sensing proper-
ties. When chemiresistor exposed to the CO2 environment,
CO2 molecules adsorbed on oxygen ions. This adsorp-
tion result in the formation of a surface carbonates and
increases the resistance of chemiresistor.26 Therefore, the
physical adsorption of CO2 on the graphene surface is the
dominant sensing mechanism.6 27–29
The gas sensing response of chemiresistors towards the
30 ppm CO2 gas as a function of operating temperature
shown in Figure 11. Each curve shows a maximum sensing
response values corresponding to temperature, excluding
pure ZnO chemiresistor. This may be due to operating
temperature value of ZnO chemiresistor exist beyond the
473 K.30 31 From the plot, it is observed that all compos-
ites possess operating temperature at 448 K. This value is
relatively low that result in the low power consumption.
The results demonstrated that the chemiresistors response
to 30 ppm CO2 increases with an increasing wt.% of
graphene. The 80 wt.% graphene-ZnO composites exhib-
ited the optimum value of sensing response (5.31) at
448 K. The sensing response value from certain temper-
ature decreases, this may be due to desorption of oxygen
ions from chemiresistor surface. When the thermal vibra-
tion becomes sufficiently enough, adsorbed oxygen will
get desorbed.32
The stability chacateristics of 80 wt.% graphene-ZnO
composite is shown in Figure 12. Inset shows the tran-
sient response characteristics. The stability was measured
for 30 days, at an interval of 5 days for 100 ppm of
6 Sci. Adv. Mater., 6, 1–7, 2014
Nemade and Waghuley
473
Fig. 12. Stability and transient response (inset) characteristics of
80 wt.% graphene-ZnO chemiresistor to 100 ppm CO2 .
CO2 . From plots, it is clearly observed that chemiresistor
has almost constant sensing response indicating the good
stability. The transient response characteristic shows that
the response time of 80 wt.% graphene-ZnO compos-
ite chemiresistor exhibited fast response time (12 s). The
recovery time of chemiresistor was found to be 24 s.
In regards to the selectivity, sensing response, operat-
ing temperature, stability and fast response time, 80 wt.%
graphene-ZnO QDs chemiresistor is superior among the
prepared chemiresistors.
4. CONCLUSIONS
In this work, we made an attempt to study the influ-
ence of graphene concentration on gas sensing properties
of ZnO QDs. The gas sensing properties of graphene-
ZnO composites chemiresistors indicated that 80 wt.% of
graphene-ZnO composite chemiresistors exhibits the high-
est sensing response among all chemiresistors, low oper-
ating temperature, good stability and fast response and
recovery time. Besides that, the selectivity response of
graphene-ZnO composite chemiresistors to CO2 and LPG
(CH4 , C3 H8 , C4 H10
was also measured and the results
implied that 80 wt.% of graphene-ZnO composite chemire-
sistor has a well selectivity to CO2 . This enhancement in
sensing response attributed to small crystallite size and
high defects density, which evident from XRD and fluores-
cence analysis. The 80 wt.% of graphene-ZnO composite
chemiresistors enables detection of CO2 at low tempera-
ture operation, which reduce the power consumption and
subsequently operation cost. This is attractive accomplish-
ment of present work. On account of good characteristics
mentioned above, 80 wt.% of graphene-ZnO composite
chemiresistors can be good practical sensor for detection
of CO2 .
Nemade and Waghuley Low Operable Temperature Chemiresistive Gas Sensing by Graphene-ZnO Quantum Dots Composites
Acknowledgments: Authors are very much thankful to
Head, Department of Physics Sant Gadge Baba Amravati
University, Amravati for providing necessary facilities.
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