Journal of ELECTRONIC MATERIALS

https://doi.org/10.1007/s11664-018-6536-7
Ó 2018 The Minerals, Metals & Materials Society

The Morphology and Optical Properties of ZnO Nanorods

Grown on MoS2 Thin Films at Various Thicknesses Using
a Chemical Bath Deposition Method

KIEU LOAN PHAN THI,1,2 LAM THANH NGUYEN,1 NGUYEN HUU KE,1
DAO ANH TUAN,1 THI QUYNH ANH LE,1 and LE VU TUAN HUNG1

1.—Department of Applied Physics, Faculty of Physics and Engineering Physics, University of

Science, Ho Chi Minh City, Vietnam. 2.—e-mail: ptkloan@hcmus.edu.vn

MoS2 thin films and ZnO nanorods were prepared by chemical bath deposition
on glass substrates to form ZnO nanorod/MoS2 thin film heterostructures. The
morphological, structural and optical properties of ZnO nanorods grown on
MoS2 thin films were investigated through scanning electron microscopy
(SEM), x-ray diffraction (XRD), Raman spectroscopy, ultraviolet–visible (UV–
Vis) and photoluminescence spectroscopy, respectively. The SEM images and
XRD patterns revealed that ZnO nanorods exhibited a hexagonal wurtzite
structure with preferred c-axis orientation, a good crystallinity and covered
the entire surface of MoS2 thin films. Furthermore, ZnO nanorods were suc-
cessfully grown on MoS2 thin films without affecting the crystal structure of
2H-MoS2 which was demonstrated through two typical peaks of 380 cm 1 and
410 cm 1 in Raman spectra. Notably, the combination of ZnO nanorods and
MoS2 thin films (ZnO nanorod/MoS2 thin film heterostructures) revealed a
significant increase of absorption in the wavelength range of 350–800 nm
characterized by UV–Vis spectroscopy. In addition, ZnO nanorod/MoS2 thin
film heterostructures also showed a significant decrease of the intensity of
photoluminescence emission.

Key words: ZnO/MoS2 heterostructure, transition metal dichalcogenide,

MoS2 thin film, ZnO nanorods, chemical bath deposition

INTRODUCTION large-area uniformity, it is very difficult to fabricate

a large-scale continuous and uniform MoS2 mono-
MoS2 has recently received increasing attention
layer, while continuous uniform MoS2 thin films
due to its great potential as a low-cost alternative to
over a large area can be easily prepared by many
graphene.1,2 Structurally, despite having a two-
methods. Among some of the methods for preparing
dimensional layered structure similar to graphene,
MoS2 thin films, chemical bath deposition7,8 is
MoS2 has a band gap which does not exist in
particularly attractive due to simplicity, low cost
graphene. Furthermore, the band gap of MoS2
and mass production, while others such as chemical
depends strongly on its number of layers. Specifi-
vapor deposition,2,5,9 pulsed laser deposition4,6 or
cally, few-layered or bulk MoS2 (Eg  1.2 eV) are
sputtering3,10 require complicated multi-step pro-
indirect gap semiconductors, whereas monolayer
cesses and expensive equipment.
MoS2 (Eg  1.9 eV) is a direct gap semiconductor.3,4
A striking advantage of MoS2 thin films is the
For this reason, MoS2 holds great promise for many
small band gap, so MoS2 thin films show strong
optoelectronic device applications.4–6 In terms of
absorption in the solar spectrum. However, the fast
recombination rate of electron–hole pairs in MoS2
thin films leads to severe limitations of solar energy
(Received October 26, 2017; accepted July 17, 2018) utilization. To solve this problem, many efforts

focused on coupling MoS2 with other semiconduc-
tors. In this way, the coupling of MoS2 with ZnO can
bring many outstanding advantages. The ZnO/MoS2
heterostructures form band alignments that facili-
tate the separation of the charge carriers, reducing
electron–hole recombination.11 Moreover, an advan-
tage of ZnO is the variety in nanostructured mor-
phologies; thus, 1D, 2D and 3D nanostructures can
be easily prepared by many methods. With 1D
nanostructures, ZnO nanorods can supply a direct
path that facilitates rapid charge transfer.12 There-
fore, the ZnO nanorod/MoS2 thin film heterostruc-
tures can further improve the separation of charge
carriers. In addition, ZnO shows strong absorption
in the ultraviolet region owing to its wide band gap
of 3.3 eV. Hence, ZnO nanorod/MoS2 thin film
heterostructures can enhance absorption in the
solar spectrum. So far, there have been many works
on MoS2/ZnO heterostructures aiming to improve
the efficiency of photocatalysts11,13 and field emis-
sion devices.14,15 However, most of the previous
works reported on the combination of ZnO and MoS2
in ZnO/MoS2 heterostructure composites.11,13,16
These composites can enhance absorption in the
solar spectrum, but unfortunately they tend to
decrease the crystallinity of ZnO. In addition, a
large MoS2 loading amount can block light absorp-
tion of the ZnO component. Recently, Zhang et al.17
reported a ZnO nanorod/MoS2 monolayer
heterostructure for increasing Raman and photolu-
minescence emission. In their experiments, the
discontinuous MoS2 monolayers were prepared by
a vapor solid growth route at the high temperature
of 950°C. Then, Chen et al.14 also reported the
preparation of MoS2 flakes from commercial bulk
MoS2 by a mechanical cleavage method to create
ZnO nanowire/few-layer MoS2 flake heterostructure
for FET transistor application. And Butanovs
et al.18 reported on few-layer MoS2 film coating on
ZnO nanowires grown at 700°C by vapor phase
sulfurization for potential applications of hydrogen–
evolution reactions and in dye-sensitized-like solar
cells.
Here, we demonstrate a simple and low-cost
method for preparing large-scale MoS2 thin films.
In this approach, both ZnO nanorods and MoS2 thin
films were grown by chemical bath method. In our
experiment, ZnO nanorod/MoS2 thin film
heterostructures were prepared on glass substrates.
The morphology of ZnO nanorods grown on MoS2
thin films with various thicknesses were investi-
gated. Additionally, the optical and structural prop-
erties of ZnO nanorod/MoS2 thin film
heterostructures were also analyzed.
EXPERIMENTAL
In our experiment, at first, MoS2 thin films were
prepared on glass substrates. Subsequently, ZnO
nanorods were grown on MoS2 thin films to develop
ZnO nanorod/MoS2 thin film heterostructures. All
Thi, Nguyen, Ke, Tuan, Le, and Hung
chemicals and reagents were purchased from Sigma
Aldrich. The schematic illustrating the development
of ZnO nanorod/MoS2 thin film heterostructures is
shown in Fig. 1.
Fabrication of MoS2 Thin Film
The growth of the MoS2 thin film on a glass
substrate involved a multi-step process. Firstly, the
glass substrate was cleaned with methanol, aceton
and de-ionized water in an ultrasonic bath. Then,
H2NCSNH2 (0.8632 g) was dissolved in 30 mL de-
ionized water for 30 min, and (NH)6Mo7O24Æ4H2O
(0.5005 g) and 6 mL N2H4Æ4H2O solution (35%) were
added in turn to the solution and each stirred for
30 min. This was followed by stirring processes to
obtain a clear solution (pH  9.8). The cleaned glass
substrates were immersed in the solution and
heated gradually to 90°C. The interactions in the
solution were reported in some works.19,20 After the
desired deposition time, the solution was cooled to
room temperature. The MoS2 thin film on the glass
substrate was taken out of the solution and rinsed
with distilled water to remove precipitates and
excess salt. Finally, the MoS2 thin film was placed
in a closed graphite box with 0.04 g of sulfur powder
and annealed at 500°C in a quartz furnace under N2
atmosphere for 90 min to improve the crystallinity.
Fabrication of ZnO Nanorods
Following the deposition of the MoS2 thin film,
ZnO nanorods were grown on the film. A ZnO seed
layer was coated on the MoS2 thin film by the dip-
coating method. A sol solution was prepared using
the procedures described in our previous report.21
The ZnO seed layer was dipped at a rate of 40 mm/
min and dried at 300°C for 15 min, repeated three
times in the same conditions. Then, the obtained
sample was immersed into an equal molar mixture
(0.1 M) of Zn(NO3)2Æ6H2O and methenamine
(C6H12N4), and deposited at 90°C for 4 h. Subse-
quently, the samples were taken out of the solutions
and rinsed with distilled water to remove excess salt
on the surface. Finally, the samples were dried in
air overnight.
The ZnO nanorod/MoS2 thin film heterostruc-
tures with different deposition times of MoS2 thin
films for 15, 20, 25 and 30 min were labeled ZM15,
ZM20, ZM25 and ZM30, respectively.
Characterization of ZnO Nanorod/MoS2 Thin
Film Heterostructures
We investigated the structural properties and
morphology of ZnO nanorod/MoS2 thin film
heterostructures using x-ray diffraction measure-
ments (XRD; D2 PHARSER; Bruker), room temper-
ature Raman spectrum in the backscattering
configuration (Labram 300; Horiba JOBIN YVON;
excitation wavelength, k = 632.8 nm) and scanning
electron microscopy (SEM; Hitachi 4700),
The Morphology and Optical Properties of ZnO Nanorods Grown on MoS2 Thin Films at
Various Thicknesses Using a Chemical Bath Deposition Method
Fig. 1. Schematic illustrating the development of ZnO nanorod/MoS2 thin film heterostructure.
respectively. The optical properties were investi-
gated by a Jasco V-730 UV–Vis–NIR spectropho-
tometer covering the wavelength range from 200 to
1100 nm and room-temperature photoluminescence
(PL) using a He-Cd laser line with the excitation
source of 325 nm.
RESULTS AND DISCUSSION
The SEM cross-section images of pristine MoS2
thin films with different deposition times are shown
in Fig. 2a, b, and c. We can see that the thickness of
the MoS2 thin film can be obtained by controlling
the deposition time. The corresponding deposition
times of 20, 25 and 30 min gave average thicknesses
of MoS2 thin films of 51, 65 and 73 nm, respectively.
In addition, the structural characterization of the
MoS2 thin film was confirmed by Raman spec-
troscopy. Figure 2d shows the Raman spectrum of
the MoS2 thin film with 20 min deposition time. We
found that MoS2 thin films exhibits peaks at
380 cm 1, 410 cm 1 and 454 cm 1 corresponding
to the E12g, A1g and 2LA(M) vibration modes of MoS2,
respectively.22 Among these vibration modes, the
E12g and A1g vibration modes indicate the formation
of a 2H-MoS2 structure corresponding to the in-
plane and out-of-plane movements of atoms, respec-
tively.23,24 Moreover, full width at half maximum
(FWHM) of the E12g and A1g vibration modes are
obtained at 14.2 cm 1 and 16.6 cm 1, respectively.
This implies the polycrystalline nature of the MoS2
thin film.5 Additionally, the difference between the
Raman shifts of E12g and A1g vibration modes is
about 29 cm 1. These results indicate that MoS2
thin films show bulk-like or multilayer behavior and
good crystallinity.5,8
The optical absorption characteristics of MoS2
thin films with deposition times were investigated
using UV–Vis spectra, as shown in Fig. 3a. The
results indicate that MoS2 thin films show peaks at
620 nm and 672 nm related to direct transitions
from the valence band to the conduction band of the
2H-MoS2 structure at the K point of the Brillouin
zone.24–26 Also, the presence of a peak at around
400 nm relates to a direct transition band edge.25
Furthermore, it can be clearly seen that MoS2 thin
films exhibit strong absorption bands in visible light
at about 400–800 nm. In addition, from the absorp-
tion spectra, it can also be found that, as the film
thickness increases, there is a slight shift in absorp-
tion wavelength towards the red end (see inset of
Fig. 3a). In addition, Fig. 3b shows the relationship
between (Ahm)2 and hm which are plotted using
Tauc’s relationship.27,28 We can estimate the band
gap values of MoS2 thin films, which are 1.6, 1.59,
1.57 and 1.56 eV for the film deposition times of 15,
20, 25 and 30 min, respectively. On the other hand,
the absorption of the films also tends to increase
with increasing film thickness. This can be
explained by the increase in concentration of the
number of absorbing particles.
In order to clarify the optical properties of the
combination of ZnO nanorods and MoS2 thin films,
the optical absorption spectra of pristine ZnO
nanorods and ZnO nanorod/MoS2 thin film
heterostructures with different deposition times of
MoS2 thin films were studied, as shown in Fig. 4.
We can see that there is a strong absorption band at
380 nm of pristine ZnO nanorods and ZnO nanorod/
MoS2 thin film heterostructures which relates to the
characteristic absorption spectrum of ZnO. More-
over, it is notable that the presence of MoS2 thin

Fig. 2. (a–c) SEM cross-section images of pristine MoS2 thin films with different deposition times of 20, 25, and 30 min, respectively. (d) Raman
spectrum of MoS2 thin film with deposition time of 20 min.
films shows enhanced absorption in the visible light
region of ZnO nanorod/MoS2 thin film heterostruc-
tures compared to pristine ZnO nanorods. The
reason for this is because band gap of MoS2 is
narrower than that of ZnO, and MoS2 can thus
enhance absorption in longer wavelength region.
Hence, comparing the spectra of pristine ZnO thin
films with those of ZnO nanorod/MoS2 thin film
heterostructures (in Fig. 4) indicates the absorption
band expansion from 350 to 800 nm. This demon-
strates that the ZnO nanorod/MoS2 thin film
heterostructures exhibit absorption bands in both
the visible and UV regions of the solar spectrum.
Also, the absorption of ZnO nanorod/MoS2 thin film
heterostructures also increases with the increase of
deposition time since the absorption is proportional
to the MoS2 thin film thickness, as was revealed in
the absorption spectra (Fig. 3b).
Thi, Nguyen, Ke, Tuan, Le, and Hung
To investigate the structural properties of the
ZnO nanorod/MoS2 thin film heterostructures,
Raman spectra were measured at room temperature
under excitation by a He-Ne laser (k = 632.8 nm),
and the results are displayed in Fig. 5a. All the ZnO
nanorod/MoS2 thin film heterostructures exhibit
E12g, A1g and 2LA(M) vibration modes of MoS2,
which demonstrates the growth of ZnO nanorods
without affecting the crystal structure of the MoS2
thin films. On the other hand, it can be clearly seen
that no peaks of ZnO nanorods can be detected in
any of the heterostructures. To further clarify this
issue, Raman spectra of pristine ZnO nanorods,
pristine MoS2 thin films (20 min) and ZM20
heterostructures have been compared, as shown in
Fig. 5b.
The results in Fig. 5b reveal that the Raman
spectrum of pristine ZnO nanorods exhitbits a peak
The Morphology and Optical Properties of ZnO Nanorods Grown on MoS2 Thin Films at
Various Thicknesses Using a Chemical Bath Deposition Method
Fig. 3. (a) Absorption spectra, and (b) plot of (Ahm)2 versus hm of
MoS2 thin films with different deposition times of 15, 20, 25 and
30 min, respectively. Insets: (a) shift of absorption spectra and (b)
color of MoS2 thin films with different deposition times.
Fig. 4. Absorption spectra of pristine ZnO nanorods, pristine MoS2
(20 min) and ZnO nanorod/MoS2 thin film heterostructures with dif-
ferent deposition times of the MoS2 thin film.
at 440 cm 1 related to the E2 vibration mode of the
wurtzite hexagonal phase ZnO,29 whereas the
Raman spectra of pristine MoS2 thin film and
ZM20 heterostructure exhibit a peak at 454 cm 1
related to the 2LA(M) vibration mode of MoS2 with a
broad band from 430 to 480 cm 1. Consequently, it
seems that the E2 vibration mode of ZnO is over-
lapped by this vibration mode of MoS2.
The structure and crystallinity of ZnO nanorods
grown on MoS2 thin film was further investigated
using XRD patterns. From Fig. 6a, we can see that
both pristine ZnO nanorods and the ZM20
heterostructure exhibit (100), (002), (101), (102),
(103), and (004) planes of ZnO (PDF 04-003-2106).
Moreover, the intensity of (002) plane is highest
among others for both the two samples. This
indicates that ZnO nanorods exhibit a preferred
orientation along the c-axis of the hexagonal
wurzite structure. In addition, the sharpness of
the (002) peak (FWHM = 0.143°) implies the good
crystallinity of the ZnO nanorods. Fascinatingly,
comparing the XRD pattern of pristine ZnO nanor-
ods with that of the ZM20 heterostructure indicates
the presence of a peak at a diffraction angle (2h) of
33.6° for the ZM20 heterostructure without being
present for pristine ZnO nanorods (Fig. 6b). This
implies the presence of the 2H-MoS2 structure
corresponding to the (101) plane (PDF 00-006-
0097) in the ZnO nanorod/MoS2 thin film
heterostructure. Therefore, from the results of the
Raman spectra and XRD patterns, it is revealed
that ZnO nanorod/MoS2 thin film heterostructures
were sucessfully prepared with good crystallinity of
both the ZnO nanorods and the MoS2 thin films.
Additionally, to determine the morphologies of
ZnO nanorods grown on MoS2 thin films, ZnO
nanorod/MoS2 thin film heterostructures have been
observed using SEM images (Fig. 7a–f). All the ZnO
nanorods grown on MoS2 thin films exhibit a
hexagonal wurtzite structure, instead of uniform
size, and cover the whole surface of the MoS2 thin
films. As shown in Fig. 7a, ZnO nanorods were
grown on MoS2 thin film with a time deposition of
20 min without a ZnO seed layer. We found that
ZnO nanorods have a large diameter in the range
 650–800 nm and that the vertical alignment of
ZnO nanorods grown on MoS2 thin film are poor.
Due to the lattice mismatch between ZnO and MoS2
( 3%),17 the vertical alignment of ZnO nanorods
are not yet well supported. Otherwise, with a ZnO
seed layer, the morphologies and orientation of ZnO
nanorods are significantly improved. Based on
SEM, a cross-section image of the ZM20
heterostructure is shown in Fig. 7f, from which it
can be seen that all ZnO nanorods exhibit good
vertical alignment with an average length of about
1.1 lm. Moreover, the results in Fig. 7a–e also
indicate that ZnO nanorods grown on MoS2 thin
films become smaller in diameter as the deposition
time of MoS2 thin films increases. Especially, the
diameter of ZnO nanorods in the ranges  100–230,
125–170, 80–103 and 50–87 nm correspond to M15,
ZM20, ZM25 and ZM30, respectively. Consequently,
these results indicate that a ZnO seed layer can

Fig. 5. Raman spectra of (a) ZnO nanorod/MoS2 thin film heterostructures with different deposition times of MoS2 thin films, and (b) pristine ZnO
nanorods, pristine MoS2 thin films and ZM20 heterostructures.
Fig. 6. XRD patterns of pristine ZnO nanorods and ZM20 heterostructures: (a) with 2h values of 30°–80° and (b) with zoom in the range of 30°–
37° of 2h values.
significantly support the growth of ZnO nanorods on
MoS2 thin films.
Finally, the recombination rate of photogenerated
electrons and holes in ZnO nanorod/MoS2 thin film
heterostructures have been analyzed using PL
spectra (Fig. 8a). The results reveal that both
pristine ZnO nanorods and ZnO nanorod/MoS2 thin
film heterostructures exhibit two main emission
bands of ZnO, corresponding to near band edge
emission (NBE) and deep level emission (DLE) at
about 380 nm and 450–800 nm, respectively. Specif-
ically, the NBE is attributed to electron transition
from the conduction band to the valence band, while
the DLE is related to intrinsic defects in ZnO
nanorods. Furthermore, in order to confirm and
further clarify defects present in the ZnO nanorods,
PL spectra were fitted with Gaussian fitting, and
the results for pristine ZnO nanorods and ZM20 are
displayed in Fig. 9. It is clearly seen that the
presence of intrinsic defects in ZnO nanorods are
Thi, Nguyen, Ke, Tuan, Le, and Hung
zinc interstitial (Zni), oxygen vacancies (Vo) and
oxygen interstitial (Oi). Essentially, Zni defects
( 3.1 eV) correspond to transition from the inter-
stitial zinc level (located below the bottom of the
conduction band) to the valence band, meanwhile Vo
( 2.2 eV) and Oi ( 1.9 eV) are generated by
transitions from the oxygen vacancies level (located
below the interstitial zinc level) to the valence band
and the conduction band to the oxygen interstitial
level (located above the top of the valence band),
respectively.30,31 Also, this implies that defect levels
can act as traps in the charge transport process.
Interestingly, although ZnO nanorod/MoS2 thin film
heterostructures exhibit similar PL emission bands
to those of pristine ZnO nanorods, their PL intensity
is lower than that of pristine ZnO nanorods. This
indicates the suppression of recombination of the
photogenerated electron–hole pairs in the
heterostructures. Moreover, the integrated PL
intensity ratio of INBE/IDLE of all samples have also
The Morphology and Optical Properties of ZnO Nanorods Grown on MoS2 Thin Films at
Various Thicknesses Using a Chemical Bath Deposition Method

Fig. 7. SEM images of (a) ZM20 heterostructure without ZnO seed layer, (b–e) ZM15, ZM20, ZM25, ZM30 heterostructures, respectively, and (f)
SEM cross-section image of ZM20 heterostructure.

Fig. 8. (a) Photoluminescence (PL) spectra and (b) the integrated PL intensity ratio of INBE/IDLE of pristine ZnO nanorods, ZM15 and ZM20,
ZM25 and ZM30 heterostructures, respectively.

Fig. 9. Gaussian fittings of PL spectra of (a) pristine ZnO nanorods and (b) ZM20.
Fig. 10. Schematic of charge separation mechanism in the ZnO/
MoS2 heterostructure.
been compared, and the results are presented in
Fig. 8b. Based on Fig. 8b, this indicates a reduction
in the intrinsic defect density of ZnO nanorods on
MoS2 films. Remarkably, the visible emission inten-
sity from defect states of the ZM20 heterostructure
shows a significant decrease and exhibits the high-
est integrated PL intensity ratio of INBE/IDLE com-
pared with the others. It is worth mentioning here
that 20 min deposition of MoS2 film reduces the
defect density of the ZnO nanorods and improves
the charge separation at the ZnO/MoS2 interface,
which reduces the recombination of the photogen-
erated electron–hole pairs. However, the results in
Fig. 8a also show that, as the depositon time of the
MoS2 films increases to 25 and 30 min, correspond-
ing to ZM25 and ZM30, respectively, the visible
emission intensity again increases. This can be due
Thi, Nguyen, Ke, Tuan, Le, and Hung
to the thicker layer of the MoS2 charge carriers
being easily trapped at the defect states of the
interface of the ZnO/MoS2 heterostructure during
the charge transport process.32 Thus, it no longer
supports the charge separation process in the ZnO
nanorod/MoS2 thin film heterostructures.
According to some previous reports33–36 and the
results of our experiment, the charge separation
mechanism of ZnO nanorod/MoS2 thin film
heterostructures is illustrated in Fig. 10, from
which it can be seen that, under illumination,
photogenerated electron–hole pairs are formed with
electron transfer from the conduction band of MoS2
to that of ZnO, with, in contrast, hole transfer from
the valence band of ZnO to that of MoS2. Therefore,
the recombination of photogenerated electron–hole
pairs is reduced.
CONCLUSIONS
In summary, the ZnO nanorod/MoS2 thin film
heterostructures were successfully prepared by a
chemical bath method. Both ZnO nanorods and
MoS2 thin films of ZnO nanorod/MoS2 thin film
heterostructures showed good crystallinity. MoS2
thin films show a 2H-phase with two typical Raman
peaks at 380 and 410 cm 1. In addition, the ZnO
nanorods grown on MoS2 thin films exhibit a
hexagonal wurtzite structure and vertical orienta-
tion on the whole surface of MoS2 thin films with an
average length of 1.1 lm. Moreover, the results
from UV–Vis and PL spectra demonstrate that the
combination of ZnO nanorods and MoS2 thin films
to form ZnO nanorod/MoS2 thin film heterostruc-
tures not only extends the range of the absorption
bands but also facilitates the separation of the
charge carriers. Remarkably, the ZnO nanorod/
51 nm-MoS2 thin film heterostructure showed the
strongest decrease of visible emissions in
The Morphology and Optical Properties of ZnO Nanorods Grown on MoS2 Thin Films at
Various Thicknesses Using a Chemical Bath Deposition Method
comparison to others with various thicknesses of the
MoS2 thin films.
ACKNOWLEDGEMENT
This research is funded by Vietnam National
University HoChiMinh City (VNU-HCM) under
Grant Number C2017-18-23.
CONFLICT OF INTEREST
The authors declare that there is no conflict of
interest regarding the publication of this paper.
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