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1 s2.0 S0921510720303962 Main
1 s2.0 S0921510720303962 Main
1 s2.0 S0921510720303962 Main
Growth of In2S3 nanolayers on F-Mica, SiO2, ZnO, and TiO2 substrates using
chemical vapor deposition
Narinder Kaur, Dipika Sharma, B.R. Mehta *
Thin Film Laboratory, Department of Physics, Indian Institute of Technology, New Delhi 110016, India
A R T I C L E I N F O A B S T R A C T
Keywords: In this study, 2D layers of β-In2S3 have been synthesized on different substrates such as SiO2, F-Mica, ZnO, and
2D layers TiO2 using the chemical vapor deposition (CVD) technique. Different morphologies of In2S3 2D nanoflakes have
β-In2S3 been obtained within the temperature range of 550–850 ◦ C. These nanolayers have been characterized by using
Chemical vapor deposition
FESEM, XRD, and Raman spectroscopy techniques. The results show well-formed nanodomains of β-In2S3 with a
Optical and photoelectric properties
tetragonal phase on different substrates by CVD technique at an optimized temperature of 750 ◦ C, although the
morphology of the grown layer depending sensitively upon the substrates. The initial results show ohmic current-
voltage characteristics, the fast photoconductive response of In2S3 layers. In2S3 grown on ZnO substrates as a
base layer show enhanced photoelectrochemical properties because of increased visible light absorption, as
indicated by optical absorption results.
* Corresponding author.
E-mail address: brmehta@physics.iitd.ac.in (B.R. Mehta).
https://doi.org/10.1016/j.mseb.2020.114889
Received 18 May 2020; Received in revised form 15 September 2020; Accepted 13 October 2020
Available online 13 November 2020
0921-5107/© 2020 Elsevier B.V. All rights reserved.
N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
to be deposited on semiconductor layers other than Mica and SiO2. In the system with a high-sensitivity ultralow noise CCD camera. Sample
present study, different morphological architectures of β-In2S3 flakes damage was controlled by using a laser power of < 1 mW. X-ray
have been synthesized using only chemical vapor deposition technique diffraction patterns of distinct morphologies of In2S3 were measured in
on different substrates such as SiO2, F-Mica, ZnO, and TiO2, and depo the 2θ range of 20◦ -60◦ with glancing angle 1◦ (Configuration = IR Stage
sition parameters have been optimized. Microstructural, phase analysis, (PhiPsi X YZ)) using Philip’s X’Pert PRO-PW vertical system operating in
and morphological analysis of the β-In2S3 nanoflakes samples have been reflection mode employing Cu-Kα radiation (λ = 1.5418 Å). Morpho
done using Raman, X-ray diffraction, and FESEM. Preliminary in logical analysis of In2S3 nanoflakes was carried out using FESEM Jeol
vestigations of photo-conducting and photoelectrochemical properties make, JSM-7800F prime with operating voltage = 10 kV without Au
of In2S3 layers have been done to assess their quality and potential coating on SiO2 and F-Mica substrate. Absorption spectra were
usefulness for functional applications. measured using a UV–visible spectrophotometer (Perkin Elmer Lambda
35). Macroscopic I–V and I-t measurements on In2S3 nanoflakes were
2. Experimental section carried out by depositing Au/Ni contacts by using the thermal evapo
ration in a two-electrode planar configuration. Keithley 2400 source
Chemical vapor deposition is the process by which 2D films of meter and Oriel cornerstone 260 monochromator with a Xenon lamp
different materials are grown from the vapor phase, by the deterioration was used for the photoresponse measurements. Spectral response for
of initial precursors on the surface of the substrate under non- measuring current in light and dark conditions with usual control
equilibrium conditions. The growth of 2D material thin films using through a program developed in Labview with GPIB control. For the
chemical vapor deposition technique includes the following steps: 1) A photoelectrochemical properties investigation, In2S3 flakes deposited on
pre-specified volume of inert gas inaugurated at a particular flow rate in the ITO substrate to be used as working electrodes. Linear sweep vol
the reaction assembly 2) Gas species transport and accommodate on the tammogram (LSV) characteristics were recorded in dark and light con
surface of the substrate 3) Chemical reaction of reactants to form a 2D ditions at a scan rate of 20 mV/s in aqueous 0.5 M Na2SO4.
material thin film on the surface of the substrate 4) The gaseous by-
products of the chemical reactions are detached and evicted from the 3. Results and discussion
reaction assembly.
3.1. Growth of β-In2S3 on SiO2 and Mica substrates
2.1. Synthesis of β-In2S3 using CVD on different substrates:
Fig. 1 (a-f) shows the field emission scanning electron microscopy
In the present study, the growth of β-In2S3 using the CVD technique (FESEM) images of In2S3 on two different substrates SiO2 and F-Mica.
has been carried out following these steps: Firstly, Ar gas as inert gas is FESEM images of In2S3 show the triangular geometries on both SiO2 and
introduced in the single zone furnace at an optimized flow rate. Sub F-Mica substrates in the temperature range of 550–850 ◦ C. Microscopy
strates like SiO2, F-Mica, and ZnO, TiO2 layers deposited on SiO2 sub shows that well-defined triangular morphology is obtained at a growth
strate (size 1 cm × 1 cm) are placed on silica boat and positioned temperature of 750 ◦ C for both SiO2 and F-Mica substrates. The size of
downstream at about 10–12 cm away from the center of single zone the triangular flakes obtained on the SiO2 substrate is about ~300 nm,
furnace. Prior to heating, the whole system was purged by Ar gas for half while on F-mica substrates, it is ~500 nm at 750 ◦ C growth temperature.
an hour. The furnace was heated in temperature range 550–850 ◦ C at the Yu Zhao and et al. reported similar results in terms of flake size and
rate of 10 ◦ C/min with the flow of Ar gas at 50 sccm for growth time of growth temperature [9]. Furthermore, analysis for the crystal structure
15 min. The temperature of sulfur was maintained near to its melting and the phase purity of In2S3 has been carried out using Raman spec
point of 150 ◦ C. After the chemical reaction, the furnace was cooled troscopy and X-ray diffraction techniques, and results are as shown in
immediately at room temperature with a cooling rate of 25 ◦ C/min. Fig. 1 (g-h).
Raman spectra for the sample prepared at the growth temperature of
2.2. Characterization techniques 750 ◦ C on SiO2 and F-Mica substrate shows the characteristic peaks for
Eg mode at 114, 135, 306, 326 cm− 1, Bg mode at 162, 245, 369 cm− 1 and
Raman analysis of In2S3 morphologies was investigated using a Ag mode at 180, 268, 368 cm− 1 indicating the growth of pure tetragonal
Renishaw invia confocal Raman microscope with a 514 nm laser β-In2S3 phase. It is noticed that at different temperatures, 550 ◦ C, 750 ◦ C,
wavelength and 1800/2400 lines per mm grating. A holographic and 850 ◦ C, and for 15 min growth time, phase pure tetragonal β-In2S3
diffraction grating with confocality control is used in the diffraction was obtained at 750 ◦ C growth temperature in case of both the
Table 1
A summaries of reported results on the growth In2S3 along with the results of the present study.
Substrate Temperat ure Ar Gas Pressure Precursors Shape Size (nm) Process of growth Time References
(◦ C) (seem) (min)
2
N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
Fig. 1. (a-f) FESEM images of In2S3 on SiO2 substrate and F-Mica substrate, (g-h) Raman spectra of In2S3 on SiO2 and F-Mica with a different temperature range from
550 to 850 ◦ C, (i) XRD patterns of In2S3 at 750 ◦ C growth temperature for SiO2 and F-Mica substrates.
substrates. At 550 ◦ C and 850 ◦ C growth temperature, the α-In2S3 phase is detected to be ~800 nm at a growth time of 15 min and a growth
and cubic phase of β-In2S3 were formed, respectively, for SiO2 substrate. temperature of 750 ◦ C.
In the case of the F-Mica substrate at 550 ◦ C temperatures, only one peak Raman spectra for samples grown at 750 ◦ C for 5 to 15 min are used
was observed at 260 cm− 1, which corresponds to sulfur only and show to have information about the growth of the number of layers. It is
inadequate growth, and at 850 ◦ C growth temperature cubic phase of shown in Fig. 3 (a & b) that as the growth time increases 5 to 15 min
β-In2S3 formed. XRD pattern of In2S3 grown at 750 ◦ C temperature on thickness of In2S3 nanoflakes increases. Raman spectra show that for
SiO2 and F-Mica substrates indicated the growth of the tetragonal phase lower thickness Raman modes Eg and Bg at 135 cm− 1 and 162 cm− 1 are
of β-In2S3, as indicated by the highest intensity peak at 27.52◦ with hkl absent while on increasing thickness up to 50 nm, they appear in the
value of (1 1 3). Other high-intensity peaks at 23.52◦ , 28.78◦ , 33.35◦ , Raman spectra. It has also been observed that Raman peak position was
43.74◦ , 47.76◦ , 50.38◦ ,56.31◦ ,59.67◦ , and 66.86◦ corresponding to hkl independent of layer thickness, which indicates that the Van der Waals
values (0 0 2), (2 2 2), (0 0 4), (2 2 4), (3 3 3), (0 4 4), (1 3 5), (3 3 5) and forces between layers were unruffled [22]. Raman results show that as
(2 2 6) planes, respectively (JCPDS card no. 51–1159) [9] were also the thickness decreases, the intensity and sharpness of Raman peaks go
observed. on reducing [23] (see Fig. 3 (a & b)). Similar results were reported by Yu
In2S3 layers were synthesized for different growth time, i.e., 5 min, Zhao and et al. [9] for the thickness-dependent growth of 2D β-In2S3
10 min, and 15 min on both SiO2 and F-Mica substrates at the growth nanoflakes by the PLD technique. XRD analysis for different layers
temperature of 750 ◦ C. Fig. 2 (a-c) and Fig. 2 (d-f) show FESEM images shown in Fig. 3 (c) confirmed the formation of the tetragonal phase of
of In2S3 on SiO2 and F-Mica substrates for growth time varying from 5 to β-In2S3 at 27.52◦ with hkl value along (1 1 3) direction and with high-
15 min, respectively. The triangular geometry was observed for 10 min intensity peaks at 23.52◦ , 28.78◦ , 33.35◦ , 43.74◦ , 47.76◦ , 50.38◦ ,
growth time, and on further increment in growth time, aggregation [9] 56.31◦ , 59.67◦ , and 66.86◦ corresponding to hkl values (0 0 2), (2 2 2),
of the triangular domains was observed. The triangular geometry of (0 0 4), (2 2 4), (3 3 3), (0 4 4), (1 3 5), (3 3 5) and (2 2 6) planes. Fig. 3 (d-f)
nanoflakes with uniform distribution is formed due to diffusion-based represents cross-sectional FESEM images of In2S3 nanoflakes grown on
and reaction limited processes [1]. On SiO2 substrate at 750 ◦ C SiO2 substrate for 5 to 15 min at 750 ◦ C. It is observed that with an
growth temperature and 10 min growth time, consistent triangular ge increase of deposition time average thickness of nanoflakes increases
ometry with an average domain size of 300 nm has been observed from ~10 to ~50 nm. These results are consistent with the Raman
without any aggregation. For the F-Mica substrate, the size of nanoflakes results.
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N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
Fig. 2. FESEM images of In2S3 grown on (a-c) SiO2 and (d-f) F-Mica substrate at an optimum temperature of 750 ◦ C for different deposition time.
Fig. 3. Raman spectra of the respective samples on (a) SiO2 and (b) F-Mica substrate (c) XRD spectra of In2S3 flakes for time range 5–15 min. (e-g) Cross-sectional
FESEM images for nanoflakes of In2S3 on SiO2 for 5 to 15 min.
3.2. Synthesis of In2S3 on ZnO and TiO2 thin films 550–850 ◦ C for 15 min growth time. It may be noted that ZnO and TiO2
layers were pre-deposited on SiO2 substrates by RF sputtering technique
ZnO and TiO2 both are metal oxides with broad bandgap value in the [2]. Fig. 4 (a-f) shows the FESEM images of In2S3 on ZnO/SiO2 and TiO2/
range 3.2–3.5 eV, high electron mobility, and strong room-temperature SiO2 substrate with a different growth temperature of 550–850 ◦ C. Fig. 4
luminescence [24-27]. As already mentioned, the ability of 2D materials (g-h) displays the XRD spectra of In2S3 grown on ZnO and TiO2,
for device applications require the deposition onto functional 3D or 2D respectively.
materials for preparing heterojunctions. With this objective, In2S3 was It is observed that distinct architectures were formed on ZnO and
deposited on the ZnO and TiO2 layers in the temperature range of TiO2 base layers with variation in growth temperature. On the ZnO base
4
N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
Fig. 4. Growth of In2S3 on ZnO and TiO2, (a-f) represents FESEM images of In2S3 grown on ZnO and TiO2 at different deposition temperature, (g-h) XRD patterns of
In2S3 grown on ZnO and TiO2 at 750 ◦ C temperature respectively, and (i) XRD pattern of In2S3 formed on ZnO for temperature range 550–850 ◦ C.
layer, triangular geometry (at 550 ◦ C), nanoflakes with random distri min for SiO2, F-Mica substrates with triangular geometry. The tetragonal
bution (at 750 ◦ C), and hexagonal grains with a size of about 900 nm (at β-In2S3 nanolayers grown on SiO2 substrate with ZnO as a base layer are
850 ◦ C) were obtained. XRD patterns for pristine ZnO and In2S3 grown shown in Fig. 4(i). Within the temperature range, 550–850 ◦ C for 15 min
on ZnO are shown in Fig. 4(g), which indicates the presence of high- growth time, hexagons and nanoflakes are formed. In contrast, for TiO2,
intensity peak corresponding to (0 0 2) plane at 30.67◦ . Lower in not much growth is observed in the low-temperature range. Depending
tensity peaks at 40.48◦ and 52.02◦ corresponds to (1 0 1) and (1 0 2) on the morphology of the substrate, CVD growth is affected, and surface
plane corresponding to the ZnO Wurtzite structure and peaks at 27.57◦ morphology of the layers is affected accordingly. On account of week
corresponding to (1 1 3) plane for In2S3 and some lower intensity peaks Van der Waals interactions between substrates and the overlayers,
at 33.35◦ and 47.76◦ corresponding to (0 0 4) and (3 3 3) planes which distinct morphologies have been formed [28]. Surfaces of SiO2 and Mica
indicate the presence of tetragonal phase of In2S3. are smooth and chemically inert with no dangling bonds on their sur
Fig. 4(d-f) shows the FESEM images for In2S3 deposited on TiO2 base faces. So, the migration energy of adatoms is minimal and responsible
layers in the temperature range of 550–850 ◦ C. It has been observed that for the lateral growth of nonlayered material. At the same time, in the
850 ◦ C growth temperatures, the growth of In2S3 flakes were observed. It case of metal oxides, ZnO, and TiO2, rough surface structure leads to
seems that in this case, the development of In2S3 is not observed at a higher growth density in comparison to nucleation density, so nano
lower temperature. Fig. 4 (h) shows phase analysis of pristine TiO2 and flakes are formed on their surfaces [29]. Also, it is seen that dangling
In2S3 deposited on TiO2, which indicates the formation of the anatase bonds present on the surface of 2D materials leads to high compatibility
phase of TiO2 with a high-intensity peak at 25.45◦ , which corresponds to with traditional 3D materials like ZnO and TiO2.
(1 1 0) plane and low-intense peaks at 48.04◦ and 55.36◦ correspond to Optical properties for 2D nanoflakes of In2S3 have been shown in
(2 1 0) and (2 1 1) planes. Peaks have shown the tetragonal phase of terms of UV–Vis absorption spectra within the wavelength range of
β-In2S3 at 23.52◦ , 27.52◦ , 28.78◦ , 33.35◦ , 43.74◦ , 47.76◦ , 50.38◦ , 320–800 nm, which includes light absorption ability for ZnO and TiO2 in
56.31◦ , 59.67◦ , and 66.86o, corresponding to planes (0 0 2), (1 1 3), the UV range 300–400 nm while for In2S3 in the visible range 500–700
(2 2 2), (0 0 4), (2 2 4), (3 3 3), (0 4 4), (1 3 5), (3 3 5) and (2 2 6) nm.
respectively. Fig. 5 shows the absorption spectra for In2S3 deposited on ZnO and
The above results show that the substrate plays a significant role TiO2 layers. Absorption spectra take place simultaneously in both the
during the growth of In2S3 layers. Well defined layers having tetragonal materials, which remarkably enhancing the light absorption ability to
phase are observed at 750 ◦ C growth temperature and growth time 15 wards the visible region. [30]. These results are similar to those reported
5
N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
Fig. 6. Areal distribution variation (a), (b) &(c) areal density variation with growth temperature 550–850 ◦ C and growth time 5–15 min on SiO2, F-Mica substrate,
ZnO, and TiO2 base layer as substrates.
6
N. Kaur et al. Materials Science & Engineering B 264 (2021) 114889
Fig. 7. (a-c) and (d-f) show Photocurrent variation with voltage and time for In2S3 deposited on F-Mica and SiO2 substrate, respectively.
CRF research facility at IIT Delhi for Raman, XRD, UV-Vis, and FESEM
measurements to be done.
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