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Deposition and characterization of Cu2SnS3 thin films by co-evaporation for

photovoltaic application

Article in Solar Energy Materials and Solar Cells · January 2015

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 Solar Energy Materials & Solar Cells 143 (2015) 128–134

Contents lists available at ScienceDirect

Solar Energy Materials & Solar Cells

journal homepage: www.elsevier.com/locate/solmat

Deposition and characterization of Cu2SnS3 thin films by co-evapora-

tion for photovoltaic application
T. Srinivasa Reddy, R. Amiruddin, M.C. Santhosh Kumar n
Optoelectronic Materials and Devices Laboratory, Department of Physics, National Institute of Technology, Tiruchirappalli, Tamil Nadu 620015, India

art ic l e i nf o a b s t r a c t

Article history: Cu2SnS3 (CTS) is a p-type direct band gap ternary compound semiconductor. Its constituent elements are
Received 11 March 2015 non-toxic, abundant in earth crust and low cost. We report the deposition of Cu2SnS3 thin films on soda-
Received in revised form lime glass substrate by co-evaporation technique at different substrate temperatures. The effect of
24 June 2015
substrate temperature on the growth of CTS thin films has been investigated. X-ray diffraction study
Accepted 24 June 2015
confirms the formation of tetragonal phase of Cu2SnS3. The Raman analysis confirms the ternary/binary
phases of the CTS thin films. The surface morphology of the film is examined by atomic force microscopy
Keywords: (AFM) and Scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) has been used for
Thin films analyzing the film composition. The X-ray photoelectron spectroscopy (XPS) shows that Cu, Sn and S are
Co-evaporation
in the oxidation states of þ 1, þ 4 and  2 respectively. The optical band gap of CTS thin films is 1.23 eV
Copper tin sulfide
and the absorption coefficient is the order of 105 cm  1. Hall measurements confirm the p-type nature of
Electrical properties
Optical properties the as-prepared CTS films. The carrier concentration, resistivity and mobility are 2.81  1021 cm  3,
1.31  10  3 Ω cm and 1.70 cm2 V  1 S  1 respectively.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction semiconductor Cu2SnS3 (CTS) is a p-type direct band gap material

and its elements are non-toxic and earth abundant. It is a known
The conventional thin film solar cell (TFSC) materials like CIGS fact that, CTS exhibits dimorphic or polymorphic phases with a
and CdTe played a major role in the development of thin film solar phase transition occurring at 780 °C. The high temperature phases
cells. These thin film solar cells composed of rare elements like In, of CTS above 780 °C are reported as isomorphic with sphalerite
Ga, Te or heavy metals, which are toxic in nature. Cu2ZnSnS4 structure (cubic) [2], and low temperature phases are reported as
(CZTS) is an emerging absorber layer material, which can replace tetragonal [4], monoclinic [5] and triclinic [6]. CTS have been
existing CdTe and CIGS absorbers. TFSCs with CZTS as absorber reported to have band gap energies in the range of 1.15 eV and an
layer have yielded efficiency of 8.4% using vacuum evaporation [1]. absorption coefficient greater than 104 cm  1 [7]. The thin films of
The compound semiconductor CZTS has direct band gap energy in Cu2SnS3 (CTS) have been prepared using several techniques like
the range of 1.4–1.6 eV and have large absorption coefficient in the direct liquid coating [8], spray pyrolysis technique [7], spin coating
[4,6], sulfurization of stacked metal precursors [2] and successive
order of 104 cm  1, which is suitable for photovoltaic absorber
ionic layer absorption and reaction (SILAR) [9].
layer in solar cells. Despite these advantages the CZTS having
In the present work copper tin sulfide (CTS) thin films have been
uncontrollable growth condition leading to the formation of the
prepared by co-evaporation technique. There are only a few reports
binary and ternary phases along with the desired CZTS phase [2].
available for deposition of ternary compound semiconductor thin films
Some Cu–Sn–S ternary compounds are formed in the presence of
using co-evaporation technique [10,11]. In this investigation CTS films
CZTS thin films. These ternary compound exhibits a variety of
are deposited on soda-lime glass at different substrate temperature
phases like Cu2SnS3, Cu3SnS4 and Cu4SnS4 [3]. Another approach from 200 °C to 300 °C. The structural, morphological, optical and
to overcome this problem is to go for a ternary material with electrical properties of the co-evaporated CTS thin films are studied
similar structure and material properties to that of CZTS. The and reported for the first time.
ternary compound Cu2SnS3 (CTS) is a promising absorber material
for photovoltaic application. The ternary compound
2. Experimental
n
Corresponding author.
E-mail addresses: [email protected], Copper tin sulfide (CTS) thin films have been deposited on
[email protected] (M.C. Santhosh Kumar). soda-lime glass substrate using co-evaporation technique. A 12ʺ

http://dx.doi.org/10.1016/j.solmat.2015.06.049
0927-0248/& 2015 Elsevier B.V. All rights reserved.
 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134 129

vacuum coater, which consists of oil diffusion pump coupled with

rotary pump, was used for deposition of CTS thin films at a vacuum
better than 7  10  6 mbar. Copper wire (Sigma-Aldrich, 99.999%),
tin wire (Sigma-Aldrich, 99.999%) and sulfur powder (Sigma-
Aldrich) were taken as source materials. Ultrasonically cleaned
soda-lime glass was used as substrates. Copper and tin were eva-
porated from two separate molybdenum boats and the sulfur
powder was evaporated from a glass crucible kept in a tungsten
basket. The working pressure of the three-source vacuum coating
unit was 5.5  10  5 mbar. After reaching the evaporation tem-
perature of source materials, shutter over the boats was moved to
sideway for the deposition the film on the substrate [10]. A 1 kW
heater with PID controller was used as the substrate heater. CTS
thin films were deposited at substrate temperature of 200 °C,
250 °C and 300 °C. The source to substrate distance was fixed at
22 cm. In the present study, thin films were deposited on optically
flat soda-lime glass substrates. The glass slides were first cleaned
with detergent solution and then thoroughly washed in running Fig. 1. XRD patterns of the Cu2SnS3 thin films at different substrate temperatures.
water. These slides were cleaned with double distilled water and
followed by ultrasonic cleaning for 30 min. These substrates were of the film deposited at substrate temperature of 250 °C were
cleaned with acetone, then dried with a hot-air dryer and loaded calculated using the relation:
into the substrate holder of vacuum chamber. The substrates were
further cleaned by ion-bombardment (HT) in vacuum chamber for ⎡ h2 + k 2 ⎤
10 min, prior to the deposition of the film. 1 l2
=⎢ ⎥+
X-ray diffraction (XRD) was used to confirm the structure and d(2hkl) ⎣ a 2 ⎦ c2 (1)
phase of the CTS thin films. Cu Kα radiation (λ ¼1.54 Å) was used to
record the spectrum in the range of angle (2θ) 20–80°. The Raman where d is the interplanar distance and (hkl) are the Miller indices.
analysis was carried out using Renishaw inVia micro-Raman The evaluated lattice parameters are a ¼5.412 Å, b ¼5.412 Å and
spectrometer. Scanning electron microscopy (SEM) and energy c¼ 10.860 Å. These values are very close to the tetragonal system
dispersive spectroscopy (EDS) was used to analyze the morphol- of CTS film (JCPDS 89-4714). The average crystallite size of the
ogy and chemical composition of the films by using Zeiss Ultra 55 samples was calculated from the full width at the half-maximum
FESEM with Oxford EDX system. The atomic force microscopy (FWHM) of the peak (β), using the Debye–Scherrer equation as
(AFM-Park NX10) was used to study the surface roughness of the follows:
films. The X-ray photoelectron spectroscopy was used to study the
binding energy for core level of the films using PHI 5000 Versa 0.94λ
D=
Probe-II. The optical band gap, absorption coefficient, extinction β cos θ (2)
coefficient and refractive index of CTS films have been computed
from optical absorbance and reflectance measurements. The where λ is the wavelength of the X-ray radiation (1.54 Å ) and θ is
optical absorbance spectra were recorded using UV–vis–NIR the Bragg angle of the peak. The average crystallite sizes of all
spectroscopy (JASCO V-670) in the range of wavelength 200– deposited CTS thin films increases from 10.7 nm to 14 nm with
2500 nm. Hall measurement technique (ECOPIA HMS-5000) was increase of substrate temperature. Thus, the average crystallite size
employed for electrical measurements using vander pauw of the film deposited at 250 °C using the highest peak (112) is
configuration. 12 nm, which is close to the value (11.4 nm) observed for CTS film
grown by spray pyrolysis technique [12].
Raman spectroscopy is a standard characterization technique to
3. Results and discussion
reveal the exact phases of ternary semiconductor compound thin
films. Fig. 2 shows the Raman spectra of the film deposited at the
3.1. Structral and Raman study
substrate temperature of 250 °C in the wavelength range
Fig. 1 shows the X-ray diffraction patterns of the CTS thin films 50–600 cm  1 with Gaussian fitting. The micro-Raman spectra
deposited at different substrate temperatures. The XRD patterns contains modes at 71 cm  1, 127 cm  1, 285 cm  1, 332 cm  1 and
indicate the as-deposited films are polycrystalline in nature. The 472 cm  1. The modes at 285 cm  1 and 332 cm  1 are character-
diffraction peaks for the samples prepared at 250 °C are istic vibration symmetry of the tetragonal phase of Cu2SnS3 thin
2θ ¼ 28.46°, 29.84°, 38.26°, 44.52°, 47.45°, 64.78° and 71.91° could films. The high intense mode at 332 cm  1 attributed to the tet-
be assigned to (112), (103), (211), (213), (220), (314) and (413) ragonal phase of Cu2SnS3, which is in close agreement with
planes respectively. The XRD patterns of the sample are in close reported Raman data by Guan et al. [9]. The mode at 285 cm  1 is
agreement with standard tetragonal phase of Cu2SnS3 (JCPDS 89- assigned to the tetragonal phase of Cu2SnS3 as reported earlier by
4714). These results are in good agreement with those reported by Han et al. [6]. The slight difference in the frequency might be due
Fernandes et al. [2]. The principal peak of the films deposited at
to composition, growth condition and microstructure of the CTS
250 °C is 28.46°corresponding to the (112) plane, which indicates
thin films. The tetragonal (Cu2SnS3) and binary phases (Cu2S,
the preferred crystallization along this plane. The secondary pha-
Sn2S3) of the film deposited at substrate temperature of 250 °C are
ses Cu2S are present for all deposited films at 31.69°. Similar binary
phases are also reported by Fernandes et al. [2]. In addition to this, reveled by XRD analysis. The mode at 472 cm  1 is a characteristic
for all deposited films, there is a peak at 21.21°. This peak binary phases of Cu2S [13]. The mode at 71 cm  1 is attributed to
corresponds to (103) plane of binary phase Sn2S3 (JCPDS 75- the binary phase of Sn2S3 phase [14]. The low intensity mode at
21830). The lattice parameters corresponding to tetragonal phase 127 cm  1, attributed to the binary phase of SnS [15].
130 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134

are in þ1, þ 4 and  2 oxidation states respectively. These results

are in good agreements with the CTS films prepared by spin
coating technique [6]. From XPS, the quantitative analysis is car-
ried out to find the elemental concentration of CTS thin films
deposited at the substrate temperature of 250 °C. The relative
concentration of Cu, Sn and S is observed as 36.96%, 19.11% and
43.68% respectively. No other major elements are detected on the
sample surface. XPS results are closer to the results observed by
EDX. The atomic percentage and molar ratios of elements in CTS
thin film are tabulated in Table 1.

3.3. Morphology

Fig. 5 shows SEM micrographs of the CTS thin films deposited

at a substrate temperature of 250 °C. Fig. 4a shows the top view
and Fig. 4b depicts the cross sectional images of the as-deposited
CTS films. From this micrograph, it is evident that fibrous with
quasi-equilateral hexagonal shaped grains are continuously dis-
Fig. 2. Raman spectrum of Cu2SnS3 thin films deposited at substrate temperature tributed throughout the sample without any visible cracks and
of 250 °C. holes. Chalapathi et al. [16] also observed similar morphology of
Cu2SnS3 thin films by co-evaporation technique. The thickness of
3.2. Composition the CTS thin films on the soda-lime glass is estimated as 690 nm
from the cross sectional view.
Table 1 shows elemental composition of CTS film deposited at Fig. 6 shows the AFM micrograph of CTS thin films deposited on
substrate temperature of 250 °C. EDX measurement is carried out glass substrate at a substrate temperature of 250 °C. AFM studies
in the as-prepared samples using Cu-Lα, Sn-Lα and S-Kα (FeS) as reveal that the as-deposited CTS films are fairly smooth and free
standards. X-ray energies correspond to Cu, Sn and S are observed from voids. The root mean square roughness (RMS) of the films
at 0.932 keV, 3.442 keV and 2.307 keV respectively. The elemental deposited at 250 °C is 19 nm. This RMS value is lower than the
composition of the film deposited at substrate temperature of value (42 nm) of the CTS film deposited using spin coating
250 °C is observed as Cu¼ 32.07 at%, Sn¼ 16.56 at% and reported by Dahman et al. [4]. The film consists of spherical shape
S¼51.37 at%. Fig. 3 shows the elemental mapping of the CTS thin grains with different diameter ranges from 180–677 nm. The for-
film deposited at substrate temperature of 250 °C. The elemental mation of this type of grains depends on the growth conditions. In
mapping confirms the presence and uniform distribution of Cu, Sn the present study, some parameters like rate of deposition, sub-
and S throughout the sample. From this data, it can be noticed that strate temperature and source–substrate distance may be the
Cu/Sn ratio of the prepared sample is 1.93 and S/(Sn þCu) ratio is cause of such crystallites formation on the substrate.
1.05. The films showed S/metal ratio closed to unity. Thus, it is
confirmed that sulfur quantity is enough for formation of the CTS
3.4. Optical study
compound films and also observed that it was homogeneous and
close to stoichiometric ratio.
The optical absorption of the deposited CTS films on soda-lime
Fig. 4 shows the XPS scan of the CTS film deposited at the
glass at different substrate temperature was studied in the wave-
substrate temperature of 250 °C. From the XPS data it is observed
length range 300–2500 nm using UV–vis–NIR spectrometer. From
that the core level photoelectron spectra of Cu 2p, Sn 3d, and S 2p,
Fig. 7, one can note that the material exhibit sharp absorption edge
along with Gaussian fitting. The binding energy for core level of Cu
and it absorbs entire visible wavelength region.
2p is shown in Fig. 3(a). The observed values of binding energies
Fig. 8 shows the absorption coefficient of all the CTS thin films
for Cu 2p3/2 and Cu 2p1/2 are 931.91 eV and 951.83 eV respectively.
deposited on soda-lime glass substrate at different temperatures.
No shake-up peaks are observed around 942–943 eV, which
The absorption coefficient was calculated using the formula:
indicates that the nonexistence of the Cu þ 2 ionic state. Similarly,
core level of the Sn 3d is shown in Fig. 3(b). The binding energy for (
αhν = A hν−E g )n (3)
the core level of the Sn 3d5/2 and Sn 3d3/2 are 486.93 eV and
495.38 eV respectively. These experimental values indicate that where Eg is the band gap, α is absorption coefficient, ν is the fre-
the presence of Sn in þ4 oxidation state. The binding energy for quency, A is a constant, n can have values 1/2, 3/2, 2, 3 depending
core level of S 2p is shown in Fig. 3(c). The binding energy of the S upon the mode of interband transition. From this graph, it is
2p3/2 and S 2p1/2 are 161.90 eV and162.92 eV respectively. These observed that the absorption coefficients (α) of all the samples are
values indicate that sample consists of S in S  2 oxidation state. No above 105 cm  1 near the fundamental absorption edge. This result
other elements are observed in the XPS scan. The XPS investiga- is in good agreement with direct-coated CTS thin films by Tiwari
tion confirms that Cu, Sn and S present in the as prepared sample et al. [8].
The band gap of the CTS films is calculated using the Tauc plot
Table 1 of (αhν)2 vs. hν for all the samples (Fig. 9). The direct band gap of
Elemental composition of the Cu2SnS3 thin films deposited at a substrate tem- the CTS films deposited at 200 °C, 250 °C and 300 °C are estimated
perature of 250 °C calculated using EDX and XPS spectroscopy techniques.
as 1.60 eV, 1.23 eV and 1.65 eV respectively. The band gap of the
Sample Measurement method Atomic percent Mole ratios CTS film at substrate temperature 250 °C is 1.23 eV, which is lower
Cu Sn S Cu:Sn:S than the band gap value (1.35 eV) obtained by spin coating [4]. The
band gap and absorption coefficient of the film at substrate tem-
250 °C EDX 32.07 16.56 51.37 1.93:1:3.10
perature 250 °C are closer to the optimum value of band gap
XPS 36.96 19.11 43.68 1.93:1:2.29
required for the photovoltaic application.
 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134 131

Fig. 3. Elemental mapping of Cu2SnS3 thin films deposited at substrate temperature of 250 °C.

The refractive index n(λ) and extinction coefficient k(λ) of the 2.81  1021 cm  3, 1.31  10  3 Ω cm and 1.70 cm2 V  1 S  1
CTS film deposited at substrate temperature 250 °C are calculated respectively.
in the wavelength range of 300–1000 nm. The extinction coeffi-
cient (k) is calculated using the relation α ¼ 4πk/λ and refractive
index (n) of the film is calculated by using the following Eq. (4): 4. Conclusion
(n − 1)2 + k 2
R=
(n + 1)2 + k 2 (4) Copper tin sulfide (Cu2SnS3) thin films were successfully pre-
pared on glass substrate by co-evaporation technique at different
The variation of the refractive index and extinction coefficient
substrate temperature (200–300 °C). Slight amorphous nature was
with wavelength is shown in Fig. 10. The refractive index values n
observed for all deposited CTS thin films. The XRD pattern of the
(λ) are constant up to the wavelength 560 nm, and then the value
film deposited at substrate temperature of 250 °C showed better
increases with increase of wavelength. The extinction coefficient
polycrystalline nature compared to the films deposited at sub-
(k) decreases with increase of the wavelength up to 560 nm and
strate temperature of 200 °C and 300 °C. The XRD pattern of the
then attains almost constant value towards higher wavelength.
films deposited at 250 °C showed polycrystalline CTS with pre-
3.5. Electrical ferred orientation along (112) plane and have an average crystallite
size of 12 nm. XPS studies confirmed the oxidation states of Cu, Sn
Electrical properties of the CTS films deposited on glass sub- and S as þ1, þ 4 and  2 respectively. The AFM studies showed
strate at different temperature are studied using Hall measure- that the as-deposited films have roughness of 19 nm and the films
ment technique at room temperature. The experimental results are free from voids. Raman studies confirmed the tetragonal phase
are tabulated in Table 2. It can be noticed that all the samples and binary phases present in the CTS thin film deposited at the
exhibit p-type semiconductor behavior. The sample prepared at of substrate temperature of 250 °C. The conversion efficiency of the
250 °C shows higher mobility, carrier concentration and lower solar cell depends on the absorption coefficient, optimum band
resistivity compared to the films deposited at 200 °C and 300 °C. gap, carrier concentration, mobility, morphology of the absorption
The lower resistivity of the film deposited at substrate tempera- layer. In the present study, CTS film deposited at substrate tem-
ture of 250 °C might be due to the dominance of highly conducting perature 250 °C having high absorption coefficient (410  5 cm  1)
ternary phase over the binary phases. The carrier concentration, and optimum band gap (1.23 eV). The morphology and nm scale
resistivity and mobility of CTS films deposited at 250 °C are grains of the film deposited at substrate temperature of 250 °C is
132 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134

Fig. 4. X-ray photoelectron spectra of Cu2SnS3 film deposited at substrate temperature of 250 °C (a) Cu 2p core level (b) Sn 3d core level (c) S 2p core level with Gaussian
fitting curves.

Fig. 5. (a) Top view and (b) cross sectional image of the Cu2SnS3 films deposited at substrate temperature of 250 °C.

continuous and uniform throughout the film without pin holes mobility varies from 1.28 to 1.70 cm2 V−1S−1 and low resistivity in
and voids. The Hall measurement showed that the films are p-type the order of 10  3 Ω cm. From the present investigation it is clear
in nature. From Hall data, it is observed that all deposited films that the CTS thin films can be a potential absorber layer material
possess higher carrier concentration in the order of 1021 cm  3, for thin film solar cells.
 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134 133

Fig. 6. Atomic force micrographs (AFM) of the Cu2SnS3 film deposited at substrate temperature 250 °C (a) 2-dimensional view (b) 3-dimentional view.

Fig. 7. Absorbance spectra of the Cu2SnS3 films deposited at different substrate

temperatures.
Fig. 9. Tauc plot of (αhν)2 vs. hν for energy band gap determination.

Fig. 8. The variation of α vs. hν of the Cu2SnS3 films deposited at different Fig. 10. The variation of the refractive index and extinction coefficient of the
temperatures. Cu2SnS3 film deposited at 250 °C.
134 T. Srinivasa Reddy et al. / Solar Energy Materials & Solar Cells 143 (2015) 128–134

Table 2
Electrical properties of the Cu2SnS3 films deposited at different substrate temperature calculated using vander pauw method.

Sample substrate temperature (°C) Carrier concentration no. (cm  3) Resistivity (Ω cm) Mobility (cm2/VS) Carrier type

200 (1.86 7 0.47)  1021 (2.63 7 0.01)  10  3 1.28 7 0.18 p

250 (2.817 0.68)  10 21 (1.317 0.11)  10  3 1.707 0.24 p
300 (2.527 0.34)  1021 (1.89 7 0.05)  10  3 1.317 0.33 p

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