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    Dependence of CZTS thin film properties and photovoltaic performance on heating rate and sulfurization time
    (Elsevier Science Sa, 2023) Olgar, M. A.; Erkan, S.; Zan, R.
    In this study, effect of heating rate and sulfurization time on the properties of CZTS thin films and their photovoltaic performances was investigated. CZTS layers were prepared by a two-stage technique comprising deposition of precursor films by sputtering on Mo-foil substrates (Mo-foil/ZnS/CuSn/Cu) and a sulfurization process utilizing Rapid Thermal Annealing (RTA) approach. Heating rates and sulfurization times at 550 degrees C were changed to determine the best conditions. CZTS films were characterized by several techniques. All samples showed Cu-poor and Zn-rich chemical composition regardless of the heating rate and annealing time of the sulfurization process. XRD diffraction patterns showed that only kesterite CZTS phase was formed in all samples. Although Raman spectroscopy measurements confirmed formation of kesterite CZTS phase in all samples, forming of Cu2SnS3 (CTS) secondary phase was detected in all films except for the sample prepared utilizing a relatively low heating rate of 1 degrees C/s and 60 s sulfurization time (CZTS-I-60). The largest crystallite size and the less micro strain and dislocation density were also found in this sample. All CZTS thin films displayed dense and compact polycrystalline surface microstructure. Optical characterizations showed that the optical band gaps of the films were in the range of 1.48-1.58 eV. PL emission spectra of the films exhibited transition from conduction band to acceptor/defect levels instead of band-to-band transition. Solar cells were fabricated and the highest Voc and conversion efficiency (4.39%) were achieved employing the film obtained with ramp rate of 1 degrees C/s and the sulfurization time of 60 s, because of better structural properties and purer crystal structure determined for this sample.
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    Enhancement in photovoltaic performance of CZTS Thin-film solar cells through varying stacking order and sulfurization time
    (Springer, 2022) Olgar, M. A.
    The CZTS samples were produced by a two-stage method, which includes deposition of Cu, Sn, Zn, and ZnS layers using magnetron sputtering to obtain CuSn/Zn/Cu and CuSn/ZnS/Cu stacks. The latter stage involves the sulfurization process of stacked films at 550 degrees C for varied sulfurization time (60, 90, 120, and 150 s) employing Rapid Thermal Processing (RTP) method to attain CZTS structure. The prepared CZTS thin films were analyzed utilizing several characterization methods. The energy-dispersive X-ray spectroscopy (EDX) measurements revealed that all sulfurized samples had Cu-poor and Zn-rich chemical composition. All samples showed that diffraction peaks belonged to pure kesterite CZTS phase subject to their XRD patterns. Besides, it was observed that the sulfurization time had a crucial effect on the crystal size of the samples. The Raman spectra of the samples verified the constitution of kesterite CZTS phase and it provides detection of some CTS-based secondary phases. The scanning electron microscopy (SEM) image of the films revealed that polycrystalline surface structures were observable in all the samples. However, plate-like surface features were observed in some samples that may refer to CTS-based secondary phases depending on chemical composition. From 1.40 to 1.48 eV optical band gap values were obtained from (alpha chv)(2) vs. photon energy (hv) plots. The Van der Pauw measurements exhibited that the CZTS samples produced employing CuSn/ZnS/Cu stack had lower resistivity (similar to 10(-3) Omega cm), higher carrier concentration values (similar to 10(21) cm(-3)), and higher charge mobility. The solar cells prepared using the most promising CZTS samples employing CuSn/Zn/Cu and CuSn/ZnS/Cu precursor films revealed 1.95% and 3.10% conversion efficiencies, respectively.
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    Fabrication of Cu-rich CZTS thin films by two-stage process: Effect of gas flow-rate in sulfurization process
    (Elsevier, 2021) Olgar, M. A.; Altuntepe, A.; Erkan, S.; Zan, R.
    In this study, CZTS thin films were prepared using a two-stage process consisting of sputter deposition of Cu, Sn and ZnS layers on the glass substrates to form CuSn/ZnS/Cu stacked precursor films followed by sulfurization process under various flow-rate (0, 20, 40, 60, 80, 100 sccm) of Ar+ H-2 mix gas in a tubular furnace. The EDX measurements of the precursor and reacted films are Cu-rich and Zn-rich composition. However, Zn and Sn loss was observed for samples annealed under the flow-rate of gas above the 60 sccm. The XRD pattern of the samples showed diffraction peaks of pure kesterite CZTS structure and the FWHM values extracted from their XRD patterns and W-H plot calculations demonstrated that CZTS-40 thin film had a more desired crystallite size. The Raman spectra of the samples confirmed the formation of CZTS phase for all samples and indicated the formation of some secondary phases such as Cu2SnS3, SnS2, Sn2S3 except for CZTS-40 thin film. All the samples displayed dense and polycrystalline microstructure according to their SEM images. The optical band gap values of CZTS samples showed variation between 1.40 and 1.48 eV. The room-temperature PL spectra of the samples revealed a broad band that had a peak value at around 1.36-1.40 eV that are close to the optical band gap values for prepared CZTS samples. (C) 2021 Elsevier B.V. All rights reserved.
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    Impact of in/ex situ annealing and reaction temperature on structural, optical and electrical properties of SnS thin films
    (Elsevier, 2021) Olgar, M. A.; Ciri, A.; Tomakin, M.; Zan, R.
    In this work, SnS thin films were prepared by in situ and ex situ annealing process of precursor films deposited by RF (Radio Frequency) magnetron sputtering employing binary SnS target. In situ annealing treatment was performed in sputtering chamber and ex situ annealing treatment was performed using RTP (Rapid Thermal Processing) system under Ar+H-2 mix gas employing 225, 300 and 375 degrees C as reaction temperatures in order to find out the best fabrication parameters of SnS thin film since it has been used as an absorber layer in the cell structure. The EDX (Energy Dispersive X-ray Spectroscopy) measurements showed that precursor and reacted films have almost stoichiometric composition except for in situ annealed sample at 375 degrees C. XRD (X-ray Diffraction) patterns of all samples revealed orthorhombic SnS phase regardless of annealing route and temperature. In addition to SnS phase, formation of SnS2 phase was observed in in situ annealed SnS samples at 225 and 300 degrees C. Moreover, in situ annealed samples displayed larger crystallite size and lower micro strain compared to ex situ annealed samples. Raman spectra of the samples confirmed formation of orthorhombic SnS phase and it was also seen that crystalline quality gave rise to shift in position of Raman bands for some samples. Only a SEM (Scanning Electron Microscopy) image of in situ annealed sample at 375 degrees C displayed distinct surface morphology. Optical band gap values of the samples showed variation between 1.35 and 1.66 eV. Electrical characterization of the films showed that resistivity values changed from 3.34x10(3) to 2.28x10(4) Omega-cm and carrier concentration values changed from 1.34x10(14) to 1.05x10(15) cm(-3). It was seen that in situ annealing at 375 degrees C exhibited more promising results for potential SnS based photovoltaic applications. (C) 2021 Elsevier B.V. All rights reserved.
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    Impact of stacking order and annealing temperature on properties of CZTS thin films and solar cell performance
    (Pergamon-Elsevier Science Ltd, 2021) Olgar, M. A.; Sarp, A. O.; Seyhan, A.; Zan, R.
    In this study, Cu2ZnSnS4 (CZTS) thin films were synthesized by a two-stage process. In the first stage, CuSn/Zn/Cu (E-type) and CuSn/ZnS/Cu (B-type) stacked films were formed using the sputtering method. In the second stage, precursor films were annealed in sulfur atmosphere utilizing various annealing temperatures (500, 525, 550 and 575 degrees C) employing the Rapid Thermal Processing (RTP) method. The EDX measurements demonstrated that almost all the samples had Cu-poor and Zn-rich compositions, as targeted. The XRD patterns of all the CZTS samples were dominated by diffraction peaks of the kesterite CZTS phase. In addition to CZTS phase, Cu-S/Sn-S based secondary phases in all E-type CZTS thin films and some B-type CZTS samples annealed at lower temperatures (500 and 525 degrees C) were observed. The samples annealed at above 525 degrees C revealed purer crystal structure in terms of secondary phases and they have more promising crystallite size in both types of CZTS thin films. The Raman spectroscopy measurements confirmed the formation of kesterite CZTS phase and distinguished the formation of Cu2SnS3 (CTS) phase for some samples. The samples annealed at 550 degrees C presented purer structure for potential solar cell application. The SEM surface and cross-section images of all CZTS samples displayed dense and polycrystalline structures but samples annealed at 550 degrees C presented a larger-grained surface and crosssection structure in both types of CZTS films. PL spectra of the B-type CZTS samples exhibited a purer band structure with respect to E type CZTS samples according to their PL band values. The best solar cell performance was achieved with CZTS thin film prepared using CuSn/ZnS/Cu stack annealed at 550 degrees C temperature with 252 mV, 32 mA/cm(2), and 3.79% parameters. (C) 2021 Elsevier Ltd. All rights reserved.
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    Impact of sulfurization parameters on properties of CZTS thin films grown using quaternary target
    (Springer, 2020) Olgar, M. A.; Seyhan, A.; Sarp, A. O.; Zan, R.
    In this study, CZTS thin films were grown by annealing of sputtered films using quaternary single target employing various annealing parameters. The effects of the post-sulfurization treatment, reaction temperature (500, 525, 550 and 575 degrees C) and sulfurization time (60, 90, 120 and 150 s) on the properties of CZTS thin films were analyzed. The optimization of reaction temperature for 60 s dwell time was examined by annealing the precursor films with/without sulfur atmosphere. It was shown that annealing of the films under the sulfur atmosphere prevents Zn-loss in the samples for higher annealing temperatures (550 and 575 degrees C) and hindering the formation of secondary phases such as Cu2-xS, Cu2SnS3(CTS). The FWHM values of the sulfurized samples revealed that the sulfurization temperature of 550 degrees C is preferable for the fabrication of CZTS samples. Further optimization was performed at 550 degrees C for various sulfurization times. It was seen that all the samples have Cu-poor and Zn-rich composition. The XRD pattern of CZTS samples displayed formation of kesterite CZTS phase but SnS(2)phase formations were also observed for longer sulfurization time (> 120 s). It was also observed that the sulfurization time has more significant contribution on the crystallite size of the samples with respect to sulfurization temperature. The Raman spectra of the CZTS samples confirmed the formation of kesterite structures for all the films and appearance of secondary phase for films prepared using longer sulfurization time (> 120 s). All the samples displayed a dense and polycrystalline surface morphology, but the sulfurized sample for 120 s displayed more homogenous and prominent morphology. The room temperature PL measurements demonstrated a broad band which peaked at about 1.36-1.37 eV, which is very close to the band gap of kesterite CZTS structure. The electrical characterization of the samples showed that all the samples have p-type conductivity and the CZTS-S-550-120 sample has a more promising result considering both resistivity and carrier concentration.
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    Impact of the ZnS layer position in a stacked precursor film on the properties of CZTS films grown on flexible molybdenum substrates
    (Elsevier, 2023) Yagmyrov, A.; Erkan, S.; Basol, B. M.; Zan, R.; Olgar, M. A.
    In the present study, CZTS thin films were prepared by annealing and reaction of Cu-Sn-ZnS precursor layers. First, sputter deposition was carried out on flexible molybdenum (Mo) foil to form Mo-foil/CuSn/ZnS/Cu, Mo-foil/CuSn/Cu/ZnS and Mo-foil/ZnS/CuSn/Cu stacked precursor structures. Annealing process was performed in sulfur atmosphere using Rapid Thermal Processing (RTP) method to obtain kesterite CZTS phase in the reacted layers. All prepared precursors and CZTS thin films displayed Cu-poor and Zn-rich chemical composition, as targeted. XRD patterns of CZTS samples showed that the kesterite phase was obtained in all samples regardless of the stacking order of the precursor films. However, the full width at half maximum (FWHM) values of the (112) preferential peaks extracted from the XRD patterns, and the corresponding structural parameters (crystallite size and microstrain), indicated that the Mo-foil/ZnS/CuSn/Cu precursor structure yielded more promising crystal-line quality. The occurrence of kesterite phase in all samples and existence of low amount of CTS phase were verified by Raman spectroscopy measurements. The CZTS sample prepared employing the Mo-foil/ZnS/CuSn/Cu precursor film structure presented more prominent, homogenous and compact surface microstructure as observed in SEM images. Optical band gap values were found to be in the range of 1.44-1.50 eV. The room temperature photoluminescence (PL) measurements showed that the transitions from the conduction band to intrinsic defect levels dominated the spectra instead of the band-to-band transitions. Electrical characterization of the films showed that Mo-foil/CuSn/ZnS/Cu and Mo-foil/ZnS/CuSn/Cu precursor films yielded lower elec-trical resistivity and higher carrier concentration due to better crystalline quality. Overall, it was seen that the CZTS thin films produced using the Mo-foil/ZnS/CuSn/Cu stacked precursor layers displayed better properties in terms of crystalline quality, surface microstructure, and optical and electrical properties, which are favorable for photovoltaic applications.
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    Improvement in the structural and optical properties of Cu2SnS3 (CTS) thin films through soft-annealing treatment
    (Academic Press Ltd- Elsevier Science Ltd, 2020) Olgar, M. A.
    In this work, Cu2SnS3 thin films were synthesized by soft-annealing treatment of Cu and Sn film layers at various temperatures (200, 250, 300, and 350 degrees C) deposited on molybdenum-coated glass (Mo/Cu/Sn) employing sequential sputter deposition technique followed by sulfurization process at 550 degrees C utilizing RTP. Effect of the soft-annealing treatment and temperature on the compositional, structural and optical properties of CTS thin film was examined using EDX, XRD, Raman spectroscopy, SEM, and optical spectroscopy techniques. All CTS films demonstrated Cu-poor composition regardless of the soft-annealing treatment according to EDX measurements. Irrespective of the soft-annealing temperature, all samples showed formation of monoclinic crystal structure of CTS phase and some secondary phases in their XRD patterns. It was found that the sample soft-annealed at 250 degrees C had more desired crystalline quality amongst the other prepared samples. Formation of the CTS structure was confirmed by Raman spectroscopy measurements. SEM images of the samples demonstrated denser and smoother microstructure by raising the soft-annealing temperature up to 250 degrees C. Optical band gap of the films showed variation between 0.85 eV and 0.90 eV that may be influenced by crystalline quality of the films.
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    Integration of single layer graphene into CZTS thin film solar cells
    (Elsevier Science Sa, 2022) Erkan, S.; Yagmyrov, A.; Altuntepe, A.; Zan, R.; Olgar, M. A.
    In this study, CZTS samples were produced on Mo and graphene/Mo coated glass substrates using qua-ternary target. The CZTS thin films deposited by RF magnetron sputtering were annealed using rapid thermal processing (RTP) method in sulphur atmosphere at 500, 525, and 550 degrees C so as to obtain glass/Mo/ CZTS and glass/Mo/graphene/CZTS (g-CZTS) structures. The obtained CZTS and g-CZTS thin films were then characterized by several methods such as EDX, XRD, Raman spectroscopy, SEM etc. The EDX data demon-strated that all CZTS thin films had Cu poor composition regardless of the sulfurization temperature and increasing the temperature led to Sn loss from the films. Diffraction peaks of kesterite CZTS phase were observed in all the samples; additionally, SnS and CuS secondary phases were also observed in CZTS samples annealed at 500 degrees C. The crystallite size of the CZTS thin films were found to be increasing with both increasing annealing temperature and use of graphene film as an inter-layer. The creation of kesterite phase with a very small CTS phase in all the samples were verified by the Raman spectroscopy measurement. The SEM images of the samples indicated that using graphene improves the crystalline quality of the CZTS films and contributes to forming more compact, homogenous and larger crystal structure. The determined optical band gap values varied from 1.41 to 1.44 eV depending on the Sn-content of the samples. The produced solar cells selected from the more promising absorber layers showed that implementing graphene in CZTS cell structure enhanced the conversion efficiency from 2.40% to 3.52% due to improvement of crystalline quality of the absorber layer. (c) 2022 Elsevier B.V. All rights reserved.
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    Phase transformation in Cu2SnS3 (CTS) thin films through pre-treatment in sulfur atmosphere
    (Springer, 2021) Olgar, M. A.; Basol, B. M.; Tomakin, M.; Bacaksiz, E.
    In this study, Cu2SnS3 (CTS) thin films prepared by a two-step sulfurization process were characterized. Cu and Sn metallic layers were first deposited on glass substrates by sputtering and then annealed in-situ while in the sputtering chamber to obtain CuSn (CT) alloys. This was followed by a pre-treatment step at temperatures between 200 and 350 degrees C in presence of S vapors. Finally, a full sulfurization step was performed at 525 degrees C to obtain the desired CTS phase. CTS films were characterized using EDX, XRD, Raman spectroscopy, SEM, optical transmission and Van der Pauw methods. It was found that all CTS samples had Cu-poor chemical composition. XRD data revealed only diffraction peaks belonging to CTS structure after the full sulfurization step. Raman spectra of the samples showed that except for the CTS sample pre-treated at 250 degrees C (CTS-250), which displayed the tetragonal crystal system, the films were dominated by the monoclinic structure. SEM surface images showed dense and polycrystalline microstructure, CTS-200 sample exhibiting a more uniform morphology. Optical band gap values were found to be ranging from 0.92 to 1.19 eV. All samples showed p-type conductivity but the sample pre-treated at 350 degrees C had higher resistivity and lower carrier concentration values. Overall, the CTS layer prepared using the pre-treatment step at 200 degrees C exhibited more promising structural and optical properties for potential photovoltaic applications. This work demonstrated that it is possible to change the crystal structure of sulfurized CTS thin films through a pre-treatment step.
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    The choice of Zn or ZnS layer in the stacked precursors for preparation of Cu2ZnSnS4 (CZTS) thin films
    (Academic Press Ltd- Elsevier Science Ltd, 2020) Olgar, M. A.; Seyhan, A.; Sarp, A. O.; Zan, R.
    Cu2ZnSnS4 (CZTS) thin films are commonly used as an absorber layer in the thin film solar cell structure. In this study, CZTS thin films were produced by sulfurization of stacked precursor films that is prepared by deposition of Cu, Zn, SnS, ZnS films on glass substrate using sputtering method. The sequential sputter deposition was performed to obtain two distinct stacked precursors, Cu/SnS/Zn/Cu and Cu/SnS/ZnS/Cu respectively. Afterwards, annealing process was implemented at various reaction temperatures (500-575 degrees C) for 1 min utilizing rapid thermal processing (RTP). The EDX measurements revealed that all the prepared CZTS samples had Cu-poor and Zn-rich composition that are non-stoichiometric chemical composition. This non-stoichiometric composition is important for high efficient CZTS based solar cells. XRD measurements revealed that all patterns are dominated by diffraction planes of kesterite CZTS. The CuS, Cu2S and SnS2 secondary phases also were detected in the XRD pattern of some CZTS films. Raman spectroscopy measurements verified formation of kesterite CZTS phase for all films and picked out CTS phase for some samples prepared using Cu/SnS/Zn/Cu precursor films. The surface microstructure of the films that were obtained through SEM displayed polycrystalline surface structure. Room temperature PL emission spectra of the films showed broad peak at around 1.37-1.38 eV, which is near to the optical band gap of kesterite CZTS structure. Electrical characterization of the samples demonstrated that B-525 CZTS thin film has more suitable electrical resistivity and carrier concentration values for CZTS based solar cell applications.