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Single-Step Deposition of Chalcopyrite (CuFeS2) Thin Films
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  • Valmar da Silva Severiano Sobrinho
    Valmar da Silva Severiano Sobrinho
    Materials Science and Engineering Post-Graduation − Federal University of Campina Grande (UFCG), Campina Grande 58429-900, PB, Brazil
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  • Thercio Henrique de Carvalho Costa*
    Thercio Henrique de Carvalho Costa
    Mechanical Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
    *Email: [email protected]
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    Orcidhttps://orcid.org/0000-0001-7429-4273
  • Michelle Cequeira Feitor
    Michelle Cequeira Feitor
    Mechanical Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
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  • Maxwell Santana Libório
    Maxwell Santana Libório
    Science and Technology School − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
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  • Rômulo Ribeiro Magalhães de Sousa
    Rômulo Ribeiro Magalhães de Sousa
    Mechanical Department – Federal University of Piauí (UFPI), Teresina 64049-550, PI, Brazil
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  • Álvaro Albueno da Silva Linhares
    Álvaro Albueno da Silva Linhares
    Mechanical Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
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  • Pâmala Samara Vieira
    Pâmala Samara Vieira
    Materials Science and Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
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    Orcidhttps://orcid.org/0009-0009-6365-2691
  • Luciano Lucas Fernandes Lima
    Luciano Lucas Fernandes Lima
    Materials Science and Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
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  • Cleânio da Luz Lima
    Cleânio da Luz Lima
    Physic Post-Graduation − Federal University of Piauí (UFPI), Teresina 64049-550, PI, Brazil
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    Orcidhttps://orcid.org/0000-0003-3958-7008
  • Edcleide Maria Araújo
    Edcleide Maria Araújo
    Materials Science and Engineering Post-Graduation − Federal University of Campina Grande (UFCG), Campina Grande 58429-900, PB, Brazil
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ACS Omega

Cite this: ACS Omega 2024, 9, 50, 49849–49856
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https://doi.org/10.1021/acsomega.4c08647
Published December 4, 2024

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Abstract

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Thin films of chalcopyrite, CuFeS2, are promising candidates for use as absorber layers in photovoltaic cells due to their low band gap and high absorbance. These films are typically deposited in two or three steps, always involving an annealing process. In this work, the CuFeS2 film was deposited on a glass substrate in a single deposition step using the cathodic cylindrical plasma deposition (CCyPD) technique. The film samples deposited were analyzed by X-ray diffraction (XRD) and Raman spectroscopy, the film thickness was measured using the optical method, and FEG-SEM analyzed the surface structural morphology. The results showed a strong dependence on the deposition temperature for phase formation, with chalcopyrite being obtained for films deposited at 600 °C. At this temperature, a uniformly distributed film with uniform grain sizes was obtained, and the experimentally obtained band gap values of the films were consistent with the theoretical values reported in the literature, demonstrating the technique’s effectiveness and precision in producing high-quality films.

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Introduction

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Chalcopyrite is theoretically and experimentally studied as a promising material for electronic applications, such as light-emitting diodes, photocatalytic cells, and nonlinear optical devices. Among chalcopyrites, those of the ABX2 type (A = Cu, Al, Ag, Nb, Na; B = Cr, Al, Fe, B, In, Ga; X = S, Se, Te) have gained prominence due to their high stability and good electronic properties. (1−8)
Thin chalcopyrite films derived from Se, In, and Te possess good thermoelectric properties. Still, they are derived from toxic or rare materials, making sulfide-based chalcopyrites a more cost-effective option for energy applications. Among these, CuFeS2, which has a band gap of approximately 0.50 eV and a high absorption coefficient, is promising for use as an absorber layer in photovoltaic cells. (9−12)
Such films have already been successfully produced in the literature using two- and three-step processes. CuAl(SeTe)2 chalcopyrite films were produced by vacuum evaporation in Al/Cu/(SeTe) multilayers, followed by high-temperature annealing for the formation and crystallization of CuAl(SeTe)2. (13−17)
Several thin films of selenium- and sulfur-based chalcopyrite, such as Cu(InGaAlFe)(SeS)2, were deposited by evaporating successive layers of Cu/(InGaAlFe)/Cu··· (InGaAlFe)/Cu, with substrates kept at high temperatures, undergoing selenization or sulfurization processes in a Se- or S-rich atmosphere, followed by annealing, ultimately forming the desired chalcopyrite thin film. (18−27)
The cage cathodic cylinder deposition (CCyPD) method was described by de Medeiros Neto et al. (28) This work offers a solution for obtaining chalcopyrite in a single deposition step. This work aimed to deposit a CuFeS2 chalcopyrite thin film in a single step using the CCyPD method. The influence of temperature on the formation of the desired phase was evaluated, and the films’ optical, electrical, and structural properties were studied.

Materials and Methods

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The raw materials used for the production of chalcopyrite films were iron powder (99.5%), copper (98%), and sulfur (99.5%). The films were deposited on soda-lime glass microscope slides with a rectangular geometry, transparent, and free of surface imperfections, measuring 26 mm × 76 mm with 1.0 and 1.2 mm thickness. The samples underwent a preparation process to reduce surface impurities and effectively prepare them for film deposition. They were washed with neutral detergent and then cleaned in an ultrasonic bath with acetone, ethanol, and deionized water for 30 min. Finally, the samples were dried with a nitrogen jet, as described by Sousa and da Cunha. (29)
The Fe, Cu, and S powders were weighed in the proportions of 30.5% Fe, 34.5% Cu, and 35.0% S, the natural proportions of chalcopyrite, (30) and ground in a Pulverisette 6 (Fritsch) high-energy planetary mill for 20 h with a ratio of 3 g of grinding media for every 1 g of powder and a rotation speed of 400 rpm, using alcohol as a lubricant for better microstructural homogenization. (23) After milling, the powder was placed in a drying and sterilization oven for 24 h at 70 °C. The resulting powder from this process was pressed with a load of 2 tons for 1 min to form the cathodic cylinders, which were then sintered in a plasma reactor for 2 h at 400 °C under a vacuum of 2 mbar and a controlled atmosphere of 8 sccm of Ar and 2 sccm of H2.
The produced cylinders were used for film deposition using the cathodic cylinder plasma deposition (CCyPD) technique described by de Medeiros Neto et al. (28) This technique utilizes the same vacuum and atmosphere conditions used for sintering, varying the temperature at 450, 500, and 600 °C. The study included premixed powder after 20 h of milling, powder after sintering, and films deposited on glass. The deposition parameters are summarized in Table 1.
Table 1. Deposition Parameters
parameters
working pressure [mBar]2
deposition time [h]6
argon flow [sccm]8
hydrogen flow [sccm]2
temperature [°C]450, 500, and 600
The X-ray diffraction (XRD) analysis was performed using a Shimadzu XRD-7000 high-resolution diffractometer with copper Kα radiation, operating at 40 kV and 30 mA, with a grazing incidence of 3°, and a step size of 0.02° every 0.5 s. For the interpretation of the XRD data, relevant literature articles were consulted, and the crystallographic databases JCPDS (Joint Committee on Powder Diffraction Standards), ICDD (International Center for Diffraction Data), ICOD (International Crystallography Open Database), and ICCD (International Center for Crystallographic Data) were utilized.
Raman scattering was conducted using the Lab-RAM HR Evolution system (HORIBA Scientific) with 16 mW, a wavelength of 532 nm, a 10% power filter, an acquisition time of 10 s, and an accumulation of 10 measurements over a spectral range of 100–1000 cm–1. Transmittance was measured with a GENESYSTM 10S UV–vis spectrophotometer from THERMO FISHER SCIENTIFIC across a spectral range between 190 and 1100 nm with a scanning speed of 2.0 nm/s. Top morphological images of the deposited films were obtained by using a Zeiss Auriga 40 FEG-SEM, with a filament voltage of 5 kV and a working distance of 5.0 mm. The thickness of the films was calculated from transmittance data using the Pointwise Unconstrained Minimization Approach (PUMA) method. (31) The band gap of the films was calculated using the Tauc linear extrapolation method. (32)

Results and Discussion

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A comparative study was initially conducted on the pure Cu, Fe, and S powders acquired, and the powder was manually mixed in the proportions indicated in the Materials and Methods section. X-ray Diffraction analysis was performed to characterize the material to be deposited, with the results presented in Figure 1. It is possible to observe the presence of S, Fe, and Cu in the mixture and a small amount of iron oxide already present in the Fe powder due to exposure to the atmosphere. However, the oxide proportion in the mixture is so low that the characteristic peaks are not noticeable. A prominent presence of sulfur is noted, with a main peak for the (222) plane at 2θ of 23.15° (COD 96-901-1363). Subsequently, the powder underwent 20 h high-energy milling and a sintering process. Figure 2 shows the comparative X-ray diffraction (XRD) of the powder after milling and after sintering.

Figure 1

Figure 1. Pure Cu, Fe, and S powders and a manually mixed Cu–Fe–S mixture.

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Figure 2

Figure 2. Cu–Fe–S powder after 20 h of milling in a high-energy ball mill.

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According to Suryanarayana, (33) during high-energy milling, powder particles are repeatedly flattened, cold-welded, fractured, and then welded again. The newly created surfaces allow particles to bond together; some energy is lost as heat, and a small portion is dissipated during the elastic and plastic deformations of the constituents. The severe deformation introduced into the particles results in various defects, such as dislocations, vacancies, stacking faults, and an increased number of grain boundaries, which enhance diffusivity in the material. Additionally, a slight increase in the temperature further aids the diffusion behavior, leading to the bonding of the constituent elements.
For the powder mixed in the high-energy mill, as shown in Figure 2, there is a noticeable decrease in the central sulfur peak and the disappearance of several of its crystallographic orientations compared to those of the manually mixed powder (Figure 1). Part of the sulfur combines with Cu and Fe, forming copper(II) sulfide (CuS) and iron disulfide (FeS2). According to Riyaz, Parveen, and Azam, (34) the formation of CuS can be identified by the appearance of diffraction peaks for the (102), (103), (006), (110), (114), and (203) planes, which characterize the hexagonal structure of CuS (JCPDS No. 78-0876). Yuan et al. (35) state that for iron disulfide (FeS2), the characteristic (stronger) diffraction peak for the (200) plane and weaker peaks for the (210) and (311) planes are observed, consistent with the standard card (JCPDS No. 42-1340). The most notable presence of iron with a characteristic peak for the (110) plane, consistent with the standard card (ICOD No. 01-089-7194), is observed in the milled powder. The probably decreased prominence of sulfur peaks provided a greater emphasis on this element in the analysis.
The absence of pure sulfur in the sintered powder was noted, which promoted an improvement during the deposition process.
The intermetallic compounds FeS, FeS2, and CuS, having higher dissociation and melting temperatures than those of pure sulfur, are expected to prevent sulfur evaporation, leading to a stable plasma deposition process with fewer arc openings.
In addition to the crystallographic planes mentioned previously, the formation of iron sulfide (FeS) is observed. It is characterized by a more intense peak for the (102) plane at 2θ of 43.2° and characteristic peaks for the (100), (101), (110), and (004) planes, all consistent with its standard card (ICOD 03-065-0408).
Iron disulfide requires less energy for formation, having a lower Gibbs free energy, meaning it occurs more spontaneously. Additionally, environments with higher oxygen presence favor the formation of disulfide, while environments with less oxygen or more reducing conditions promote the formation of iron sulfide. (36) This could explain the presence of disulfide as a result of the milling process in an uncontrolled atmosphere, while sulfide appears in a reducing atmosphere and a low pressure.
Finally, in Figure 2, a comparison of the XRD patterns of the powder after 20 h of milling with the result after sintering shows the absence of pure sulfur and greater crystallinity of the material after the sintering process, with sharper and well-defined high-intensity peaks, indicating regularly and repetitively arranged atoms, which reflect X-rays more efficiently.
Figure 3 illustrates the XRD results of the deposited films. According to Khalid et al., (37) in the sample deposited at 600 °C, peaks corresponding to chalcopyrite can be observed, as per ICDD No. 01-083-0984. The characteristic peak of FeS is also noticeable in all three samples, following the standard card (ICOD 03-065-0408).

Figure 3

Figure 3. XRD of the films deposited on glass at the three temperatures.

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As noted by Gao et al., (38) the formation of FeS2 can be observed for the (211) plane, consistent with the standard card (JCPDS 65-7643). For the film heated to 600 °C, the presence of the (201) plane is also noted. According to Bakr, Kamil, and Jabbar, (39) the presence of CuS, characterized by the peak at 2θ of 47.8°, is observed, which agrees with its standard card (ICCD 06-0464) and is noted for deposition temperatures of 450 and 500 °C.
Nafees, Ikram, and Ali (40) observed that at approximately 600 °C, copper(II) sulfide (CuS) undergoes dissociation, resulting in the formation of copper(I) sulfide (Cu2S) and, in oxidative atmospheres, copper oxides. The same study also found that in reducing atmospheres the formation of these oxides is significantly inhibited. Krylova, Dukštienė, and Prosyčeva (41) identified the presence of Cu2S based on the characteristic peak at 2θ, observed at approximately 34°, in accordance with the standard card (JCPDS #33-490).
We can conclude that Cu, Fe, and S constituent phases are present under all three deposition conditions, but only at 600 °C was chalcopyrite of the CuFeS2 type found.
In Figure 4, we observe the presence of FeS and FeS2 at all deposition temperatures. According to Anthony et al. and Keller-Besrest and Collin, (42,43) the region of vibrations highlights the presence of FeS near 700 cm–1 (RRUFF database at http://rruff.info/ (2024): Troilite, FeS (RRUFFID: R070242)).

Figure 4

Figure 4. Raman spectra obtained from the three deposition temperature conditions: 450, 500, and 600 °C.

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According to Klimm and Botcharnikov, (44) the presence of pyrite FeS2 can be noted by the disturbance near 550 cm–1 (RRUFF database at http://rruff.info/ (2024): Pyrite, FeS2 (RRUFFID: R070692)).
The Raman peak near 471 cm–1 corresponds to a vibration mode of CuS associated with the S–S stretching mode of S2 ions, indicating that Raman spectroscopy can distinguish between copper sulfides with and without S–S bonding. For this sulfide, the disturbances in lower frequency regions (below 322 cm–1 highlighted in the graph) can be attributed to the Cu2–xS (0.6 ≤ x ≤ 1) phonon mode, with the method being susceptible to the presence of this defect phase. (45,46)
According to the Raman analysis results of Jiang et al. (47) and Minceva-Sukarova et al., (48) the region around 200 cm–1 is associated with the presence of Cu2S, which appears in the film deposited at 600 °C, in agreement with the XRD results.
Wang et al. (49) state that CuFeS2 chalcopyrite has a crystal symmetry that can be decomposed into 15 vibrational modes. Among them, the mode around 300 cm–1, highlighted in Figure 4, corresponds to the nonpolar active mode with higher vibrational intensity than any other of its modes. This mode is associated with anion pairs, while the others are associated with anions and cations.
Then, films containing CuFeS2, FeS2, and Cu2S phases were obtained, all of which are of interest for applications in solar cells. (50−53) However, eliminating high-purity films with secondary phases may be required for direct applications as the active layer in photovoltaic devices. Various theoretical approaches suggest effective methods, such as chemical etching, commonly used in CZTS and CIGS films. (54−56) Furthermore, studies demonstrate that annealing, with optimized thermal treatment parameters, can eliminate unwanted phases, as exemplified by the formation of high-purity CIGSSe films without selenization. (57) These results indicate that future investigations focused on controlling secondary phases through thermal treatment or chemical methods are promising for optimizing the properties of chalcopyrite films.
Figure 5 shows the SEM images for the three deposition conditions. It is observed that for the sample deposited at 450 °C, the grains are in the nanometer scale, as indicated by the lack of resolution for grain size calculation, with low contrast that prevents complete distinction, showing only nucleation regions and low coalescence, which indicates a nonuniform film. High coalescence during film formation is observed for the films deposited at 500 and 600 °C, with micrometer-scale grains in both films.

Figure 5

Figure 5. SEM-FEG for samples (A) deposited at 450 °C, (B) 500 °C, and (C) 600 °C.

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Figure 5 also shows the grain size distribution for the samples deposited at 500 and 600 °C, obtained from SEM surface analysis using ImageJ software. Figure 5B displays a greater dispersion in grain length values, characterized by a smoother Gaussian distribution and an average grain size of 0.86 ± 0.28 μm. Figure 5C, for the sample deposited at 600 °C, presents more concentrated grain length values around 0.39 μm, with the Gaussian body indicating more homogeneous grain sizes. We can conclude that the film deposited at 600 °C is more uniformly distributed with a higher grain density.
Figure 6 compares the actual (measured) transmittance to that obtained using the PUMA method within the wavelength range the algorithm covers.

Figure 6

Figure 6. Comparison between experimental and calculated transmittances for all deposition conditions.

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The curves calculated by using the optical constants and thickness closely match the experimental curves. The quadratic error between the transmittance curve and the calculated curve is of a low order of magnitude for all deposition conditions, as seen in Table 2.
Table 2. Quadratic Error of the Difference between the Calculated Transmittance and Actual Curves for All of the Analyzed Samples
sample450 °C500 °C600 °C
quadratic error5.33 × 10–53.94 × 10–57.66 × 10–5
The film thicknesses obtained from the optical method can be seen in Table 3. It is noted, according to Bittencourt, (58) that with an increase in temperature, there is a higher ionization rate in the plasma and, consequently, a higher deposition rate, leading to an increase in film thickness.
Table 3. Thickness of the Deposited Films
samplesthickness (nm)
450 °C51
500 °C124
600 °C218
The thickness of the films deposited at 450 °C is lower than those deposited at 500 °C, which is related to the decrease in the transmittance of these films. However, this correlation does not apply to the films deposited at 600 °C, as they consist of different materials. X-ray diffraction (XRD) and Raman spectroscopy analyses indicated the presence of FeS and FeS2 phases in all three films. However, in the films deposited at 450 and 500 °C, CuS phases were identified, while in the films deposited at 600 °C, these phases were replaced by Cu2S and CuFeS2.
Transmittance is a function of optical parameters, including the wavelength of the incident radiation (λ), the refractive index of the substrate (s), the film thickness (d), the refractive index of the film (n), and the absorption coefficient of the film (k), according to the relation T = T(λ, s(λ), d, n(λ), k(λ)). (31) Therefore, it is not possible to directly compare the transmittances of films with different phases by considering only the thickness as a parameter.
In the films deposited at temperatures of 450 and 500 °C, no CuFeS2 chalcopyrite formation is observed; instead, only phases with Cu, Fe, and S are present. Despite being good conductors, they have direct band gaps of 2.23 and 1.80 eV for the deposition temperatures of 450 and 500 °C, respectively. This behavior can be seen in the results presented in Figure 7a.

Figure 7

Figure 7. Band gap of the films deposited at 450 and 500 °C temperatures. (a) values for direct transition; (b) values for indirect transition.

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In Figure 7b, we obtain negative results when mathematically determining the band gap values for an indirect transition, indicating that this type of transition does not exist in these films.
Figure 8 shows that the lowest band gap result for the indirect transition was obtained for deposition at 600 °C.

Figure 8

Figure 8. Indirect band gap obtained from CuFeS2 films deposited at 600 °C for (a) direct and (b) indirect transition.

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The difference in band gap between the films shown in Figures 7 and 8 is because CuFeS2-type chalcopyrite has an indirect transition, with an intermediate band formed by the empty 3d orbitals of Fe. The band gap values obtained for this material are consistent with the literature; as for CuFeS2, the conduction band edge is separated from the bottom of the intermediate band by an indirect gap of approximately 0.50 eV. (9)

Conclusions

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In this study, the deposition of phase CuFeS2 chalcopyrite films on glass substrates was carried out by using a single deposition step through the CCyPD method. The results of this work allow us to conclude that
1.

Structural studies using X-ray diffraction (XRD) and Raman spectroscopy identified the presence of CuFeS2 in films deposited at 600 °C, demonstrating a strong dependence between phase formation and deposition temperature.

2.

The long milling process and sintering of the cylinders contribute to more stable deposition due to the higher dissociation temperature of the formed phases.

3.

The CCyPD technique proves promising for thin film deposition, including chalcopyrites, which can be achieved in a single deposition step.

4.

The experimentally obtained band gap values of the films agree with the theoretical values calculated and reported in the literature. This highlights the effectiveness and precision of the technique in producing high-quality films.

Author Information

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  • Corresponding Author
  • Authors
    • Valmar da Silva Severiano Sobrinho - Materials Science and Engineering Post-Graduation − Federal University of Campina Grande (UFCG), Campina Grande 58429-900, PB, Brazil
    • Michelle Cequeira Feitor - Mechanical Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
    • Maxwell Santana Libório - Science and Technology School − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
    • Rômulo Ribeiro Magalhães de Sousa - Mechanical Department – Federal University of Piauí (UFPI), Teresina 64049-550, PI, Brazil
    • Álvaro Albueno da Silva Linhares - Mechanical Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
    • Pâmala Samara Vieira - Materials Science and Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil;  Orcidhttps://orcid.org/0009-0009-6365-2691
    • Luciano Lucas Fernandes Lima - Materials Science and Engineering Post-Graduation − Federal University of Rio Grande do Norte (UFRN), Natal 59078-970, RN, Brazil
    • Cleânio da Luz Lima - Physic Post-Graduation − Federal University of Piauí (UFPI), Teresina 64049-550, PI, Brazil;  Orcidhttps://orcid.org/0000-0003-3958-7008
    • Edcleide Maria Araújo - Materials Science and Engineering Post-Graduation − Federal University of Campina Grande (UFCG), Campina Grande 58429-900, PB, Brazil
  • Funding

    The Article Processing Charge for the publication of this research was funded by the Coordination for the Improvement of Higher Education Personnel - CAPES (ROR identifier: 00x0ma614).

  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de nível superior─Brazil (CAPES)─Finance Code 001. The National Council for Scientific and Technological Development─CNPq and FAPERN Process N. 10959064-720.000038/2022-89.

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    Wang, K.; Qin, P.; Ge, Z.-H.; Feng, J. Highly Enhanced Thermoelectric Properties of P-Type CuInSe2 Alloys by the Vacancy Doping. Scr. Mater. 2018, 149, 88– 92,  DOI: 10.1016/j.scriptamat.2018.02.023
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    Hassan, N.-A.; Jaf, Z. N.; Salman, S. H.; Khudayer, I. H.; Ibrahem, H.; Miran, H. A. Influence of In-Dopant on the Optoelectronic Properties of Thermal Evaporated CuAlTe2 Films. Solid State Commun. 2023, 371, 115260  DOI: 10.1016/j.ssc.2023.115260
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    Korzun, B. V.; Fadzeyeva, A. A.; Mudryi, A. V.; Schorr, S. Optical Absorption and Photoluminescence of CuAlTe2. Phys. Status Solidi C 2006, 3 (8), 2626– 2629,  DOI: 10.1002/pssc.200669543
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    Marsillac, S.; Wahiba, T. B.; El Moctar, C.; Bernede, J. C.; Khelil, A. Evolution of the Properties of CuAlSe2 Thin Films with the Oxygen Content. Sol. Energy Mater. Sol. Cells 2002, 71 (4), 425– 434,  DOI: 10.1016/S0927-0248(01)00097-6
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    Arnou, P.; Lomuscio, A.; Weiss, T. P.; Siopa, D.; Giraldo, S.; Saucedo, E.; Scarpulla, M. A.; Dale, P. J. Continuous-Wave Laser Annealing of Metallic Layers for CuInSe 2 Solar Cell Applications: Effect of Preheating Treatment on Grain Growth. RSC Adv. 2020, 10 (1), 584– 594,  DOI: 10.1039/C9RA06896A
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    Barkat, L.; Hamdadou, N.; Morsli, M.; Khelil, A.; Bernede, J. C. Growth and Characterization of CuFeS2 Thin Films. J. Cryst. Growth 2006, 297 (2), 426– 431,  DOI: 10.1016/j.jcrysgro.2006.10.105
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    Growth and characterization of CuFeS2 thin films
    Barkat, L.; Hamdadou, N.; Morsli, M.; Khelil, A.; Bernede, J. C.
    Journal of Crystal Growth (2006), 297 (2), 426-431CODEN: JCRGAE; ISSN:0022-0248. (Elsevier B.V.)
    CuFeS2 thin films, were grown by sulfurization of CuFe alloy precursor. Cu/Fe.../Cu thin layers were sequentially deposited by vacuum evapn. on a substrate heated at a temp. Ts = 723 K. After deposition of the metal alloy precursor, there is an interdiffusion of the metals all along the thickness. The relative thicknesses of the layers deposited achieve the desired at. ratio Cu/Fe: 2.5. These precursors are sulfured in a vacuum chamber using an S source. The sulfurization duration is 20 min. At the end of the process, the film exhibits a (112) preferential orientation. Thus, the structure of the film is the expected tetragonal structure of CuFeS2. The XPS study shows that there is no O contamination of the film, except the surface because it was exposed to air. The compn. measured is in good agreement with that measured by electron microprobe anal.
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    Cao, H.; Deng, H.; Zhou, W.; Tao, J.; Chen, L.; Huang, L.; Sun, L.; Yue, F.; Yang, P.; Chu, J. Investigation of Microstructural and Optical Properties of Cu (In, Al) Se2 Thin Films with Various Copper Content. J. Alloys Compd. 2015, 651, 208– 213,  DOI: 10.1016/j.jallcom.2015.08.148
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    Goushi, Y.; Hakuma, H.; Tabuchi, K.; Kijima, S.; Kushiya, K. Fabrication of Pentanary Cu (InGa)(SeS) 2 Absorbers by Selenization and Sulfurization. Sol. Energy Mater. Sol. Cells 2009, 93 (8), 1318– 1320,  DOI: 10.1016/j.solmat.2009.02.004
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    López-García, J.; Montero, J.; Maffiotte, C.; Guillén, C.; Herrero, J. Crystallization of Wide-Bandgap CuAlSe2 Thin Films Deposited on Antimony Doped Tin Oxide Substrates. J. Alloys Compd. 2015, 648, 104– 110,  DOI: 10.1016/j.jallcom.2015.05.196
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    Malagutti, M. A.; Lohani, K.; D’Incau, M.; Nautiyal, H.; Ataollahi, N.; Scardi, P. Optimizing CuFeS2 Chalcopyrite Thin Film Synthesis: A Comprehensive Three-Step Approach Using Ball-Milling, Thermal Evaporation, and Sulfurization Applied for Thermoelectric Generation. Appl. Sci. 2023, 13 (18), 10172,  DOI: 10.3390/app131810172
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    Marsillac, S.; Bernede, J. C.; El Moctar, C.; Pouzet, J. Physico-Chemical Characterization of CuAlSe2 Films Obtained by Reaction, Induced by Annealing, between Se Vapour and Al/Cu/AI···Cu/Al/Cu Thin Films Sequentially Deposited. Mater. Sci. Eng. B 1997, 45 (1–3), 69– 75,  DOI: 10.1016/S0921-5107(96)02031-4
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    Zeng, L.; Zhang, L.; Liang, Y.; Zeng, C.; Qiu, Z.; Lin, H.; Hong, R. Growth-Promoting Mechanism of Bismuth-Doped Cu (In, Ga) Se2 Solar Cells Fabricated at 400° C. ACS Appl. Mater. Interfaces 2022, 14 (20), 23426– 23435,  DOI: 10.1021/acsami.2c03228
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    Growth-Promoting Mechanism of Bismuth-Doped Cu(In,Ga)Se2 Solar Cells Fabricated at 400 °C
    Zeng, Longlong; Zhang, Linquan; Liang, Yunfeng; Zeng, Chunhong; Qiu, Zeyu; Lin, Haofeng; Hong, Ruijiang
    ACS Applied Materials & Interfaces (2022), 14 (20), 23426-23435CODEN: AAMICK; ISSN:1944-8244. (American Chemical Society)
    The classical high-temp. synthesis process of Cu(In,Ga)Se2 (CIGS) solar cells limits their applications on high-temp. intolerant substrates. In this study, a novel low-temp. (400 °C) fabrication strategy of CIGS solar cells is reported using the bismuth (Bi)-doping method, and its growth-promoting mechanism is systematically studied. Different concns. of Bi are incorporated into pure chalcopyrite quaternary target sputtered-CIGS films by controlling the thickness of the Bi layer. Bi induces considerable grain growth improvement, and an av. of approx. 3% abs. efficiency enhancement is achieved for Bi-doped solar cells in comparison with the Bi-free samples. Solar cells doped with a 50 nm Bi layer yield the highest efficiency of 13.04% (without any antireflective coating) using the low-temp. technol. The copper-bismuth-selenium compds. (Cu-Bi-Se, mainly Cu1.6Bi4.8Se8) are crucial in improving the crystallinity of absorbers during the annealing process. These Bi-contg. compds. are conclusively obsd. at the grain boundaries and top and bottom interfaces of CIGS films. The growth promotion is found to be assocd. with the superior diffusion capacity of Cu-Bi-Se compds. in CIGS films, and these liq. compds. function as carriers to facilitate crystn. Bi atoms do not enter the CIGS lattices, and the band gaps (Eg) of absorbers remain unchanged. Bi doping reduces the no. of CIGS grain boundaries and increases the copper vacancy content in CIGS films, thereby boosting the carrier concns. Cu-Bi-Se compds. in grain boundaries significantly enhance the cond. of grain boundaries and serve as channels for carrier transport. The valence band, Fermi energy level (EF), and conduction band of Bi-doped CIGS films all move downward. This band shift strengthens the band bending of the CdS/CIGS heterojunction and eventually improves the open circuit voltage (Voc) of solar cells. An effective doping method and a novel mechanism can facilitate the low-temp. prepn. of CIGS solar cells.
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    Zhang, Q.; Deng, H.; Yu, J.; Cao, H.; Chen, L.; Tao, J.; Zheng, X.; Yang, P.; Sun, L.; Chu, J. Effects of Bismuth-Doping on the Properties of Cu (In, Al) Se2 Thin Films Prepared by Selenization of Sputtered Stacked Precursors. Mater. Lett. 2018, 213, 19– 22,  DOI: 10.1016/j.matlet.2017.11.004
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    Zhang, Q.; Deng, H.; Yu, J.; Tao, J.; Sun, L.; Yang, P.; Chu, J. Grain Growth Enhancing through Preheating Treatment of a Sputtered Stacked Metallic Precursor for Cu (In, Al) Se2 Thin Film Solar Cells Application. Mater. Sci. Eng. B 2019, 242, 31– 36,  DOI: 10.1016/j.mseb.2019.03.008
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    de Medeiros Neto, J. f.; Lima, L. L. F.; Vieira, P. S.; da Costa, B. T.; Libório, M. S.; de Queiroz, J. C. A.; de Medeiros Aires, M.; Nascimento, I. O.; de Souza, I. A.; Feitor, M. C. Plasma Deposition from Cathodic Cylinders: A Technology for Reduction of Metallic Oxides and Deposition of Wear-Resistant Films. Surf. Coat. Technol. 2024, 488, 131027  DOI: 10.1016/j.surfcoat.2024.131027
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    Sousa, M. G.; da Cunha, A. F. High SnS Phase Purity Films Produced by Rapid Thermal Processing of RF-Magnetron Sputtered SnS2-x Precursors. Appl. Surf. Sci. 2019, 472, 64– 70,  DOI: 10.1016/j.apsusc.2018.04.118
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    High SnS phase purity films produced by rapid thermal processing of RF-magnetron sputtered SnS2-x precursors
    Sousa, M. G.; da Cunha, A. F.
    Applied Surface Science (2019), 472 (), 64-70CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)
    The work reported below aimed at establishing a suitable route to prep. single phase SnS thin films for photovoltaic applications. The growth approach consisted in the deposition of SnS2-x precursor layers by RF-magnetron sputtering followed by rapid thermal annealing. The samples were placed on a graphite susceptor covered with a transparent glass dome in an atm. of N2 + 5%H2S, with and without addnl. tin sulfide vapor in the atm. around the samples. The resulting films were studied by SEM, energy dispersive spectroscopy, X-ray diffraction, Raman scattering and spectrophotometry to det. which set of growth conditions yielded the desired properties. In order to minimize the material loss through evapn., improve the films' morphol. and eliminate the residual SnS2 phase, the use of a transparent glass dome to confine the tin sulfide vapor in a smaller vol. over the sample, is an effective approach. Clearly, the material loss was reduced. The samples grown on Mo at a low heating rate of 0.2 °C/s and 500 °C during 5 min showed good properties but still contained residues of the SnS2 phase. By increasing the heating rate to 2 °C/s and above, it was possible to eliminate the SnS2 phase and still maintain a good morphol., thus obtaining single phase SnS films deemed as essential for optimized photovoltaic performance.
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    Tauc, J.; Grigorovici, R.; Vancu, A. Optical Properties and Electronic Structure of Amorphous Germanium. Phys. Status Solidi B 1966, 15 (2), 627– 637,  DOI: 10.1002/pssb.19660150224
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    Optical properties and electronic structure of amorphous germanium
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    Physica Status Solidi (1966), 15 (2), 627-37CODEN: PHSSAK; ISSN:0031-8957.
    The optical consts. of amorphous Ge are detd. for photon energies 0.08-1.6 ev. From 0.08 to 0.5 ev., the absorption is due to k-conserving transitions of holes between the valence bands as in p-type crystals; the spin-orbit splitting is 0.20 and 0.21 ev. in nonannealed and annealed samples, resp. The effective masses of the holes in the 3 bands are 0.49 m (0.43 m), 0.04 m, and 0.08 m. An absorption band is observed below the main absorption edge (at 300°K. the max. of this band is at 0.86 ev.); the absorption in this band increases with increasing temp. This band is due to excitons bound to neutral acceptors, and these are presumably the same ones that play a decisive role in the transport properties, which are considered to be assocd. with vacancies. The absorption edge has the form ω2ε2 ∼ (ℏω - Eg)2 (Eg = 0.88 ev. at 300°K.). This suggests that the optical transitions conserve energy but not k vector, and that the ds. of states near the band extrema have the same energy dependence as in cryst. Ge. A simple theory describing this situation is proposed, and comparison of it with the exptl. results leads to an estimate of the localization of the conduction-band wave functions. 24 references.
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    Khalid, S.; Ahmed, E.; Malik, M. A.; Lewis, D. J.; Bakar, S. A.; Khan, Y.; O’Brien, P. Synthesis of Pyrite Thin Films and Transition Metal Doped Pyrite Thin Films by Aerosol-Assisted Chemical Vapour Deposition. New J. Chem. 2015, 39 (2), 1013– 1021,  DOI: 10.1039/C4NJ01461H
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    Synthesis of pyrite thin films and transition metal doped pyrite thin films by aerosol-assisted chemical vapor deposition
    Khalid, Sadia; Ahmed, Ejaz; Azad Malik, M.; Lewis, David J.; Abu Bakar, Shahzad; Khan, Yaqoob; O'Brien, Paul
    New Journal of Chemistry (2015), 39 (2), 1013-1021CODEN: NJCHE5; ISSN:1144-0546. (Royal Society of Chemistry)
    Diethyldithiocarbamato-metal complexes of the general formula [M(S2CN(Et)2)n] (M = Fe(III), Co(III), Ni(II), Cu(II), Zn(II) and n = 2, 3) have been synthesized and used as precursors for the deposition of iron pyrite (FeS2) and transition metal doped iron pyrite (MxFe1-xS2) thin films on glass and indium tin oxide (ITO) coated glass substrates by aerosol assisted chem. vapor deposition (AACVD). Thermogravimetric anal. (TGA) confirmed that all the five complexes decomp. into their corresponding metal sulfides. The iron complex [Fe(S2CNEt2)3] (1) deposited pure cubic pyrite (FeS2) films with granular crystallites at 350 °C, whereas at 450 °C pyrite and marcasite were deposited. MxFe1-xS2 (where M = Co, Ni, Cu, or Zn) films were deposited by varying the relative concn. of complexes [Fe(S2CNEt2)3] (1) and [Co(S2CNEt2)3] (2), [Ni(S2CNEt2)2] (3), [Cu(S2CNEt2)2] (4) and [Zn(S2CNEt2)2] (5) at 350 °C. The formation of a solid soln. was confirmed by powder X-ray diffraction (p-XRD). The surface morphol. of the films was studied by SEM (SEM) while the height profiles of the films were revealed by at. force microscopy (AFM). The elemental compns. of the films were confirmed by energy-dispersive X-ray (EDX) spectroscopy. To the best of our knowledge, these complexes are the first in their class to be used as single source precursors to deposit MxFe1-xS2 thin films.
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    Gao, Y.; Li, Z.; Fu, Z.; Zhang, H.; Wang, G.; Zhou, H. Highly Selective Capacitive Deionization of Copper Ions in FeS2@N, S Co-Doped Carbon Electrode from Wastewater. Sep. Purif. Technol. 2021, 262, 118336  DOI: 10.1016/j.seppur.2021.118336
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    Highly selective capacitive deionization of copper ions in FeS2@N, S co-doped carbon electrode from wastewater
    Gao, Yong; Li, Zhaolei; Fu, Zhen; Zhang, Haimin; Wang, Guozhong; Zhou, Hongjian
    Separation and Purification Technology (2021), 262 (), 118336CODEN: SPUTFP; ISSN:1383-5866. (Elsevier B.V.)
    Capacitive deionization (CDI) as a promising water treatment technique aroused great concern for selective electrosorption of heavy metal ions from complex wastewater. Here, for the first time, we developed FeS2@N, S co-doped carbon (FeS2@NSC) composites as a novel electrode material for high-efficiency selective electrosorption of Cu2+ ion under various cations coexistence system. On account of the synergistic effect of elec. double layers and pseudocapacitance of FeS2@NSC electrode, the superior electrosorption performance of 508.5 mg•g-1 and high coeff. of selectivity (Cu2+/Na+) of 71.6 at molar ratio of 1:10 for Cu2+ ion were achieved at 1.0 V. Significantly, the FeS2@NSC electrode had obvious Cu2+ ion selective electrosorption behavior in mixed ions environment including Cu2+, Pb2+, Cd2+, Zn2+, Co2+ and Mn2+ ions. Finally, the ex-situ XRD and XPS characterization demonstrated that the highly selective electrosorption of Cu2+ ion in FeS2@NSC was dominated by the Faradic redox reaction of the Fe2+/Fe3+ and Cu2+/Cu+ couples. The selective electrosorption performance of FeS2@NSC electrode was also confirmed by treatment of real copper-contg. electroplating wastewater.
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    Bakr, N.; Kamil, A.; Jabbar, M. Preparation and Study of Some Physical Properties of CuxZn1-xS Thin Films. J. Chem., Biol. Phys. Sci. 2018, 8, 077-088  DOI: 10.24214/jcbps.C.8.1.07788
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    Klimm, K.; Botcharnikov, R. E. The Determination of Sulfate and Sulfide Species in Hydrous Silicate Glasses Using Raman Spectroscopy. Am. Mineral. 2010, 95 (10), 1574– 1579,  DOI: 10.2138/am.2010.3590
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    Hurma, T.; Kose, S. XRD Raman Analysis and Optical Properties of CuS Nanostructured Film. Optik 2016, 127 (15), 6000– 6006,  DOI: 10.1016/j.ijleo.2016.04.019
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    XRD Raman analysis and optical properties of CuS nanostructured film
    Hurma, T.; Kose, S.
    Optik (Munich, Germany) (2016), 127 (15), 6000-6006CODEN: OTIKAJ; ISSN:0030-4026. (Elsevier GmbH)
    Raman spectroscopy and X-ray diffraction (XRD) methods were applied to det. the phase compn. and crystal quality of CuS nanostructured film grown by spray pyrolysis. The film has polycryst. structure with preferential growth along the (101) plane. The grain size for the film was found to be lower than 20 nm. The very sharp Raman peak around 470 cm-1 in the high frequency region was identified as the S-S stretching mode of S2 ions at the 4e sites. Other Raman peaks were around 266 cm-1, 118 cm-1 and 68 cm-1 in the low frequency region due to CuS phase. Particles of nanometric size show low wavenumber vibrational modes that can be obsd. by Raman spectroscopy. Optical properties were obtained from UV-vis absorption, transmittance and reflectance spectra of the nanostructured CuS film. The optical consts. of the film such as refractive index, extinction coeff. and, optical cond. were investigated. The film was found to be p-type by using hot probe method.
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    Yeryukov, N. A.; Milekhin, A. G.; Sveshnikova, L. L.; Duda, T. A.; Pokrovsky, L. D.; Gutakovskii, A. K.; Batsanov, S. A.; Rodyakina, E. E.; Latyshev, A. V.; Zahn, D. R. T. Synthesis and Characterization of Cu x S (X = 1–2) Nanocrystals Formed by the Langmuir–Blodgett Technique. J. Phys. Chem. C 2014, 118 (40), 23409– 23414,  DOI: 10.1021/jp507355t
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    Synthesis and Characterization of CuxS (x = 1-2) Nanocrystals Formed by the Langmuir-Blodgett Technique
    Yeryukov, Nikolay A.; Milekhin, Alexander G.; Sveshnikova, Larisa L.; Duda, Tatyana A.; Pokrovsky, Lev D.; Gutakovskii, Anton K.; Batsanov, Stepan A.; Rodyakina, Ekaterina E.; Latyshev, Alexander V.; Zahn, Dietrich R. T.
    Journal of Physical Chemistry C (2014), 118 (40), 23409-23414CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
    The results on the investigation of structural and vibrational properties of CuxS (x = 1-2) nanocrystals formed using the Langmuir-Blodgett technique are reported. The synthesis requires deposition of high quality Langmuir-Blodgett films of copper behenates on a solid substrate (Si, Au, and Pt). The Langmuir-Blodgett film is then sulfidized, which results in the formation of the copper sulfide nanocrystals embedded in behenic acid matrix. Finally, free-standing CuxS nanocrystals are obtained after temp. annealing at 120-400°C in an Ar atm. Morphol. (size, shape, and areal d.) and the crystal structure of nanocrystals were detd. by direct structural methods, including scanning and transmission electron microscopies and high-energy electron diffraction. Surface-enhanced Raman scattering (SERS) by optical phonons in CuxS nanocrystals in the vicinity of metal nanoclusters provided a significant enhancement factor (about 25) and allowed the fine structure of their phonon spectrum to be obsd. SERS spectra of CuxS nanocrystals under annealing reveal the high frequency shift of optical phonon modes from 475 to 492 cm-1, which is explained by the existence of minor copper-deficient crystal phases. The combination of surface-enhanced Raman scattering spectroscopy, electron diffraction, and electron transmission microscopy allowed the authors to establish at least three stable phases: CuS, Cu1.8S, and Cu2S.
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    Jiang, Y.; Xu, Y.; Zhang, Q.; Zhao, X.; Xiao, F.; Wang, X.; Ma, G. Templated Synthesis of Cu2S Hollow Structures for Highly Active Ozone Decomposition. Catalysts 2024, 14 (2), 153,  DOI: 10.3390/catal14020153
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  • Abstract

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    Figure 1

    Figure 1. Pure Cu, Fe, and S powders and a manually mixed Cu–Fe–S mixture.

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    Figure 2

    Figure 2. Cu–Fe–S powder after 20 h of milling in a high-energy ball mill.

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    Figure 3

    Figure 3. XRD of the films deposited on glass at the three temperatures.

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    Figure 4

    Figure 4. Raman spectra obtained from the three deposition temperature conditions: 450, 500, and 600 °C.

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    Figure 5

    Figure 5. SEM-FEG for samples (A) deposited at 450 °C, (B) 500 °C, and (C) 600 °C.

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    Figure 6

    Figure 6. Comparison between experimental and calculated transmittances for all deposition conditions.

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    Figure 7

    Figure 7. Band gap of the films deposited at 450 and 500 °C temperatures. (a) values for direct transition; (b) values for indirect transition.

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    Figure 8

    Figure 8. Indirect band gap obtained from CuFeS2 films deposited at 600 °C for (a) direct and (b) indirect transition.

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  • References

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      Growth-Promoting Mechanism of Bismuth-Doped Cu(In,Ga)Se2 Solar Cells Fabricated at 400 °C
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      Sousa, M. G.; da Cunha, A. F.
      Applied Surface Science (2019), 472 (), 64-70CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)
      The work reported below aimed at establishing a suitable route to prep. single phase SnS thin films for photovoltaic applications. The growth approach consisted in the deposition of SnS2-x precursor layers by RF-magnetron sputtering followed by rapid thermal annealing. The samples were placed on a graphite susceptor covered with a transparent glass dome in an atm. of N2 + 5%H2S, with and without addnl. tin sulfide vapor in the atm. around the samples. The resulting films were studied by SEM, energy dispersive spectroscopy, X-ray diffraction, Raman scattering and spectrophotometry to det. which set of growth conditions yielded the desired properties. In order to minimize the material loss through evapn., improve the films' morphol. and eliminate the residual SnS2 phase, the use of a transparent glass dome to confine the tin sulfide vapor in a smaller vol. over the sample, is an effective approach. Clearly, the material loss was reduced. The samples grown on Mo at a low heating rate of 0.2 °C/s and 500 °C during 5 min showed good properties but still contained residues of the SnS2 phase. By increasing the heating rate to 2 °C/s and above, it was possible to eliminate the SnS2 phase and still maintain a good morphol., thus obtaining single phase SnS films deemed as essential for optimized photovoltaic performance.
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    30. 30
      Haldar, S. K. Introduction to Mineralogy and Petrology, 2nd ed.; Elsevier, 2020; Vol. 1.
      There is no corresponding record for this reference.
    31. 31
      Birgin, E. G.; Chambouleyron, I.; Martınez, J. M. Estimation of the Optical Constants and the Thickness of Thin Films Using Unconstrained Optimization. J. Comput. Phys. 1999, 151 (2), 862– 880,  DOI: 10.1006/jcph.1999.6224
      There is no corresponding record for this reference.
    32. 32
      Tauc, J.; Grigorovici, R.; Vancu, A. Optical Properties and Electronic Structure of Amorphous Germanium. Phys. Status Solidi B 1966, 15 (2), 627– 637,  DOI: 10.1002/pssb.19660150224
      32
      Optical properties and electronic structure of amorphous germanium
      Tauc, J.; Grigorovici, R.; Vancu, A.
      Physica Status Solidi (1966), 15 (2), 627-37CODEN: PHSSAK; ISSN:0031-8957.
      The optical consts. of amorphous Ge are detd. for photon energies 0.08-1.6 ev. From 0.08 to 0.5 ev., the absorption is due to k-conserving transitions of holes between the valence bands as in p-type crystals; the spin-orbit splitting is 0.20 and 0.21 ev. in nonannealed and annealed samples, resp. The effective masses of the holes in the 3 bands are 0.49 m (0.43 m), 0.04 m, and 0.08 m. An absorption band is observed below the main absorption edge (at 300°K. the max. of this band is at 0.86 ev.); the absorption in this band increases with increasing temp. This band is due to excitons bound to neutral acceptors, and these are presumably the same ones that play a decisive role in the transport properties, which are considered to be assocd. with vacancies. The absorption edge has the form ω2ε2 ∼ (ℏω - Eg)2 (Eg = 0.88 ev. at 300°K.). This suggests that the optical transitions conserve energy but not k vector, and that the ds. of states near the band extrema have the same energy dependence as in cryst. Ge. A simple theory describing this situation is proposed, and comparison of it with the exptl. results leads to an estimate of the localization of the conduction-band wave functions. 24 references.
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    33. 33
      Suryanarayana, C. Mechanical Alloying and Milling. Prog. Mater. Sci. 2001, 46 (1), 1– 184,  DOI: 10.1016/S0079-6425(99)00010-9
      There is no corresponding record for this reference.
    34. 34
      Riyaz, S.; Parveen, A.; Azam, A. Microstructural and Optical Properties of CuS Nanoparticles Prepared by Sol–Gel Route. Perspect. Sci. 2016, 8, 632– 635,  DOI: 10.1016/j.pisc.2016.06.041
      There is no corresponding record for this reference.
    35. 35
      Yuan, B.; Luan, W.; Tu, S.; Wu, J. One-Step Synthesis of Pure Pyrite FeS 2 with Different Morphologies in Water. New J. Chem. 2015, 39 (5), 3571– 3577,  DOI: 10.1039/C4NJ02243B
      There is no corresponding record for this reference.
    36. 36
      Roberts, W. M. B.; Buchanan, A. S. The Effects of Temperature, Pressure, and Oxygen on Copper and Iron Sulphides Synthesised in Aqueous Solution. Miner. Deposita 1971, 6, 23– 33,  DOI: 10.1007/BF00207114
      There is no corresponding record for this reference.
    37. 37
      Khalid, S.; Ahmed, E.; Malik, M. A.; Lewis, D. J.; Bakar, S. A.; Khan, Y.; O’Brien, P. Synthesis of Pyrite Thin Films and Transition Metal Doped Pyrite Thin Films by Aerosol-Assisted Chemical Vapour Deposition. New J. Chem. 2015, 39 (2), 1013– 1021,  DOI: 10.1039/C4NJ01461H
      37
      Synthesis of pyrite thin films and transition metal doped pyrite thin films by aerosol-assisted chemical vapor deposition
      Khalid, Sadia; Ahmed, Ejaz; Azad Malik, M.; Lewis, David J.; Abu Bakar, Shahzad; Khan, Yaqoob; O'Brien, Paul
      New Journal of Chemistry (2015), 39 (2), 1013-1021CODEN: NJCHE5; ISSN:1144-0546. (Royal Society of Chemistry)
      Diethyldithiocarbamato-metal complexes of the general formula [M(S2CN(Et)2)n] (M = Fe(III), Co(III), Ni(II), Cu(II), Zn(II) and n = 2, 3) have been synthesized and used as precursors for the deposition of iron pyrite (FeS2) and transition metal doped iron pyrite (MxFe1-xS2) thin films on glass and indium tin oxide (ITO) coated glass substrates by aerosol assisted chem. vapor deposition (AACVD). Thermogravimetric anal. (TGA) confirmed that all the five complexes decomp. into their corresponding metal sulfides. The iron complex [Fe(S2CNEt2)3] (1) deposited pure cubic pyrite (FeS2) films with granular crystallites at 350 °C, whereas at 450 °C pyrite and marcasite were deposited. MxFe1-xS2 (where M = Co, Ni, Cu, or Zn) films were deposited by varying the relative concn. of complexes [Fe(S2CNEt2)3] (1) and [Co(S2CNEt2)3] (2), [Ni(S2CNEt2)2] (3), [Cu(S2CNEt2)2] (4) and [Zn(S2CNEt2)2] (5) at 350 °C. The formation of a solid soln. was confirmed by powder X-ray diffraction (p-XRD). The surface morphol. of the films was studied by SEM (SEM) while the height profiles of the films were revealed by at. force microscopy (AFM). The elemental compns. of the films were confirmed by energy-dispersive X-ray (EDX) spectroscopy. To the best of our knowledge, these complexes are the first in their class to be used as single source precursors to deposit MxFe1-xS2 thin films.
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    38. 38
      Gao, Y.; Li, Z.; Fu, Z.; Zhang, H.; Wang, G.; Zhou, H. Highly Selective Capacitive Deionization of Copper Ions in FeS2@N, S Co-Doped Carbon Electrode from Wastewater. Sep. Purif. Technol. 2021, 262, 118336  DOI: 10.1016/j.seppur.2021.118336
      38
      Highly selective capacitive deionization of copper ions in FeS2@N, S co-doped carbon electrode from wastewater
      Gao, Yong; Li, Zhaolei; Fu, Zhen; Zhang, Haimin; Wang, Guozhong; Zhou, Hongjian
      Separation and Purification Technology (2021), 262 (), 118336CODEN: SPUTFP; ISSN:1383-5866. (Elsevier B.V.)
      Capacitive deionization (CDI) as a promising water treatment technique aroused great concern for selective electrosorption of heavy metal ions from complex wastewater. Here, for the first time, we developed FeS2@N, S co-doped carbon (FeS2@NSC) composites as a novel electrode material for high-efficiency selective electrosorption of Cu2+ ion under various cations coexistence system. On account of the synergistic effect of elec. double layers and pseudocapacitance of FeS2@NSC electrode, the superior electrosorption performance of 508.5 mg•g-1 and high coeff. of selectivity (Cu2+/Na+) of 71.6 at molar ratio of 1:10 for Cu2+ ion were achieved at 1.0 V. Significantly, the FeS2@NSC electrode had obvious Cu2+ ion selective electrosorption behavior in mixed ions environment including Cu2+, Pb2+, Cd2+, Zn2+, Co2+ and Mn2+ ions. Finally, the ex-situ XRD and XPS characterization demonstrated that the highly selective electrosorption of Cu2+ ion in FeS2@NSC was dominated by the Faradic redox reaction of the Fe2+/Fe3+ and Cu2+/Cu+ couples. The selective electrosorption performance of FeS2@NSC electrode was also confirmed by treatment of real copper-contg. electroplating wastewater.
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    39. 39
      Bakr, N.; Kamil, A.; Jabbar, M. Preparation and Study of Some Physical Properties of CuxZn1-xS Thin Films. J. Chem., Biol. Phys. Sci. 2018, 8, 077-088  DOI: 10.24214/jcbps.C.8.1.07788
      There is no corresponding record for this reference.
    40. 40
      Nafees, M.; Ikram, M.; Ali, S. Thermal Behavior and Decomposition of Copper Sulfide Nanomaterial Synthesized by Aqueous Sol Method. Dig. J. Nanomater. Biostruct. 2015, 10 (2), 635– 641
      There is no corresponding record for this reference.
    41. 41
      Krylova, V.; Dukštienė, N.; Prosyčeva, I. Deposition and Characterization of Copper Sulphide Layers on the Home-Made Polycarbonate Plates. Chemija 2014, 25 (3), 137– 144
      There is no corresponding record for this reference.
    42. 42
      Keller-Besrest, F.; Collin, G. Structural Aspects of the α Transition in Stoichiometric FeS: Identification of the High-Temperature Phase. J. Solid State Chem. 1990, 84 (2), 194– 210,  DOI: 10.1016/0022-4596(90)90319-S
      There is no corresponding record for this reference.
    43. 43
      Anthony, J. W.; Bideaux, R. A.; Bladh, K. W.; Nichols, M. C. Handbook of Mineralogy; Mineral Data Publ., 2001; Vol. 1.
      There is no corresponding record for this reference.
    44. 44
      Klimm, K.; Botcharnikov, R. E. The Determination of Sulfate and Sulfide Species in Hydrous Silicate Glasses Using Raman Spectroscopy. Am. Mineral. 2010, 95 (10), 1574– 1579,  DOI: 10.2138/am.2010.3590
      There is no corresponding record for this reference.
    45. 45
      Hurma, T.; Kose, S. XRD Raman Analysis and Optical Properties of CuS Nanostructured Film. Optik 2016, 127 (15), 6000– 6006,  DOI: 10.1016/j.ijleo.2016.04.019
      45
      XRD Raman analysis and optical properties of CuS nanostructured film
      Hurma, T.; Kose, S.
      Optik (Munich, Germany) (2016), 127 (15), 6000-6006CODEN: OTIKAJ; ISSN:0030-4026. (Elsevier GmbH)
      Raman spectroscopy and X-ray diffraction (XRD) methods were applied to det. the phase compn. and crystal quality of CuS nanostructured film grown by spray pyrolysis. The film has polycryst. structure with preferential growth along the (101) plane. The grain size for the film was found to be lower than 20 nm. The very sharp Raman peak around 470 cm-1 in the high frequency region was identified as the S-S stretching mode of S2 ions at the 4e sites. Other Raman peaks were around 266 cm-1, 118 cm-1 and 68 cm-1 in the low frequency region due to CuS phase. Particles of nanometric size show low wavenumber vibrational modes that can be obsd. by Raman spectroscopy. Optical properties were obtained from UV-vis absorption, transmittance and reflectance spectra of the nanostructured CuS film. The optical consts. of the film such as refractive index, extinction coeff. and, optical cond. were investigated. The film was found to be p-type by using hot probe method.
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    46. 46
      Yeryukov, N. A.; Milekhin, A. G.; Sveshnikova, L. L.; Duda, T. A.; Pokrovsky, L. D.; Gutakovskii, A. K.; Batsanov, S. A.; Rodyakina, E. E.; Latyshev, A. V.; Zahn, D. R. T. Synthesis and Characterization of Cu x S (X = 1–2) Nanocrystals Formed by the Langmuir–Blodgett Technique. J. Phys. Chem. C 2014, 118 (40), 23409– 23414,  DOI: 10.1021/jp507355t
      46
      Synthesis and Characterization of CuxS (x = 1-2) Nanocrystals Formed by the Langmuir-Blodgett Technique
      Yeryukov, Nikolay A.; Milekhin, Alexander G.; Sveshnikova, Larisa L.; Duda, Tatyana A.; Pokrovsky, Lev D.; Gutakovskii, Anton K.; Batsanov, Stepan A.; Rodyakina, Ekaterina E.; Latyshev, Alexander V.; Zahn, Dietrich R. T.
      Journal of Physical Chemistry C (2014), 118 (40), 23409-23414CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
      The results on the investigation of structural and vibrational properties of CuxS (x = 1-2) nanocrystals formed using the Langmuir-Blodgett technique are reported. The synthesis requires deposition of high quality Langmuir-Blodgett films of copper behenates on a solid substrate (Si, Au, and Pt). The Langmuir-Blodgett film is then sulfidized, which results in the formation of the copper sulfide nanocrystals embedded in behenic acid matrix. Finally, free-standing CuxS nanocrystals are obtained after temp. annealing at 120-400°C in an Ar atm. Morphol. (size, shape, and areal d.) and the crystal structure of nanocrystals were detd. by direct structural methods, including scanning and transmission electron microscopies and high-energy electron diffraction. Surface-enhanced Raman scattering (SERS) by optical phonons in CuxS nanocrystals in the vicinity of metal nanoclusters provided a significant enhancement factor (about 25) and allowed the fine structure of their phonon spectrum to be obsd. SERS spectra of CuxS nanocrystals under annealing reveal the high frequency shift of optical phonon modes from 475 to 492 cm-1, which is explained by the existence of minor copper-deficient crystal phases. The combination of surface-enhanced Raman scattering spectroscopy, electron diffraction, and electron transmission microscopy allowed the authors to establish at least three stable phases: CuS, Cu1.8S, and Cu2S.
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    47. 47
      Jiang, Y.; Xu, Y.; Zhang, Q.; Zhao, X.; Xiao, F.; Wang, X.; Ma, G. Templated Synthesis of Cu2S Hollow Structures for Highly Active Ozone Decomposition. Catalysts 2024, 14 (2), 153,  DOI: 10.3390/catal14020153
      There is no corresponding record for this reference.
    48. 48
      Minceva-Sukarova, B.; Najdoski, M.; Grozdanov, I.; Chunnilall, C. J. Raman Spectra of Thin Solid Films of Some Metal Sulfides. J. Mol. Struct. 1997, 410–411, 267– 270,  DOI: 10.1016/S0022-2860(96)09713-X
      48
      Raman spectra of thin solid films of some metal sulfides
      Minceva-Sukarova, B.; Najdoski, M.; Grozdanov, I.; Chunnilall, C. J.
      Journal of Molecular Structure (1997), 410-411 (), 267-270CODEN: JMOSB4; ISSN:0022-2860. (Elsevier)
      Thin solid films of metal sulfides: Cu2S, CuS, PbS, Sb2-xBixS3, Ag2S and HgS, and 2 selenides: Cu2Se and PbSe, were prepd. by the technique of electroless chem. deposition. For the purpose of recording the Raman spectra, the metal sulfides (selenides) were deposited on glass substrates. All deposited thin films, as well as bulk samples, were characterized by the x-ray diffraction technique. The recorded Raman spectra were compared with the corresponding spectra of bulk metal sulfides (selenides) and discussed in terms of available structural data.
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    49. 49
      Wang, C.; Xue, S.; Hu, J.; Tang, K. Raman, Far Infrared, and Mössbauer Spectroscopy of CuFeS2 Nanocrystallites. Jpn. J. Appl. Phys. 2009, 48 (2R), 023003,  DOI: 10.1143/JJAP.48.023003
      49
      Raman, far infrared, and Moessbauer spectroscopy of CuFeS2 nanocrystallites
      Wang, Chunrui; Xue, Shaolin; Hu, Junqing; Tang, Kaibin
      Japanese Journal of Applied Physics (2009), 48 (2), 023003/1-023003/3CODEN: JJAPB6 ISSN:. (Japan Society of Applied Physics)
      The Raman, far IR, and Mossbauer spectroscopy and photoluminescence of CuFeS2 nanocrystallites are reported. The vibrational and magnetic properties of CuFeS2 nanocrystallites were much sensitive to size than to shape. A new mode was obsd. in Raman and far IR spectra of CuFeS2 nanorods with an av. diam. of 30 nm. The emission light of CuFeS2 nanorods was blue. It may originate from the inner shell transition of 3Eg → 1A1g in the Cu+. The magnetic transition was obsd. in CuFeS2 nanocrystallites, which was only obsd. in the bulk materials at elevated pressure (up to 1.6 GPa).
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    50. 50
      Chakraborty, R. N.; Mahanta, D. S.; Mazumder, S.; Senthilkumar, K. Ion Implantation Induced P-Type Conductivity in FeS2 Thin Film. Phys. Scr. 2024, 99 (5), 055953,  DOI: 10.1088/1402-4896/ad3861
      There is no corresponding record for this reference.
    51. 51
      Kamal, M. S.; Uddin, S.; Kabir, F.; Alam, M.; Rahman, M.; Rahman, M. Numerical Modeling and Analysis of FeS2-Based Solar Cell Employing CuBi2O4 as Back Surface Field Layer. Energy Sources, Part A 2024, 46, 12901– 12912,  DOI: 10.1080/15567036.2024.2402924
      There is no corresponding record for this reference.
    52. 52
      Phuong, H. N.; Van Man, T.; Tung, H. T.; Jun, H. K.; Van Thang, B.; Vinh, L. Q. Effect of Precursors on Cu2S Counter Electrode on the Quantum Dot Sensitized Solar Cell Performance. J. Korean Phys. Soc. 2022, 80 (12), 1133– 1142,  DOI: 10.1007/s40042-022-00460-8
      There is no corresponding record for this reference.
    53. 53
      Van Thang, B.; Tung, H. T.; Phuc, D. H.; Nguyen, T. P.; Van Man, T.; Vinh, L. Q. High-Efficiency Quantum Dot Sensitized Solar Cells Based on Flexible RGO-Cu2S Electrodes Compared with PbS, CuS, Cu2S CEs. Sol. Energy Mater. Sol. Cells 2023, 250, 112042  DOI: 10.1016/j.solmat.2022.112042
      There is no corresponding record for this reference.
    54. 54
      Sousa, M. G.; da Cunha, A. F.; Teixeira, J. P.; Leitão, J. P.; Otero-Irurueta, G.; Singh, M. K. Optimization of Post-Deposition Annealing in Cu2ZnSnS4 Thin Film Solar Cells and Its Impact on Device Performance. Sol. Energy Mater. Sol. Cells 2017, 170, 287– 294,  DOI: 10.1016/j.solmat.2017.05.065
      54
      Optimization of post-deposition annealing in Cu2ZnSnS4 thin film solar cells and its impact on device performance
      Sousa, M. G.; da Cunha, A. F.; Teixeira, J. P.; Leitao, J. P.; Otero-Irurueta, G.; Singh, M. K.
      Solar Energy Materials & Solar Cells (2017), 170 (), 287-294CODEN: SEMCEQ; ISSN:0927-0248. (Elsevier B.V.)
      In this work we present an optimization of the post-deposition annealing, in Cu2ZnSnS4 (CZTS) thin film solar cells, applied at different stages of the solar cell prepn., namely, bare CZTS absorber, CZTS/CdS heterojunction and CZTS/CdS/i-ZnO/ITO complete solar cell. We performed current-d. measurements, SEM (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), Raman scattering, photoluminescence (PL) and XPS studies to enlighten the mechanisms by which solar cells performance improvement comes about. As a result, we concluded that the optimum post-deposition annealing for CZTS is at 300°C for 15 min and at atm. pressure. The highest efficiency gain was obtained when the absorber layer compn. is close to the ideal one and when a single annealing step is performed on complete solar cells, where, we obtained efficiency improvements from below 1% to over 6.6%. Despite the obsd. improvement in device performance for annealing at intermediate stages it is, however, less pronounced than for full cell annealing. In this process we demonstrate very substantial cell performance improvements. XRD results show a shift of all Bragg peaks to lower diffraction angle values, after post-deposition annealing. Also, the intensity of the peaks decreases and their full width at half max. increases. PL measurements show that, post-deposition annealing, leads to a clear redn. of the non-radiative recombination channels and that the electronic structure is dominated by fluctuating potentials. XPS measurements reveal an interdiffusion of Cu, Zn and possibly Cd across the interface between buffer and CZTS absorber layers as the source of the significant obsd. cell performance enhancement.
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    55. 55
      Fernandes, P. A.; Salomé, P. M. P.; Da Cunha, A. F. Precursors’ Order Effect on the Properties of Sulfurized Cu2ZnSnS4 Thin Films. Semicond. Sci. Technol. 2009, 24 (10), 105013,  DOI: 10.1088/0268-1242/24/10/105013
      There is no corresponding record for this reference.
    56. 56
      Bertin, E.; Durand, O.; Létoublon, A.; Cornet, C.; Arzel, L.; Choubrac, L.; Bernard, R.; Gautron, É.; Harel, S.; Jullien, M.; Rohel, T.; Assmann, L.; Barreau, N. Unveiling the Role of Copper Content in the Crystal Structure and Phase Stability of Epitaxial Cu(In,Ga)S2 Films on GaP/Si(001). Mater. Sci. Semicond. Process. 2023, 166, 107685  DOI: 10.1016/j.mssp.2023.107685
      There is no corresponding record for this reference.
    57. 57
      Issac Nelson, P.; Mohan, A.; Kannan, R. R.; Vidhya, B.; Kumari, P.; Reddy, V. R. M.; Kim, W. K.; Ashraf, I. M.; Shkir, M. A Novel Selenization-Free Chalcopyrite CIGSSe Formation in a Heat-Treated Cu2Se/S/Ga3Se2/S/In3Se2Multilayer Thin Film (ML) and ML/n-Si Heterojunction Characteristics. Surf. Interfaces 2023, 41, 103246  DOI: 10.1016/j.surfin.2023.103246
      There is no corresponding record for this reference.
    58. 58
      Bittencourt, J. A. Fundamentals of Plasma Physics; Springer Science & Business Media, 2013.
      There is no corresponding record for this reference.