Scalable and Universal Route for the Deposition of Binary, Ternary, and Quaternary Metal Sulfide Materials from Molecular Precursors

This article references 70 other publications.

1. 1

   Lim, J.; Park, M.; Bae, W. K.; Lee, D.; Lee, S.; Lee, C.; Char, K. Highly efficient cadmium-free quantum dot light-emitting diodes enabled by the direct formation of excitons within [email protected] ZnSeS quantum dots. ACS Nano 2013, 7 (10), 9019– 9026,  DOI: 10.1021/nn403594j

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   1

   Highly Efficient Cadmium-Free Quantum Dot Light-Emitting Diodes Enabled by the Direct Formation of Excitons within [email protected] Quantum Dots

   Lim, Jaehoon; Park, Myeongjin; Bae, Wan Ki; Lee, Donggu; Lee, Seonghoon; Lee, Changhee; Char, Kookheon

   ACS Nano (2013), 7 (10), 9019-9026CODEN: ANCAC3; ISSN:1936-0851. (American Chemical Society)

   We demonstrate bright, efficient, and environmentally benign InP quantum dot (QD)-based light-emitting diodes (QLEDs) through the direct charge carrier injection into QDs and the efficient radiative exciton recombination within QDs. The direct exciton formation within QDs is facilitated by an adoption of a soln.-processed, thin conjugated polyelectrolyte layer, which reduces the electron injection barrier between cathode and QDs via vacuum level shift and promotes the charge carrier balance within QDs. The efficient radiative recombination of these excitons is enabled in structurally engineered [email protected] heterostructured QDs, in which excitons in the InP domain are effectively passivated by thick ZnSeS compn.-gradient shells. The resulting QLEDs record 3.46% of external quantum efficiency and 3900 cd m-2 of max. brightness, which represent 10-fold increase in device efficiency and 5-fold increase in brightness compared with previous reports. We believe that such a comprehensive scheme in designing device architecture and the structural formulation of QDs provides a reasonable guideline for practical realization of environmentally benign, high-performance QLEDs in the future.

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2. 2

   Shen, H.; Bai, X.; Wang, A.; Wang, H.; Qian, L.; Yang, Y.; Titov, A.; Hyvonen, J.; Zheng, Y.; Li, L. S. High-Efficient Deep-Blue Light-Emitting Diodes by Using High Quality ZnxCd1-xS/ZnS Core/Shell Quantum Dots. Adv. Funct. Mater. 2014, 24 (16), 2367– 2373,  DOI: 10.1002/adfm.201302964

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   High-Efficient Deep-Blue Light-Emitting Diodes by Using High Quality ZnxCd1-xS/ZnS Core/Shell Quantum Dots

   Shen, Huaibin; Bai, Xianwei; Wang, Aqiang; Wang, Hongzhe; Qian, Lei; Yang, Yixing; Titov, Alexandre; Hyvonen, Jake; Zheng, Ying; Li, Lin Song

   Advanced Functional Materials (2014), 24 (16), 2367-2373CODEN: AFMDC6; ISSN:1616-301X. (Wiley-VCH Verlag GmbH & Co. KGaA)

   High-quality violet-blue emitting ZnxCd1-xS/ZnS core/shell quantum dots (QDs) are synthesized by a new method, called "nucleation at low temp./shell growth at high temp.". The resulting nearly monodisperse ZnxCd1-xS/ZnS core/shell QDs have high PL quantum yield (near to 100̂), high color purity (FWHM) <25 nm, good color tunability in the violet-blue optical window from 400 to 470 nm, and good chem./photochem. stability. More importantly, the new well-established protocols are easy to apply to large-scale synthesis; around 37 g ZnxCd1-xS/ZnS core/shell QDs can be easily synthesized in one batch reaction. Highly efficient deep-blue quantum dot-based light-emitting diodes (QD-LEDs) are demonstrated by employing the ZnxCd1-xS/ZnS core/shell QDs as emitters. The bright and efficient QD-LEDs show a max. luminance up to 4100 cd m-2, and peak external quantum efficiency (EQE) of 3.8̂, corresponding to 1.13 cd A-1 in luminous efficiency. Such high value of the peak EQE can be comparable with OLED technol. These results signify a remarkable progress, not only in the synthesis of high-quality QDs but also in QD-LEDs that offer a practical platform for the realization of QD-based violet-blue display and lighting.

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3. 3

   Cui, Y.; Zhou, Z.; Li, T.; Wang, K.; Li, J.; Wei, Z. Versatile Crystal Structures and (Opto) electronic Applications of the 2D Metal Mono-, Di-, and Tri-Chalcogenide Nanosheets. Adv. Funct. Mater. 2019, 29, 1900040,  DOI: 10.1002/adfm.201900040

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   Bragagnolo, J. A.; Barnett, A. M.; Phillips, J. E.; Hall, R. B.; Rothwarf, A.; Meakin, J. D. The design and fabrication of thin-film CdS/Cu 2 S cells of 9.15-percent conversion efficiency. IEEE Trans. Electron Devices 1980, 27 (4), 645– 651,  DOI: 10.1109/T-ED.1980.19917

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   Riha, S. C.; Parkinson, B. A.; Prieto, A. L. Solution-based synthesis and characterization of Cu2ZnSnS4 nanocrystals. J. Am. Chem. Soc. 2009, 131 (34), 12054– 12055,  DOI: 10.1021/ja9044168

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   Solution-Based Synthesis and Characterization of Cu2ZnSnS4 Nanocrystals

   Riha, Shannon C.; Parkinson, Bruce A.; Prieto, Amy L.

   Journal of the American Chemical Society (2009), 131 (34), 12054-12055CODEN: JACSAT; ISSN:0002-7863. (American Chemical Society)

   Recent advances have been made in thin-film solar cells using CdTe and CuIn1-xGaxSe2 (CIGS) nanoparticles, which have achieved impressive efficiencies. Despite these efficiencies, CdTe and CIGS are not amenable to large-scale prodn. because of the cost and scarcity of Te, In, and Ga. Cu2ZnSnS4 (CZTS), however, is an emerging solar cell material that contains only earth-abundant elements and has a near-optimal direct band gap of 1.45-1.65 eV and a large absorption coeff. The direct synthesis of CZTS nanocrystals using the hot-injection method is presented. In-depth characterization indicated that pure stoichiometric CZTS nanocrystals with an av. particle size of 12.8±1.8 nm were formed. Optical measurements showed a band gap of 1.5 eV which is optimal for a single-junction solar device.

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6. 6

   Riha, S. C.; Parkinson, B. A.; Prieto, A. L. Compositionally Tunable Cu2ZnSn (S1–x Se x) 4 Nanocrystals: Probing the Effect of Se-Inclusion in Mixed Chalcogenide Thin Films. J. Am. Chem. Soc. 2011, 133 (39), 15272– 15275,  DOI: 10.1021/ja2058692

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   6

   Compositionally Tunable Cu2ZnSn(S1-xSex)4 Nanocrystals: Probing the Effect of Se-Inclusion in Mixed Chalcogenide Thin Films

   Riha, Shannon C.; Parkinson, B. A.; Prieto, Amy L.

   Journal of the American Chemical Society (2011), 133 (39), 15272-15275CODEN: JACSAT; ISSN:0002-7863. (American Chemical Society)

   Nanocrystals of multicomponent chalcogenides, such as Cu2ZnSnS4 (CZTS), are potential building blocks for low-cost thin-film photovoltaics (PVs). CZTS PV devices with modest efficiencies were realized through postdeposition annealing at high temps. in Se vapor. However, little is known about the precise role of Se in the CZTS system. The authors report the direct soln.-phase synthesis and characterization of Cu2ZnSn(S1-xSex)4 nanocrystals (0 ≤ x ≤ 1) with the aim of probing the role of Se incorporation into CZTS. The authors' results indicate that increasing the amt. of Se increases the lattice parameters, slightly decreases the band gap, and most importantly increases the elec. cond. of the nanocrystals without a need for annealing.

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7. 7

   Miskin, C. K.; Yang, W. C.; Hages, C. J.; Carter, N. J.; Joglekar, C. S.; Stach, E. A.; Agrawal, R. 9.0% efficient Cu2ZnSn (S, Se) 4 solar cells from selenized nanoparticle inks. Prog. Photovoltaics 2015, 23 (5), 654– 659,  DOI: 10.1002/pip.2472

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   9.0% efficient Cu2ZnSn(S,Se)4 solar cells from selenized nanoparticle inks

   Miskin, Caleb K.; Yang, Wei-Chang; Hages, Charles J.; Carter, Nathaniel J.; Joglekar, Chinmay S.; Stach, Eric A.; Agrawal, Rakesh

   Progress in Photovoltaics (2015), 23 (5), 654-659CODEN: PPHOED; ISSN:1062-7995. (John Wiley & Sons Ltd.)

   Thin-film solar cells using Cu2ZnSn(S,Se)4 absorber materials continue to attract increasing attention. The synthesis of kesterite Cu2ZnSnS4 nanoparticles by a modified method of hot injection is explained. Characterization of the nanoparticles by energy dispersive X-ray spectroscopy, X-ray diffraction, Raman, and transmission electron microscopy is presented and discussed. When suspended in an ink, coated, and processed into a device, the nanoparticles obtained by this synthesis achieve a total area (active area) efficiency of 9.0% (9.8%) using AM 1.5 illumination and light soaking. This improvement over the previous efficiency of 7.2% is attributed to the modified synthesis approach, as well as fine-tuned conditions for selenizing the coated nanoparticles into a dense absorber layer.

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8. 8

   Sinsermsuksakul, P.; Hartman, K.; Bok Kim, S.; Heo, J.; Sun, L.; Hejin Park, H.; Chakraborty, R.; Buonassisi, T.; Gordon, R. G. Enhancing the efficiency of SnS solar cells via band-offset engineering with a zinc oxysulfide buffer layer. Appl. Phys. Lett. 2013, 102 (5), 053901,  DOI: 10.1063/1.4789855

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   Enhancing the efficiency of SnS solar cells via band-offset engineering with a zinc oxysulfide buffer layer

   Sinsermsuksakul, Prasert; Hartman, Katy; Bok Kim, Sang; Heo, Jaeyeong; Sun, Leizhi; Hejin Park, Helen; Chakraborty, Rupak; Buonassisi, Tonio; Gordon, Roy G.

   Applied Physics Letters (2013), 102 (5), 053901/1-053901/5CODEN: APPLAB; ISSN:0003-6951. (American Institute of Physics)

   SnS is a promising earth-abundant material for photovoltaic applications. Heterojunction solar cells were made by vapor deposition of p-type Sn(II) sulfide, SnS, and n-type Zn oxysulfide, Zn(O,S), using a device structure of soda-lime glass/Mo/SnS/Zn(O,S)/ZnO/ITO. A record efficiency was achieved for SnS-based thin-film solar cells by varying the O-to-S ratio in Zn(O,S). Increasing the S content in Zn(O,S) raises the conduction band offset between Zn(O,S) and SnS to an optimum slightly pos. value. A record SnS/Zn(O,S) solar cell with a S/Zn ratio of 0.37 exhibits short circuit c.d. (Jsc), open circuit voltage (Voc), and fill factor (FF) of 19.4 mA/cm2, 0.244 V, and 42.97%, resp., as well as an NREL-certified total-area power-conversion efficiency of 2.04% and an uncertified active-area efficiency of 2.46%. (c) 2013 American Institute of Physics.

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9. 9

   Catti, M.; Noel, Y.; Dovesi, R. Full piezoelectric tensors of wurtzite and zinc blende ZnO and ZnS by first-principles calculations. J. Phys. Chem. Solids 2003, 64 (11), 2183– 2190,  DOI: 10.1016/S0022-3697(03)00219-1

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   Full piezoelectric tensors of wurtzite and zinc blende ZnO and ZnS by first-principles calculations

   Catti, M.; Noel, Y.; Dovesi, R.

   Journal of Physics and Chemistry of Solids (2003), 64 (11), 2183-2190CODEN: JPCSAW; ISSN:0022-3697. (Elsevier Science B.V.)

   The complete piezoelec. tensors of both the wurtzite and zinc blende polymorphs of ZnO and ZnS have been computed by ab initio periodic LCAO (LCAO) methods, based mainly on the Hartree-Fock Hamiltonian, with an all-electron Gaussian-type basis set. The computational scheme was based on the Berry phases theory, yielding directly the proper piezoelec. stress coeffs. eik=(.vdelta.Pi/.vdelta..vepsiln.k)E; also the strain coeffs. dik=(.vdelta..vepsiln.k/.vdelta.Ei)τ were obtained, by intermediate calcn. of the full elasticity tensors of all four crystals. In particular, the e15 wurtzite shear consts. were included for the first time in such calcns. A careful study of the clamped-ion and internal-strain piezoelec. components shows that the latter ones are well simulated by classical point-charge calcns. including quantum-mech. structural relaxation. The much larger piezoelec. response of ZnO with respect to ZnS is explained by analyzing signs and ratios of the resp. clamped-ion and internal-strain components.

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10. 10

    Liu, H.; Shi, X.; Xu, F.; Zhang, L.; Zhang, W.; Chen, L.; Li, Q.; Uher, C.; Day, T.; Snyder, G. J. Copper ion liquid-like thermoelectrics. Nat. Mater. 2012, 11 (5), 422– 425,  DOI: 10.1038/nmat3273

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    Copper ion liquid-like thermoelectrics

    Liu, Huili; Shi, Xun; Xu, Fangfang; Zhang, Linlin; Zhang, Wenqing; Chen, Lidong; Li, Qiang; Uher, Ctirad; Day, Tristan; Snyder, G. Jeffrey

    Nature Materials (2012), 11 (5), 422-425CODEN: NMAACR; ISSN:1476-1122. (Nature Publishing Group)

    Advanced thermoelec. technol. offers a potential for converting waste industrial heat into useful electricity, and an emission-free method for solid state cooling. Worldwide efforts to find materials with thermoelec. figure of merit, zT values significantly above unity, are frequently focused on cryst. semiconductors with low thermal cond. Here we report on Cu2-xSe, which reaches a zT of 1.5 at 1,000 K, among the highest values for any bulk materials. Whereas the Se atoms in Cu2-xSe form a rigid face-centered cubic lattice, providing a cryst. pathway for semiconducting electrons (or more precisely holes), the copper ions are highly disordered around the Se sublattice and are superionic with liq.-like mobility. This extraordinary liq.-like' behavior of copper ions around a cryst. sublattice of Se in Cu2-xSe results in an intrinsically very low lattice thermal cond. which enables high zT in this otherwise simple semiconductor. This unusual combination of properties leads to an ideal thermoelec. material. The results indicate a new strategy and direction for high-efficiency thermoelec. materials by exploring systems where there exists a cryst. sublattice for electronic conduction surrounded by liq.-like ions.

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11. 11

    Sassi, S.; Candolfi, C.; Vaney, J.-B.; Ohorodniichuk, V.; Masschelein, P.; Dauscher, A.; Lenoir, B. Assessment of the thermoelectric performance of polycrystalline p-type SnSe. Appl. Phys. Lett. 2014, 104 (21), 212105,  DOI: 10.1063/1.4880817

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    Assessment of the thermoelectric performance of polycrystalline p-type SnSe

    Sassi, S.; Candolfi, C.; Vaney, J.-B.; Ohorodniichuk, V.; Masschelein, P.; Dauscher, A.; Lenoir, B.

    Applied Physics Letters (2014), 104 (21), 212105/1-212105/4CODEN: APPLAB; ISSN:0003-6951. (American Institute of Physics)

    Reported is the evaluation of the thermoelec. performance of polycryst. p-type SnSe, a material in which unprecedented values of the thermoelec. figure of merit ZT were recently discovered in single crystals. Besides anisotropic transport properties, this results confirm that this compd. exhibits intrinsically very low thermal cond. values. The elec. properties show trends typical of lightly doped, intrinsic semiconductors with thermopower values reaching 500 μV K-1 in a broad temp. range. An orthorhombic-to-orthorhombic transition sets in at 823 K, a temp. at which the power factor reaches its max. value. A max. ZT of 0.5 was obtained at 823 K, suggesting that proper optimization of the transport properties of SnSe might lead to higher ZT values. These findings indicate that this system represents an interesting exptl. platform for the search of highly efficient thermoelec. materials. (c) 2014 American Institute of Physics.

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12. 12

    Zhao, L.-D.; Lo, S.-H.; Zhang, Y.; Sun, H.; Tan, G.; Uher, C.; Wolverton, C.; Dravid, V. P.; Kanatzidis, M. G. Ultralow thermal conductivity and high thermoelectric figure of merit in SnSe crystals. Nature 2014, 508 (7496), 373– 377,  DOI: 10.1038/nature13184

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    Ultralow thermal conductivity and high thermoelectric figure of merit in SnSe crystals

    Zhao, Li-Dong; Lo, Shih-Han; Zhang, Yongsheng; Sun, Hui; Tan, Gangjian; Uher, Ctirad; Wolverton, C.; Dravid, Vinayak P.; Kanatzidis, Mercouri G.

    Nature (London, United Kingdom) (2014), 508 (7496), 373-377CODEN: NATUAS; ISSN:0028-0836. (Nature Publishing Group)

    The thermoelec. effect enables direct and reversible conversion between thermal and elec. energy, and provides a viable route for power generation from waste heat. The efficiency of thermoelec. materials is dictated by the dimensionless figure of merit, ZT (where Z is the figure of merit and T is abs. temp.), which governs the Carnot efficiency for heat conversion. Enhancements above the generally high threshold value of 2.5 have important implications for com. deployment, esp. for compds. free of Pb and Te. Here we report an unprecedented ZT of 2.6 ± 0.3 at 923 K, realized in SnSe single crystals measured along the b axis of the room-temp. orthorhombic unit cell. This material also shows a high ZT of 2.3 ± 0.3 along the c axis but a significantly reduced ZT of 0.8 ± 0.2 along the a axis. We attribute the remarkably high ZT along the b axis to the intrinsically ultralow lattice thermal cond. in SnSe. The layered structure of SnSe derives from a distorted rock-salt structure, and features anomalously high Grueneisen parameters, which reflect the anharmonic and anisotropic bonding. We attribute the exceptionally low lattice thermal cond. (0.23 ± 0.03 W m-1 K-1 at 973 K) in SnSe to the anharmonicity. These findings highlight alternative strategies to nanostructuring for achieving high thermoelec. performance.

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13. 13

    Xu, Y.; Hu, E.; Hu, K.; Xu, Y.; Hu, X. J. T. I. Tribol. Int. 2015, 92, 172– 183,  DOI: 10.1016/j.triboint.2015.06.011

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    Formation of an adsorption film of MoS2 nanoparticles and dioctyl sebacate on a steel surface for alleviating friction and wear

    Xu, Yong; Hu, Enzhu; Hu, Kunhong; Xu, Yufu; Hu, Xianguo

    Tribology International (2015), 92 (), 172-183CODEN: TRBIBK; ISSN:0301-679X. (Elsevier Ltd.)

    Solid sphere-like nano-MoS2 particles were synthesized via a modified chem. method. The as-synthesized nano-MoS2 could improve the tribol. properties of dioctyl sebacate (DOS) more compared with a com. 2H micro-MoS2. The lubrication of micro-MoS2 in DOS was ascribed to the tribofilm formed by the tribochem. reactions. When the nano-MoS2 was applied as an additive in DOS, a solid complex adsorption film beside the tribofilm was formed on the friction surface to reduce the friction and wear. The adsorption film was composed of MoS2, DOS, and their chem. bonded compds.

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    Huang, H.; Tu, J.; Gan, L.; Li, C. J. W. Wear 2006, 261 (2), 140– 144,  DOI: 10.1016/j.wear.2005.09.010

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    An investigation on tribological properties of graphite nanosheets as oil additive

    Huang, H. D.; Tu, J. P.; Gan, L. P.; Li, C. Z.

    Wear (2006), 261 (2), 140-144CODEN: WEARAH; ISSN:0043-1648. (Elsevier B.V.)

    Graphite nanosheets with av. diam. of 500 nm and thickness about 15 nm were prepd. by stirring ball milling. The tribol. behavior of the graphite nanosheets as additive in paraffin oil were investigated with a four-ball and a pin-on-disk friction and wear tester. The wear surfaces of the steel ball lubricated with the additive-contg. paraffin oil were analyzed by means of SEM. It has been found that the graphite nanosheets as additive in oil at proper concn. show better tribol. properties than pure paraffin oil. The load-carrying capacity and antiwear ability of the lubricating oil were improved. Moreover, the friction coeff. of the lubricating oil was decreased by the addn. of the graphite nanosheets. The optimal concn. of the additive in paraffin oil is about 1.0 × 10-2 wt.%.

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    Prasad, S.; Zabinski, J. Lubricants: super slippery solids. Nature 1997, 387 (6635), 761,  DOI: 10.1038/42820

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    Lubricants: super slippery solids

    Prasad, Somuri; Zabinski, Jeffrey

    Nature (London) (1997), 387 (6635), 761, 763CODEN: NATUAS; ISSN:0028-0836. (Macmillan Magazines)

    There is no expanded citation for this reference.

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16. 16

    Yu, X.; Shavel, A.; An, X.; Luo, Z.; Ibáñez, M.; Cabot, A. Cu2ZnSnS4-Pt and Cu2ZnSnS4-Au heterostructured nanoparticles for photocatalytic water splitting and pollutant degradation. J. Am. Chem. Soc. 2014, 136 (26), 9236– 9239,  DOI: 10.1021/ja502076b

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    16

    Cu2ZnSnS4-Pt and Cu2ZnSnS4-Au Heterostructured Nanoparticles for Photocatalytic Water Splitting and Pollutant Degradation

    Yu, Xuelian; Shavel, Alexey; An, Xiaoqiang; Luo, Zhishan; Ibanez, Maria; Cabot, Andreu

    Journal of the American Chemical Society (2014), 136 (26), 9236-9239CODEN: JACSAT; ISSN:0002-7863. (American Chemical Society)

    Cu2ZnSnS4, based on abundant and environmental friendly elements and with a direct band gap of 1.5 eV, is a main candidate material for solar energy conversion through both photovoltaics and photocatalysis. We detail here the synthesis of quasi-spherical Cu2ZnSnS4 nanoparticles with unprecedented narrow size distributions. We further detail their use as seeds to produce CZTS-Au and CZTS-Pt heterostructured nanoparticles. Such heterostructured nanoparticles are shown to have excellent photocatalytic properties toward degrdn. of Rhodamine B and hydrogen generation by water splitting.

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17. 17

    Al-Shakban, M.; Matthews, P. D.; Savjani, N.; Zhong, X. L.; Wang, Y.; Missous, M.; O’Brien, P. The synthesis and characterization of Cu 2 ZnSnS 4 thin films from melt reactions using xanthate precursors. J. Mater. Sci. 2017, 52 (21), 12761– 12771,  DOI: 10.1007/s10853-017-1367-0

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    17

    Synthesis and characterization of Cu2ZnSnS4 thin films from melt reactions using xanthate precursors

    Al-Shakban, Mundher; Matthews, Peter D.; Savjani, Nicky; Zhong, Xiang L.; Wang, Yuekun; Missous, Mohamed; O'Brien, Paul

    Journal of Materials Science (2017), 52 (21), 12761-12771CODEN: JMTSAS; ISSN:0022-2461. (Springer)

    Kesterite, Cu2ZnSnS4 (CZTS), is a promising absorber layer for use in photovoltaic cells. We report the use of copper, zinc and tin xanthates in melt reactions to produce Cu2ZnSnS4 (CZTS) thin films. The phase of the as-produced CZTS is dependent on decompn. temp. X-ray diffraction patterns and Raman spectra show that films annealed between 375 and 475 °C are tetragonal, while at temps. <375 °C hexagonal material was obtained. The elec. parameters of the CZTS films have also been detd. The conduction of all films was p-type, while the other parameters differ for the hexagonal and tetragonal materials: resistivity (27.1 vs 1.23 Ω cm), carrier concn. (2.65 × 10+15 vs 4.55 × 10+17 cm-3) and mobility (87.1 vs 11.1 cm2 V-1 s-1). The Hall coeffs. were 2.36 × 103 vs. 13.7 cm3 C-1.

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18. 18

    Green, M. A.; Dunlop, E. D.; Hohl-Ebinger, J.; Yoshita, M.; Kopidakis, N.; Ho-Baillie, A. W.Y. Solar cell efficiency tables (Version 55). Prog. Photovoltaics 2020, 28, 3– 15,  DOI: 10.1002/pip.3228

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    Ezenwa, T. E.; McNaughter, P. D.; Raftery, J.; Lewis, D. J.; O’Brien, P. Full compositional control of PbS x Se 1– x thin films by the use of acylchalcogourato lead (ii) complexes as precursors for AACVD. Dalton Trans. 2018, 47 (47), 16938– 16943,  DOI: 10.1039/C8DT03443E

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    Full compositional control of PbSxSe1-x thin films by the use of acylchalcogourato lead(II) complexes as precursors for AACVD

    Ezenwa, Tagbo Emmanuel; McNaughter, Paul D.; Raftery, James; Lewis, David J.; O'Brien, Paul

    Dalton Transactions (2018), 47 (47), 16938-16943CODEN: DTARAF; ISSN:1477-9226. (Royal Society of Chemistry)

    Se and S derivs. of Pb(II) acylchalcogourato complexes were used to deposit PbSxSe1-x thin films by AACVD. By variation of the mole ratio of S and Se precursors in the aerosol feed soln. the full range of PbSxSe1-x was obtained, i.e. 0 ≥ x ≥ 1. The films showed no contaminant phases demonstrating the potential for acylchalcogourato metal complexes as precursors for metal chalcogenide thin films. The crystal structure for bis[N,N-diethyl-N'-2-naphthoylthioureato]lead(II) was solved and displayed the expected decreases in Pb-E bond lengths from the previously reported Se variant.

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20. 20

    Murtaza, G.; Venkateswaran, S. P.; Thomas, A. G.; O’Brien, P.; Lewis, D. J. Chemical vapour deposition of chromium-doped tungsten disulphide thin films on glass and steel substrates from molecular precursors. J. Mater. Chem. C 2018, 6 (35), 9537– 9544,  DOI: 10.1039/C8TC01991F

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    Chemical vapour deposition of chromium-doped tungsten disulphide thin films on glass and steel substrates from molecular precursors

    Murtaza, Ghulam; Venkateswaran, Sai P.; Thomas, Andrew G.; O'Brien, Paul; Lewis, David J.

    Journal of Materials Chemistry C: Materials for Optical and Electronic Devices (2018), 6 (35), 9537-9544CODEN: JMCCCX; ISSN:2050-7534. (Royal Society of Chemistry)

    Polycryst. thin films of chromium-doped tungsten disulfide (WS2) were deposited onto glass and steel substrates by aerosol-assisted chem. vapor deposition (AACVD) using bis(diethyldithiocarbamato)disulfidothioxo tungsten(VI) (WS3L2) and tris(diethyldithiocarbamato) chromium(III) [Cr(S2CNEt2)3] (CrL3) complexes as precursors in different molar ratios at 450°. The deposited films were characterized by p-XRD, SEM, and EDX and Raman spectroscopies. Chromium doping of ≤15 mol% was achieved in WS2 thin films.

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21. 21

    Vikraman, D.; Thiagarajan, S.; Karuppasamy, K.; Sanmugam, A.; Choi, J.-H.; Prasanna, K.; Maiyalagan, T.; Thaiyan, M.; Kim, H.-S. Shape-and size-tunable synthesis of tin sulfide thin films for energy applications by electrodeposition. Appl. Surf. Sci. 2019, 479, 167– 176,  DOI: 10.1016/j.apsusc.2019.02.056

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    Shape- and size-tunable synthesis of tin sulfide thin films for energy applications by electrodeposition

    Vikraman, Dhanasekaran; Thiagarajan, Shrividhya; Karuppasamy, K.; Sanmugam, Anandhavelu; Choi, Jong-Hyeok; Prasanna, K.; Maiyalagan, T.; Thaiyan, Mahalingam; Kim, Hyun-Seok

    Applied Surface Science (2019), 479 (), 167-176CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)

    Size and shape tunable tin sulfide (SnS) thin film structures are successfully prepd. by a simple cost-effective electrodeposition route. Scanning electron micrographs (SEM) effectively demonstrated the SnS shape modification. An EDTA (EDTA) electrolyte was successfully used to alter the size of SnS. The SEM results also give evidence of the surface modification of SnS which was prepd. with EDTA. Atomic force micrographs established the topol. variations of SnS. Energy dispersive X-ray results confirmed the stoichiometric compn. SnS prepd. with and without EDTA. X-ray diffraction results revealed the polycryst. orthorhombic structure of the SnS thin film. The optical band gap derived from the Tauc's plot was found to be in the 1.23-1.26 eV range. The near band edge emission peak for SnS was obsd. using photoluminescence properties. This simple strategy to synthesize a smooth, dense-packed and crack-free morphol. could be an attractive way to produce SnS as a capable material for energy harvesting and optoelectronic devices.

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22. 22

    Udachyan, I.; R. S., V.; C. S., P. K.; Kandaiah, S. Anodic fabrication of nanostructured CuxS and CuNiSx thin films and their hydrogen evolution activities in acidic electrolytes. New J. Chem. 2019, 43, 7674– 7682,  DOI: 10.1039/C9NJ00962K

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    Anodic fabrication of nanostructured CuxS and CuNiSx thin films and their hydrogen evolution activities in acidic electrolytes

    Udachyan, Iranna; R. S., Vishwanath; C. S., Pradeep Kumara; Kandaiah, Sakthivel

    New Journal of Chemistry (2019), 43 (20), 7674-7682CODEN: NJCHE5; ISSN:1144-0546. (Royal Society of Chemistry)

    The electrochem. anodization method is advantageous for direct growth of highly ordered and large surface area hybrid nanostructures. Herein, we report the facile electrochem. anodization of copper and copper-nickel electrodes to prep. the resp. nanostructured metal sulfide thin films. Vertically aligned 2D nanowall (30-50 nm thickness) like features of mixed-valent CuxS and nanostructures of hybrid Cu-NiSx were grown by controlled galvanostatic deposition (1 mA cm-2). The nanostructured Ni electrodeposits on copper favor the facile anodization and growth of a hybrid mixed-valent CuNiSx thin film. XRD and XPS investigations confirm the presence of mixed-valent Cu and Ni ions as their sulfide thin films. These modified electrodes exhibit pseudocapacitive behavior with a good redox capacitance. The overpotentials required by the Cu-NiSx and CuxS electrodes to attain the benchmark c.d. of 10 mA cm-2 in 0.5 M H2SO4 are just 195 mV and 270 mV resp. The hybrid electrode structure (CuNiSx) exhibits improved long-term hydrogen evolution stability (>7 h) compared to the unmodified pristine Cu-Ni electrode (<2 h) in acidic electrolytes. The synergistic effect of porous electrodeposited Ni on the Cu surface and coordinatively unsatd. surface local sites on the hybrid metal sulfides further reduce the overpotential requirement and improve the acidic stability.

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23. 23

    Ortiz-Ramos, D. E.; Martínez-Enríquez, A. I.; González, L. A. CuS films grown by a chemical bath deposition process with amino acids as complexing agents. Mater. Sci. Semicond. Process. 2019, 89, 18– 25,  DOI: 10.1016/j.mssp.2018.08.016

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    CuS films grown by a chemical bath deposition process with amino acids as complexing agents

    Ortiz-Ramos, Daniela E.; Martinez-Enriquez, Arturo I.; Gonzalez, Luis A.

    Materials Science in Semiconductor Processing (2019), 89 (), 18-25CODEN: MSSPFQ; ISSN:1369-8001. (Elsevier Ltd.)

    CuS thin films were deposited by an ammonia-free chem. bath deposition process. This approach uses amino acids (alanine, glycine and serine) as complexing agents. The conditions under which amino acids form complexes and release Cu ions are discussed. All the resulting CuS films, formed by nanoflake particles, had the hexagonal cryst. structure (covellite). Moreover, the coexistence of Cu+ and Cu2+ states in these films were confirmed by XPS. Amino acids as complexing agents were then obsd. to affect mainly to the growth kinetics of the CuS films. Thus, thicknesses of 42, 55.4 and 70 nm were obtained for the films processed with soln. reactions contg. alanine, glycine and serine, resp. The optical band gaps of the films with moderate transmittance had values in the range from 2.25 to 2.4 eV. Finally, the resulting CuS films with elec. resistivities from 1.84 × 10-3 to 2.8 × 10-3 Ω-cm showed a decrease of photosensitivity with the film thickness.

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24. 24

    Mahdi, M. S.; Ibrahim, K.; Ahmed, N. M.; Hmood, A.; Azzez, S. A. Growth and Characterization of Tin Sulphide Nanostructured Thin Film by Chemical Bath Deposition for Near-Infrared Photodetector Application. Solid State Phenom. 2019, 290, 220– 224,  DOI: 10.4028/www.scientific.net/SSP.290.220

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    Park, G. H.; Nielsch, K.; Thomas, A. 2D Transition Metal Dichalcogenide Thin Films Obtained by Chemical Gas Phase Deposition Techniques. Adv. Mater. Interfaces 2019, 6 (3), 1800688,  DOI: 10.1002/admi.201800688

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    Dasgupta, N. P.; Meng, X.; Elam, J. W.; Martinson, A. B. Atomic layer deposition of metal sulfide materials. Acc. Chem. Res. 2015, 48 (2), 341– 348,  DOI: 10.1021/ar500360d

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    Atomic Layer Deposition of Metal Sulfide Materials

    Dasgupta, Neil P.; Meng, Xiangbo; Elam, Jeffrey W.; Martinson, Alex B. F.

    Accounts of Chemical Research (2015), 48 (2), 341-348CODEN: ACHRE4; ISSN:0001-4842. (American Chemical Society)

    A review. The field of nanoscience is delivering increasingly intricate yet elegant geometric structures incorporating an ever-expanding palette of materials. Atomic layer deposition (ALD) is a powerful driver of this field, providing exceptionally conformal coatings spanning the periodic table and at.-scale precision independent of substrate geometry. This versatility is intrinsic to ALD and results from sequential and self-limiting surface reactions. This characteristic facilitates digital synthesis, in which the film grows linearly with the no. of reaction cycles. While the majority of ALD processes identified to date produce metal oxides, novel applications in areas such as energy storage, catalysis, and nanophotonics are motivating interest in sulfide materials. Recent progress in ALD of sulfides has expanded the diversity of accessible materials as well as a more complete understanding of the unique chalcogenide surface chem. ALD of sulfide materials typically uses metalorg. precursors and hydrogen sulfide (H2S). As in oxide ALD, the precursor chem. is crit. to controlling both the film growth and properties including roughness, crystallinity, and impurity levels. By modification of the precursor sequence, multicomponent sulfides have been deposited, although challenges remain because of the higher propensity for cation exchange reactions, greater diffusion rates, and unintentional annealing of this more labile class of materials. A deeper understanding of these surface chem. reactions has been achieved through a combination of in situ studies and quantum-chem. calcns. As this understanding matures, so does our ability to deterministically tailor film properties to new applications and more sophisticated devices. This Account highlights the attributes of ALD chem. that are unique to metal sulfides and surveys recent applications of these materials in photovoltaics, energy storage, and photonics. Within each application space, the benefits and challenges of novel ALD processes are emphasized and common trends are summarized. We conclude with a perspective on potential future directions for metal chalcogenide ALD as well as untapped opportunities. Finally, we consider challenges that must be addressed prior to implementing ALD metal sulfides into future device architectures.

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    Mochel, J. M. Electrically conducting coatings on glass and other ceramic bodies. US Patent US2564707, 1951.

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    Hill, J. E.; Chamberlin, R. R. Process for making conductive film. US Patent US3148084, 1964.

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29. 29

    Sayed, M. H.; Robert, E. V.; Dale, P. J.; Gütay, L. Cu2SnS3 based thin film solar cells from chemical spray pyrolysis. Thin Solid Films 2019, 669, 436– 439,  DOI: 10.1016/j.tsf.2018.11.002

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    Cu2SnS3 based thin film solar cells from chemical spray pyrolysis

    Sayed, Mohamed H.; Robert, Erika V. C.; Dale, Phillip J.; Guetay, Levent

    Thin Solid Films (2019), 669 (), 436-439CODEN: THSFAP; ISSN:0040-6090. (Elsevier B.V.)

    A simple and eco-friendly method for soln. processing of Cu2SnS3 p-type semiconductor absorbers using a water-based precursor soln. is presented. Cu2SnS3 layers were processed by chem. spray pyrolysis deposition of the precursor soln. onto Mo-coated glass substrates at 350°C. The as-prepd. layers were placed inside a graphite susceptor with S and SnS powders and were annealed in a tube furnace at 550°C. The impact of the annealing step on structural, morphol. and device characteristics of the prepd. layers was studied. The as-prepd. layers were crack-free with fine grains and dominant tetragonal Cu2SnS3 structure. A denser and compact Cu2SnS3 layer with larger grains was formed upon annealing accompanied by a structural phase transition from the tetragonal polymorph to the monoclinic phase. The as-prepd. Cu2SnS3 layers showed no photovoltaic activity, whereas the annealed layers showed a device efficiency of 0.65%. A short air annealing of the complete Cu2SnS3 device at 250 °C improved the overall device performance and increased the device efficiency to 1.94%. Mech. removal of shunt paths led to Cu2SnS3 device with 2.28% efficiency.

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30. 30

    Chen, Q.; Jia, Z.; Yuan, H.; Zhu, W.; Ni, Y.; Zhu, X.; Dou, X. The properties of the earth abundant Cu 2 SnS 3 thin film prepared by spray pyrolysis and rapid thermal annealing route. J. Mater. Sci.: Mater. Electron. 2019, 30 (5), 4519– 4526,  DOI: 10.1007/s10854-019-00740-3

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    The properties of the earth abundant Cu2SnS3 thin film prepared by spray pyrolysis and rapid thermal annealing route

    Chen, Qinmiao; Jia, Zhen; Yuan, Hongcun; Zhu, Wei; Ni, Yi; Zhu, Xifang; Dou, Xiaoming

    Journal of Materials Science: Materials in Electronics (2019), 30 (5), 4519-4526CODEN: JSMEEV; ISSN:0957-4522. (Springer)

    Ternary compd. Cu2SnS3 (CTS) was fabricated by simple, low cost and high efficient spray pyrolysis and rapid thermal annealing route. The influences of annealing temp. and annealing duration on the properties of the prepd. CTS thin film were investigated in detail. X-ray diffraction spectrometer, Scanning Electron Microscope, UV-Vis-IR spectrophotometer and I-V test system were employed for the anal. of the structural, morphol., optical and photoelec. properties of the prepd. CTS thin film, resp. The characterization results show that the CTS thin film prepd. under the optimal annealing condition of 500 °C and 15 min presents as tetragonal structure with preferential (1,1,2), bandgap value of 1.44 eV, crystal grain size of around 80 nm and photoelec. conversion efficiency as high as 1.24%.

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31. 31

    Moumen, A.; Hartiti, B.; Comini, E.; Arachchige, H. M. M.; Fadili, S.; Thevenin, P. Preparation and characterization of nanostructured CuO thin films using spray pyrolysis technique. Superlattices Microstruct. 2019, 127, 2– 10,  DOI: 10.1016/j.spmi.2018.06.061

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    Preparation and characterization of nanostructured CuO thin films using spray pyrolysis technique

    Moumen, Abderrahim; Hartiti, Bouchaib; Comini, Elisabetta; El khalidi, Zahira; Arachchige, Hashitha M. M. Munasinghe; Fadili, Salah; Thevenin, Philippe

    Superlattices and Microstructures (2019), 127 (), 2-10CODEN: SUMIEK; ISSN:0749-6036. (Elsevier Ltd.)

    In this work, the suitability of CuO thin films on gas sensors and solar cells applications was investigated. CuO thin films were deposited using spray pyrolysis. The effect of substrates temp. on the films structural and optical properties was discussed. X-ray diffraction showed the appearance of tenorite phase of cupric oxide CuO without impurities indicating the formation of pure cupric oxide material. Raman spectroscopy confirmed the results obtained in XRD and showed CuO phase formation. A crystallinity improvement was measured increasing the temp. from 300 °C to 375 °C. Optical properties such as band gap energy, refractive index, extinction coeff. and optical cond. were extd. using transmittance/absorbance data giving by UV-Visible spectrophotometer. Low transmittance, high absorbance and small band gap energy were obsd. at the highest substrate temp., these characteristics make CuO an appropriate material to be used as absorber layer in photovoltaic applications. The performances of CuO thin film for acetone sensing were proved: 33% of response, 160 s and 360 s as response and recovery time, resp.

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32. 32

    Knapp, C. E.; Carmalt, C. J. Solution based CVD of main group materials. Chem. Soc. Rev. 2016, 45 (4), 1036– 1064,  DOI: 10.1039/C5CS00651A

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    Solution based CVD of main group materials

    Knapp, Caroline E.; Carmalt, Claire J.

    Chemical Society Reviews (2016), 45 (4), 1036-1064CODEN: CSRVBR; ISSN:0306-0012. (Royal Society of Chemistry)

    This crit. review focuses on the soln. based chem. vapor deposition (CVD) of main group materials with particular emphasis on their current and potential applications. Deposition of thin films of main group materials, such as metal oxides, sulfides and arsenides, have been researched owing to the array of applications which utilize them including solar cells, transparent conducting oxides (TCOs) and window coatings. Soln. based CVD processes, such as aerosol-assisted (AA)CVD have been developed due to their scalability and to overcome the requirement of suitably volatile precursors as the technique relies on the soly. rather than volatility of precursors which vastly extends the range of potentially applicable compds. An introduction into the applications and precursor requirements of main group materials will be presented first followed by a detailed discussion of their deposition reviewed according to this application. The challenges and prospects for further enabling research in terms of emerging main group materials will be discussed.

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33. 33

    Akhtar, M.; Akhter, J.; Malik, M. A.; O’Brien, P.; Tuna, F.; Raftery, J.; Helliwell, M. Deposition of iron sulfide nanocrystals from single source precursors. J. Mater. Chem. 2011, 21 (26), 9737– 9745,  DOI: 10.1039/c1jm10703h

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    Deposition of iron sulfide nanocrystals from single source precursors

    Akhtar, Masood; Akhter, Javeed; Malik, M. Azad; O'Brien, Paul; Tuna, Floriana; Raftery, James; Helliwell, Madeleine

    Journal of Materials Chemistry (2011), 21 (26), 9737-9745CODEN: JMACEP; ISSN:0959-9428. (Royal Society of Chemistry)

    Sym. and unsym. dithiocarbamato complexes of Fe(III) [Fe(S2CNRR')3] where R = Et, R' = iPr (1); R, R' = Hex (2); R = Me, R' = Et (3); and R, R' = Et (4) were used as single source precursors to synthesize iron sulfide nanocrystals by thermolysis in oleylamine, hexadecylamine and octadecene at different temps. The nanocrystals obtained were studied by powder XRD and TEM and magnetic measurements. Nanocrystals of iron sulfide with greigite (Fe3S4), pyrrhotite (FeS) and mixed phase were grown at different thermolysis temps. from each precursor. The precursors with shorter alkyl chain length required higher temp. to give the product. Sym. alkyl groups with longer chain alkyl groups gave pure greigite phase at lower thermolysis temp. of 170°, but a mixt. of greigite and pyrrhotite at higher temps. The unsym. alkyl groups gave mixed phase (greigite and pyrrhotite) iron sulfide nanocrystals at all temps. The magnetic properties of the iron sulfide nanocrystals were investigated.

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34. 34

    Tedstone, A. A.; Lewis, E. A.; Savjani, N.; Zhong, X. L.; Haigh, S. J.; O’Brien, P.; Lewis, D. J. Single-Source Precursor for Tungsten Dichalcogenide Thin Films: Mo_1–xW_xS₂ (0 ≤ x ≤ 1) Alloys by Aerosol-Assisted Chemical Vapor Deposition. Chem. Mater. 2017, 29 (9), 3858– 3862,  DOI: 10.1021/acs.chemmater.6b05271

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    Single-Source Precursor for Tungsten Dichalcogenide Thin Films: Mo1-xWxS2 (0 ≤ x ≤ 1) Alloys by Aerosol-Assisted Chemical Vapor Deposition

    Tedstone, Aleksander A.; Lewis, Edward A.; Savjani, Nicky; Zhong, Xiang Li; Haigh, Sarah J.; O'Brien, Paul; Lewis, David J.

    Chemistry of Materials (2017), 29 (9), 3858-3862CODEN: CMATEX; ISSN:0897-4756. (American Chemical Society)

    Abstr.: The coordination complex WS3L2 (where L = S2CN(CH2CH3)2 ) can be used to deposit tungsten disulfide (WS2) thin films by aerosol-assisted chem. vapor deposition (AACVD). When WS3L2 is used in conjunction with the previ-ously reported precursor, MoL4 which produces molybdenum disulfide (MoS2) by AACVD, alloyed thin films of the type Mo1-xWxS2 are produced. The W/Mo ratio can be controlled by changing the relative concns. of precursors in the carrier aerosol, allowing straightforward manipulation of the optical properties of the material and exquisite control of the final film compn.

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35. 35

    O’Brien, P.; Waters, J. Deposition of Ni and Pd Sulfide Thin Films via Aerosol-Assisted CVD. Chem. Vap. Deposition 2006, 12 (10), 620– 626,  DOI: 10.1002/cvde.200506387

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    Deposition of Ni and Pd sulfide thin films via aerosol-assisted CVD

    O'Brien, Paul; Waters, John

    Chemical Vapor Deposition (2006), 12 (10), 620-626CODEN: CVDEFX; ISSN:0948-1907. (Wiley-VCH Verlag GmbH & Co. KGaA)

    Thin films of Ni sulfide (NiS1.03, NiS2, α-Ni7S6, or mixts. thereof) and Pd sulfide (PdS, Pd16S7, Pd4S, or mixts. thereof) were prepd. by aerosol-assisted (AA)CVD using dithiocarbamate precursors M(S2CNRR')2 (M = Ni, Pd; RR' = Et2, MeEt, MeBu, or MenHex). The solid-state structure of Ni(S2CNMeBu)2, was detd. by x-ray single-crystal diffraction and is characteristic of known Ni dithiocarbamates. Films were grown on glass substrates at 400-525° and characterized by XRD, energy dispersive anal. of x-rays (EDAX), and SEM.

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36. 36

    Horley, G. A.; Lazell, M. R.; O’Brien, P. Deposition of Thin Films of Gallium Sulfide from a Novel Liquid Single-Source Precursor, Ga (SOCNEt2) 3, by Aerosol-Assisted CVD. Chem. Vap. Deposition 1999, 5 (5), 203– 205,  DOI: 10.1002/(SICI)1521-3862(199910)5:5<203::AID-CVDE203>3.0.CO;2-L

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    Deposition of thin films of gallium sulfide from a novel liquid single-source precursor, Ga(SOCNEt2)3, by aerosol-assisted CVD

    Horley, Graeme H.; Lazell, Mike R.; O'Brien, Paul

    Chemical Vapor Deposition (1999), 5 (5), 203-205CODEN: CVDEFX; ISSN:0948-1907. (Wiley-VCH Verlag GmbH)

    Thin films of fcc. GaS were grown by aerosol-assisted CVD on borosilicate glasses at 350° using Ga(SOCNEt2)3 as single-source precursor. The liq. monothiocarbamato precursor was prepd. from a toluene suspension of Na(SOCNEt2) which was added to a hexane soln. of GaCl3 followed by stirring at room temp. for 4 h. The GaS films were analyzed by XRD, SEM with EDAX, and XPS. The films were highly oriented showing an unusual spherical morphol. similar to that obsd. by Barron (1992, 1993).

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37. 37

    Kemmler, M.; Lazell, M.; O’Brien, P.; Otway, D.; Park, J.-H.; Walsh, J. The growth of thin films of copper chalcogenide films by MOCVD and AACVD using novel single-molecule precursors. J. Mater. Sci.: Mater. Electron. 2002, 13 (9), 531– 535,  DOI: 10.1023/A:1019665428255

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    37

    The growth of thin films of copper chalcogenide films by MOCVD and AACVD using novel single-molecule precursors

    Kemmler, M.; Lazell, M.; O'Brien, P.; Otway, D. J.; Park, Jin-Ho; Walsh, J. R.

    Journal of Materials Science: Materials in Electronics (2002), 13 (9), 531-535CODEN: JSMEEV; ISSN:0957-4522. (Kluwer Academic Publishers)

    Highly oriented cryst. films of copper sulfide and copper selenide have been grown on glass by low-pressure metal-org. chem. vapor deposition (LP-MOCVD) and by aerosol-assisted chem. vapor deposition (AACVD), using the air-stable compds. [Cu(E2CNMenHex)2]* (where E=S,Se). Thin films of non-stoichiometric cubic CuS and CuSe have been deposited in the temp. range 450-500 °C.

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38. 38

    Haggata, S.; Malik, M. A.; Motevalli, M.; O’Brien, P.; Knowles, J. Synthesis and Characterization of Some Mixed Alkyl Thiocarbamates of Gallium and Indium, Precursors for III/VI Materials: The X-ray Single-Crystal Structures of Dimethyl-and Diethylindium Diethyldithiocarbamate. Chem. Mater. 1995, 7 (4), 716– 724,  DOI: 10.1021/cm00052a017

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    38

    Synthesis and Characterization of Some Mixed Alkyl Thiocarbamates of Gallium and Indium, Precursors for III/VI Materials: The X-ray Single-Crystal Structures of Dimethyl- and Diethylindium Diethyldithiocarbamate

    Haggata, S. W.; Malik, M. Azad; Motevalli, M.; O'Brien, P.; Knowles, J. C.

    Chemistry of Materials (1995), 7 (4), 716-24CODEN: CMATEX; ISSN:0897-4756. (American Chemical Society)

    Mixed alkyl/dithiocarbamates R2MS2CNEt2 (M = In or Ga and R = Me, Et, or neopentyl) were prepd. and characterized. The In complexes are well-defined cryst. solids, and x-ray single-crystal structures are reported for the Me and Et compds. Both compds. have S2C2 coordination at In, and all bond lengths and angles are in the normal range. The Ga complexes are all liqs. The In compds. were used to successfully deposit thin films of various phases of InxSy by low-pressure MOCVD onto GaAs(100) substrates. The Me complex deposits orthorhombic InS39 and monoclinic In6S739 phases between 425 and 400°; growth at 325° resulted in the cubic β-In2S3 phase. But the Et compd. deposits monophasic β-In2S3 over the 400-350°, the neopentyl In compd. deposits In6S7 at 400 and 375° with the presence of a small amt. of the β-In2S3. Preliminary results of deposition expts. with the Ga precursors were less successful, and only very thin films were grown.

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39. 39

    Nyamen, L. D.; Revaprasadu, N.; Pullabhotla, R. V.; Nejo, A. A.; Ndifon, P. T.; Malik, M. A.; O’Brien, P. Synthesis of multi-podal CdS nanostructures using heterocyclic dithiocarbamato complexes as precursors. Polyhedron 2013, 56, 62– 70,  DOI: 10.1016/j.poly.2013.03.027

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    Synthesis of multi-podal CdS nanostructures using heterocyclic dithiocarbamato complexes as precursors

    Nyamen, Linda D.; Revaprasadu, Neerish; Pullabhotla, Rajasekhar V. S. R.; Nejo, Adeola A.; Ndifon, Peter T.; Malik, Mohammad Azad; O'Brien, Paul

    Polyhedron (2013), 56 (), 62-70CODEN: PLYHDE; ISSN:0277-5387. (Elsevier Ltd.)

    Bis(dipiperidinyldithiocarbamato)cadmium(II) (1) and bis(ditetrahydroquinolinyldithio-carbamato)cadmium(II) (2) were used as precursors for the synthesis of oleylamine (OA), decylamine (DA) and dodecylamine (DDA) capped CdS nanoparticles. The optical properties of these particles were studied. The absorption spectra for the amine capped CdS particles are blue shifted in relation to the bulk material. The corresponding photoluminescence spectra show a narrow band edge emission. High quality cryst. CdS particles of different shapes, ranging from short nanorods and elongated nanorods (rods, bipods, tripods and tetrapods) to nanocubes were obtained when the reaction temp. was varied between 180 and 270°. A decrease in the length of the rods and bipodal nanoparticles was obsd. with an increase in the length of the chain of the amine (capping agent) used. The p-XRD patterns revealed the hexagonal phase of CdS to be dominant in all the samples. IR studies suggest that the mode of bonding of the amines (oleylamine, decylamine and dodecylamine) on the CdS nanoparticle surfaces is through electron donation from the nitrogen atoms.

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40. 40

    Garg, B.; Garg, R.; Reddy, M. Synthesis and spectral characterization of zinc (II), cadmium (II) and mercury (II) with tetrahydroquinoline and isoquinoline dithiocarbamates. Indian J. Chem. 1993, 32A, 697– 700

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    Synthesis and spectral characterization of zinc(II), cadmium(II) and mercury(II) with tetrahydroquinoline and tetrahydroisoquinoline dithiocarbamates

    Garg, B. S.; Garg, R. K.; Reddy, M. J.

    Indian Journal of Chemistry, Section A: Inorganic, Bio-inorganic, Physical, Theoretical & Analytical Chemistry (1993), 32A (8), 697-700CODEN: ICACEC; ISSN:0376-4710.

    A few complexes of Zn(II), Cd(II) and Hg(II), ML2, with 2 new heterocyclic ligands viz. tetrahydroquinoline and tetrahydroisoquinoline dithiocarbamates were synthesized and characterized from elemental anal., IR, UV-visible, 1H NMR spectra, x-ray powder diffraction and TG-DTA studies. The IR and 1H NMR data showed that the ligands behave as isobidentate ones. The electronic spectra show that mostly ligand centered charge transfer transitions occur. In thermal studies, interesting fragmentation patterns are reported and kinetic parameters such as order of the thermal reactions (n) and activation energy (Ea) also were evaluated.

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41. 41

    O’Brien, P.; Nomura, R. Single-molecule precursor chemistry for the deposition of chalcogenide (S or Se)-containing compound semiconductors by MOCVD and related methods. J. Mater. Chem. 1995, 5 (11), 1761– 1773,  DOI: 10.1039/jm9950501761

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    Single-molecule precursor chemistry for the deposition of chalcogenide(S or Se)-containing compound semiconductors by MOCVD and related methods

    O'Brien, Paul; Nomura, Ryoki

    Journal of Materials Chemistry (1995), 5 (11), 1761-73CODEN: JMACEP; ISSN:0959-9428. (Royal Society of Chemistry)

    A review with 146 refs. of recent development in the deposition of II-VI and III-VI compd. semiconductors by MOCVD methods using single-compd. precursors is presented. The use of such precursors is placed in the context of the potential technol. importance of these materials and relevant aspects of conventional MOCVD.

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42. 42

    Zeng, N. T.; Hopkinson, D. G.; Spencer, B. F.; McAdams, S. G.; Tedstone, A. A.; Haigh, S. J.; Lewis, D. J. Direct synthesis of MoS₂ or MoO₃ via thermolysis of a dialkyl dithiocarbamato molybdenum(IV) complex. Chem. Commun. 2019, 55 (1), 99– 102,  DOI: 10.1039/C8CC08932A

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    Direct synthesis of MoS2 or MoO3 via thermolysis of a dialkyl dithiocarbamato molybdenum(IV) complex

    Zeng, Niting; Hopkinson, David G.; Spencer, Ben F.; McAdams, Simon G.; Tedstone, Aleksander A.; Haigh, Sarah J.; Lewis, David J.

    Chemical Communications (Cambridge, United Kingdom) (2019), 55 (1), 99-102CODEN: CHCOFS; ISSN:1359-7345. (Royal Society of Chemistry)

    Direct synthesis of either 2H-MoS2 or α-MoO3 is made possible by thermolysis of the same single source precursor in either argon or air at moderate temps.

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    https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC1cXitlOktLrK&md5=011245df1afb8a38648eb588111f0c25
43. 43

    Higgins, E. P. C.; McAdams, S. G.; Hopkinson, D. G.; Byrne, C.; Walton, A. S.; Lewis, D. J.; Dryfe, R. A. W. Room-Temperature Production of Nanocrystalline Molybdenum Disulfide (MoS₂) at the Liquid-Liquid Interface. Chem. Mater. 2019, 31 (15), 5384– 5391,  DOI: 10.1021/acs.chemmater.8b05232

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    43

    Room-Temperature Production of Nanocrystalline Molybdenum Disulfide (MoS2) at the Liquid-Liquid Interface

    Higgins, Eliott P. C.; McAdams, Simon G.; Hopkinson, David G.; Byrne, Conor; Walton, Alex S.; Lewis, David J.; Dryfe, Robert A. W.

    Chemistry of Materials (2019), 31 (15), 5384-5391CODEN: CMATEX; ISSN:0897-4756. (American Chemical Society)

    Scalable synthesis of 2D materials is a prerequisite for their com. exploitation. Here, a novel method of producing nanocryst. MoS2 at the liq.-liq. interface is demonstrated by decompg. a mol. precursor (tetrakis(N,N-diethyldithiocarbamato) Mo(IV)) in an org. solvent. The decompn. occurs over a few hours at room temp. without stirring or the addn. of any surfactants, producing MoS2 which can be isolated onto substrates of choice. The formation of MoS2 at the liq.-liq. interface can be accelerated by the inclusion of hydroxide ions in the aq. phase, which we propose to act as a catalyst. The precursor concn. was varied to minimize MoS2 thickness, and the org. solvent was chosen to optimize the speed and quality of formation. The kinetics of the MoS2 formation was studied, and a reaction mechanism is proposed. The synthesis method is, to the best of our knowledge, the 1st reported room-temp. synthesis of transition-metal dichalcogenides, offering a potential soln. to scalable 2D material prodn.

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44. 44

    Lee, W. Y.; Besmann, T. M.; Stott, M. W. Preparation of MoS 2 thin films by chemical vapor deposition. J. Mater. Res. 1994, 9 (6), 1474– 1483,  DOI: 10.1557/JMR.1994.1474

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    Preparation of MoS2 thin films by chemical vapor deposition

    Lee, Woo Y.; Besmann, Theodore M.; Stott, Michael W.

    Journal of Materials Research (1994), 9 (6), 1474-83CODEN: JMREEE; ISSN:0884-2914.

    The chem. vapor deposition (CVD) of MoS2 by reaction of H2S with Mo halides was detd. to be thermodynamically favored over a wide range of temp., pressure, and precursor concn. conditions as long as excess H2S was available. The thermochem. stability of H2S, MoF6, and MoCl5 was also assessed to address their suitability as precursors for the CVD of MoS2. The results from the thermodn. anal. were used as guidance in the deposition of MoS2 thin films from MoF6 and H2S. The (002) basal planes of MoS2 films deposited above 700 K were preferentially oriented perpendicular to the substrate surface.

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    https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADyaK2cXks12rtL8%253D&md5=eecc5c3e548d12f4eaa7973db0827416
45. 45

    Tyagi, S.; Kumar, A.; Kumar, M.; Singh, B. P. Large area vertical aligned MoS2 layers toward the application of thin film transistor. Mater. Lett. 2019, 250, 64– 67,  DOI: 10.1016/j.matlet.2019.04.117

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    Large area vertical aligned MoS2 layers toward the application of thin film transistor

    Tyagi, Shrestha; Kumar, Ashwani; Kumar, Manoj; Singh, Beer Pal

    Materials Letters (2019), 250 (), 64-67CODEN: MLETDJ; ISSN:0167-577X. (Elsevier B.V.)

    The current study investigates the fabrication of semiconducting molybdenum disulfide thin film using reactive magnetron sputtering technique at 300 °C for thin film transistors (TFTs) application. X-ray diffraction (XRD), Raman spectroscopy, XPS and Field emission-SEM (FE-SEM) techniques were used to identify the structural, elemental compositional and morphol. properties of the synthesized thin film. XRD and Raman data confirm the growth of hexagonal structure and FE-SEM images indicate the vertical aligned layered morphol. The fabricated TFT demonstrates excellent performance in terms of field-effect mobility of 24.17 cm2 V-1 s-1 and a high Ion/Ioff ratio of the order of 106.

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46. 46

    Li, S.; Lee, J. K.; Zhou, S.; Pasta, M.; Warner, J. H. Synthesis of Surface Grown Pt Nanoparticles on Edge-Enriched MoS2 Porous Thin Films for Enhancing Electrochemical Performance. Chem. Mater. 2019, 31 (2), 387– 397,  DOI: 10.1021/acs.chemmater.8b03540

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    46

    Synthesis of Surface Grown Pt Nanoparticles on Edge-Enriched MoS2 Porous Thin Films for Enhancing Electrochemical Performance

    Li, Sha; Lee, Ja Kyung; Zhou, Si; Pasta, Mauro; Warner, Jamie H.

    Chemistry of Materials (2019), 31 (2), 387-397CODEN: CMATEX; ISSN:0897-4756. (American Chemical Society)

    A hybrid catalyst - Pt nanocrystals deposited on the surface of MoS2 vertically standing nanoplatelets was synthesized via CVD and subsequent thermal annealing (TA) of Pt precursor. The hybrid material shows promising results as an electrocatalyst for the H evolution reaction (HER). By varying Pt synthesis condition - precursor loading and TA temp. - the deposition sites, size and morphol. of Pt nanostructure can be controlled. The size effect of Pt nanoparticle on catalytic activity and sintering resistance is discussed. Higher Pt loading yields better HER performance despite of smaller sp. surface area; higher TA temp. delivers larger av. particle size of Pt crystals and lower HER activity. Larger av. size leads to fast sintering and thus poor durability of the catalyst. Based on the correlation between HER performance and growth behaviors of Pt on MoS2 surfaces, optimization route for a highly active and stable cocatalyst can be established. The optimized Pt-MoS2 catalyst (400°, 11%) reported in this study possesses superior overpotential of 9 mV (close to zero), Tafel slope of 44 mV/dec and moderate exchange c.d. of 373 μA/cm2; it exhibits activity degrdn. of 140 mV @ 20 mA/cm2 after 10,000 cycles. The Tafel slope indicates the combination of Volmer-Heyrovsky steps as HER mechanism in this particular hybrid catalyst system. The outstanding HER activity attributes to highly dispersed Pt nanoparticles grown on MoS2 basal surfaces, large MoS2 edge d. and Pt - S bonding effect induced activity improvement of MoS2 as well as 3-dimensional porous network assisted superaerophobic surface.

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    https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC1MXjtVKjsw%253D%253D&md5=6da208743a4b0c10b1668edd509d7158
47. 47

    Adeogun, A.; Afzaal, M.; O’Brien, P. Studies of Molybdenum Disulfide Nanostructures Prepared by AACVD Using Single-Source Precursors. Chem. Vap. Deposition 2006, 12 (10), 597– 599,  DOI: 10.1002/cvde.200504203

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    Studies of molybdenum disulfide nanostructures prepared by AACVD using single-source precursors

    Adeogun, Adekunle; Afzaal, Mohammad; O'Brien, Paul

    Chemical Vapor Deposition (2006), 12 (10), 597-599CODEN: CVDEFX; ISSN:0948-1907. (Wiley-VCH Verlag GmbH & Co. KGaA)

    Nanostructures of hexagonal MoS2 thin films synthesized using air-stable, single-source mol. precursors of molybdenum dithiocarbamates [Mo(S2CNR2)4] (R = Et, nBu) are reported. On increasing the length of the substituent alkyl groups of the precursor, changes in the type of structures grown under similar growth conditions can be obsd.

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    https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BD28XhtFyrt7bN&md5=7d6d213df0ad40c6e75c14b8c6f53445
48. 48

    Zhao, H.; Mu, X.; Zheng, C.; Liu, S.; Zhu, Y.; Gao, X.; Wu, T. Structural defects in 2D MoS2 nanosheets and their roles in the adsorption of airborne elemental mercury. J. Hazard. Mater. 2019, 366, 240– 249,  DOI: 10.1016/j.jhazmat.2018.11.107

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    Structural defects in 2D MoS2 nanosheets and their roles in the adsorption of airborne elemental mercury

    Zhao, Haitao; Mu, Xueliang; Zheng, Chenghang; Liu, Shaojun; Zhu, Yanqiu; Gao, Xiang; Wu, Tao

    Journal of Hazardous Materials (2019), 366 (), 240-249CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)

    Here, ab initio calcns. and exptl. approach were adopted to reveal the mechanism of Hg0 adsorption on MoS2 nanosheets that contain various types of defects. The ab initio calcn. showed that, among different structural defects, S vacancies (Vs) in the MoS2 nanosheets exhibited outstanding potential to strongly adsorb Hg0. The MoS2 material was then prepd. in a controlled manner under conditions, such as temp., concn. of precursors, etc., that were detd. by adopting the new method developed here. Characterization confirmed that the MoS2 material is of graphene-like layered structure with abundant structural defects. The integrated dynamic and steady state (IDSS) testing demonstrated that the Vs-rich nanosheets showed excellent Hg0 adsorption capability. Ab initial calcn. on charge d. difference, PDOS, and adsorption pathways revealed that the adsorption of Hg0 on the Vs-rich MoS2 surface is non-activated chemisorption.

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49. 49

    Savjani, N.; Lewis, E. A.; Bissett, M. A.; Brent, J. R.; Dryfe, R. A.; Haigh, S. J.; O’Brien, P. Synthesis of Lateral Size-Controlled Monolayer 1 [email protected] Oleylamine as Supercapacitor Electrodes. Chem. Mater. 2016, 28 (2), 657– 664,  DOI: 10.1021/acs.chemmater.5b04476

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    49

    Synthesis of Lateral Size-Controlled Monolayer [email protected] as Supercapacitor Electrodes

    Savjani, Nicky; Lewis, Edward A.; Bissett, Mark A.; Brent, Jack R.; Dryfe, Robert A. W.; Haigh, Sarah J.; O'Brien, Paul

    Chemistry of Materials (2016), 28 (2), 657-664CODEN: CMATEX; ISSN:0897-4756. (American Chemical Society)

    A new wet chem. approach, based on the hot injection-thermolytic decompn. of the single-source precursor [Mo2O2S2(S2COEt)2] in oleylamine, is described for the prodn. of nano-dimensional [email protected] High quality freestanding MoS2 nanosheets capped with oleylamine have been prepd. and subjected to detailed compositional analyses for the 1st time. The selection of the appropriate reaction temps. (200-325°) in the simple yet robust procedure allows control of the lateral nanosheet dimensions which range from 4.5 to 11.5 nm, as [email protected] entities which maintain a consistent chem. compn. (MoS2·oleylamine0.28-0.33). This work provides the 1st example of at. resoln. STEM imaging of these fine-scale nanosheet materials, providing new insights into their morphol. and demonstrating that those freestanding MoS2 nanosheets are pure, highly cryst., randomly oriented monolayers. The [email protected] samples were analyzed by attenuated total reflectance FTIR spectroscopy (ATR-FTIR), transmission electron microscope (TEM) imaging, aberration cor. scanning transmission electron microscope (STEM) imaging, energy dispersive x-ray (EDX) spectrum imaging, powder X-ray diffractometry (p-XRD), TGA, and Raman spectroscopy. Composite materials of the as-synthesized MoS2 nanosheets and exfoliated graphene were then used to construct coin-cell supercapacitor electrodes with a specific capacitance of 50 mF/cm2, demonstrating its utility as an energy storage material.

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50. 50

    Su, D.; Dou, S.; Wang, G. Ultrathin MoS2 Nanosheets as Anode Materials for Sodium-Ion Batteries with Superior Performance. Adv. Energy Mater. 2015, 5 (6), 1401205,  DOI: 10.1002/aenm.201401205

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    Ultrathin MoS2 Nanosheets as Anode Materials for Sodium-Ion Batteries with Superior Performance

    Su, Dawei; Dou, Shixue; Wang, Guoxiu

    Advanced Energy Materials (2015), 5 (6), 1401205/1-1401205/6CODEN: ADEMBC; ISSN:1614-6840. (Wiley-Blackwell)

    Few-layer MoS2 nanosheets are successfully synthesized using a simple and scalable ultrasonic exfoliation technique. The thicknesses of the MoS2 nanosheets ares about 10 nm as measured by SEM (SEM) and at. force microscopy (AFM). The unique nanosheet architecture renders the high-rate transportation of sodium ions due to the short diffusion paths provided by ultrathin thickness and the large interlayer space within the MoS2 crystal structure (d(002) = 6.38 Å). When applied as anode materials in sodium-ion batteries, MoS2 nanosheets exhibit a high, reversible sodium storage capacity and excellent cyclability. The MoS2 nanosheets also demonstrate good electrochem. performance at high current densities.

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51. 51

    Tedstone, A. A.; Lewis, D. J.; Hao, R.; Mao, S. M.; Bellon, P.; Averback, R. S.; Warrens, C. P.; West, K. R.; Howard, P.; Gaemers, S.; Dillon, S. J.; O’Brien, P. Mechanical Properties of Molybdenum Disulfide and the Effect of Doping: An in Situ TEM Study. ACS Appl. Mater. Interfaces 2015, 7 (37), 20829– 20834,  DOI: 10.1021/acsami.5b06055

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    Mechanical Properties of Molybdenum Disulfide and the Effect of Doping: An in Situ TEM Study

    Tedstone, Aleksander A.; Lewis, David J.; Hao, Rui; Mao, Shi-Min; Bellon, Pascal; Averback, Robert S.; Warrens, Christopher P.; West, Kevin R.; Howard, Philip; Gaemers, Sander; Dillon, Shen J.; O'Brien, Paul

    ACS Applied Materials & Interfaces (2015), 7 (37), 20829-20834CODEN: AAMICK; ISSN:1944-8244. (American Chemical Society)

    Direct observations on nanopillars composed of molybdenum disulfide (MoS2) and chromium-doped MoS2 and their response to compressive stress have been made. Time-resolved transmission electron microscopy (TEM) during compression of the submicrometer diam. pillars of MoS2- and Cr-doped MoS2 (Cr: 0, 10, and 50 at %) allow the deformation process of the material to be obsd. and can be directly correlated with mech. response to applied load. The addn. of chromium to the MoS2 changed the failure mode from plastic deformation to catastrophic brittle fracture, an effect that was more pronounced as chromium content increased.

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    Singh, R. C.; Singh, M. P.; Singh, O.; Chandi, P. S. Influence of synthesis and calcination temperatures on particle size and ethanol sensing behaviour of chemically synthesized SnO₂ nanostructures. Sens. Actuators, B 2009, 143 (1), 226– 232,  DOI: 10.1016/j.snb.2009.09.032

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    Influence of synthesis and calcination temperatures on particle size and ethanol sensing behavior of chemically synthesized SnO2 nanostructures

    Singh, Ravi Chand; Singh, Manmeet Pal; Singh, Onkar; Chandi, Paramdeep Singh

    Sensors and Actuators, B: Chemical (2009), B143 (1), 226-232CODEN: SABCEB; ISSN:0925-4005. (Elsevier B.V.)

    Nanoparticles of SnO2 were prepd. through chem. route at 5, 25, and 50°. The particles were calcined at 400, 600, and 800° and their structural and morphol. anal. was carried out using x-ray diffraction and TEM. The reaction temp. was found to be playing a crit. role in controlling nanostructure sizes as well as agglomeration. That particles prepd. at 5 and 50° were smaller and less agglomerated as compared to the particles prepd. at 25°. The study also reveals that particle size and agglomeration increases with increase in calcination temp. Thick film gas sensors were fabricated using SnO2 powder, and sensing response of all the sensors to ethanol vapors was investigated at different temps. The investigations reveal that sensing response of SnO2 nanoparticles is size dependent and smaller particles are highly sensitive.

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53. 53

    Wolden, C. A.; Kurtin, J.; Baxter, J. B.; Repins, I.; Shaheen, S. E.; Torvik, J. T.; Rockett, A. A.; Fthenakis, V. M.; Aydil, E. S. Photovoltaic manufacturing: Present status, future prospects, and research needs. J. Vac. Sci. Technol., A 2011, 29 (3), 030801,  DOI: 10.1116/1.3569757

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    Photovoltaic manufacturing: Present status, future prospects, and research needs

    Wolden, Colin A.; Kurtin, Juanita; Baxter, Jason B.; Repins, Ingrid; Shaheen, Sean E.; Torvik, John T.; Rockett, Angus A.; Fthenakis, Vasilis M.; Aydil, Eray S.

    Journal of Vacuum Science & Technology, A: Vacuum, Surfaces, and Films (2011), 29 (3), 030801/1-030801/16CODEN: JVTAD6; ISSN:0734-2101. (American Institute of Physics)

    A review. In May 2010 the United States National Science Foundation sponsored a two-day workshop to review the state-of-the-art and research challenges in photovoltaic (PV) manufg. This article summarizes the major conclusions and outcomes from this workshop, which was focused on identifying the science that needs to be done to help accelerate PV manufg. A significant portion of the article focuses on assessing the current status of and future opportunities in the major PV manufg. technologies. These are solar cells based on cryst. silicon (c-Si), thin films of cadmium telluride (CdTe), thin films of copper indium gallium diselenide, and thin films of hydrogenated amorphous and nanocryst. silicon. Current trends indicate that the cost per W of c-Si and CdTe solar cells are being reduced to levels beyond the constraints commonly assocd. with these technologies. With a focus on TW/yr prodn. capacity, the issue of material availability is discussed along with the emerging technologies of dye-sensitized solar cells and org. photovoltaics that are potentially less constrained by elemental abundance. Lastly, recommendations are made for research investment, with an emphasis on those areas that are expected to have cross-cutting impact. (c) 2011 American Institute of Physics.

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    Zakutayev, A. Brief review of emerging photovoltaic absorbers. Current Opinion in Green and Sustainable Chemistry 2017, 4, 8– 15,  DOI: 10.1016/j.cogsc.2017.01.002

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    Austin, I.; Goodman, C.; Pengelly, A. New semiconductors with the chalcopyrite structure. J. Electrochem. Soc. 1956, 103 (11), 609– 610,  DOI: 10.1149/1.2430171

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    New semiconductors with chalcopyrite structure

    Austin, I. G.; Goodman, C. H. L.; Pengelly, A. E.

    Journal of the Electrochemical Society (1956), 103 (), 609-10CODEN: JESOAN; ISSN:0013-4651.

    cf. C.A. 51, 70c. Compds. of the chalcopyrite group are related to well-known semiconductors such as Ge and the zinc blende compds. This relation is discussed and some new data are presented regarding the prepn. and properties of 5 chalcopyrite compds., AgInS2, AgInSe2, CuInSe2, AgInTe2, and CuInTe2.

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    Kondo, K. i.; Teranishi, T.; Sato, K. Optical Absorption of CuFeS₂ and Fe-Doped CuAlS₂ and CuGaS₂. J. Phys. Soc. Jpn. 1974, 36 (1), 311– 311,  DOI: 10.1143/JPSJ.36.311

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    Optical absorption of copper iron sulfide (CuFeS2) and iron-doped copper aluminum sulfide (CuAlS2) and copper gallium sulfide (CuGaS2)

    Kondo, Ken'ichi; Teranishi, Teruo; Sato, Katsuaki

    Journal of the Physical Society of Japan (1974), 36 (1), 311CODEN: JUPSAU; ISSN:0031-9015.

    Strong absorption bands of CuAl1-xFexS2 at 1.3 eV and 2.0 eV and of CuGa1-xFexS2 at 1.2 eV and 1.9 eV are not related to the presence of Cu ions and originate from Fe3+ ions. The large value of oscillator strength (∼7 × 10-2) suggests that these absorptions arise not from the d-d transition, but from the charge-transfer transitions relating to Fe3+. It is highly probable that the absorption edge of CuFeS2 at ∼0.6 eV is the foot of the corresponding transition.

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    Barkat, L.; Hamdadou, N.; Morsli, M.; Khelil, A.; Bernede, J. 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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    Korzun, B.; Galyas, A. Thin Films of CuFeS₂ Prepared by Flash Evaporation Technique and Their Structural Properties. J. Electron. Mater. 2019, 48 (5), 3351– 3354,  DOI: 10.1007/s11664-019-07005-z

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    Thin Films of CuFeS2 Prepared by Flash Evaporation Technique and Their Structural Properties

    Korzun, Barys; Galyas, Anatoly

    Journal of Electronic Materials (2019), 48 (5), 3351-3354CODEN: JECMA5; ISSN:0361-5235. (Springer)

    Thin films of chalcopyrite CuFeS2 were deposited on glass substrates by flash evapn. The resulting film structure was analyzed by SEM (SEM) combined with energy dispersive x-ray spectroscopy (EDS). It was detected that the thin films consist of sep. grains of almost equal areas of about (200-400) μm2. The thin films of chalcopyrite CuFeS2 have chem. compn. with an at. content of Cu, Fe, and S of 25.22 at.%, 23.38 at.%, and 51.40 at.% and at. ratios of Cu/Fe and S/(Cu + Fe) equal to 1.08 and 1.06, resp., which slightly differ from the theor. values equal to 1 for both at. ratios. A small inclusion of the second phase with chem. compn. with the at. content of Cu, Fe, and S of 29.24 at.%, 25.24 at.%, and 45.52 at.% was detected and can be attributed to talnakhite Cu9Fe8S16. The obsd. cracking of the thin films is explained by the sepn. of the addnl. phase with the structure of chalcocite Cu2S, which occurs during cooling of the thin films.

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59. 59

    Prabukanthan, P.; Thamaraiselvi, S.; Harichandran, G.; Theerthagiri, J. Single-step electrochemical deposition of Mn²⁺ doped FeS₂ thin films on ITO conducting glass substrates: Physical, electrochemical and electrocatalytic properties. J. Mater. Sci.: Mater. Electron. 2019, 30 (4), 3268– 3276,  DOI: 10.1007/s10854-018-00599-w

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    Single-step electrochemical deposition of Mn2+ doped FeS2 thin films on ITO conducting glass substrates: physical, electrochemical and electrocatalytic properties

    Prabukanthan, P.; Thamaraiselvi, S.; Harichandran, G.; Theerthagiri, J.

    Journal of Materials Science: Materials in Electronics (2019), 30 (4), 3268-3276CODEN: JSMEEV; ISSN:0957-4522. (Springer)

    Mn2+ doped FeS2 thin films were deposited on ITO coated conducting glass substrate at 50 °C in an aq. medium by simple electrochem. deposition technique. The structural and phase purity of the Mn2+ doped FeS2 thin films were investigated using XRD technique. The XRD anal. revelaed that the fabricated thin films were cubic structure along with the (200) plane preferential orientation. The diffraction peak slightly shifted towards lower 2θ values which confirmed that doping of Mn ions into FeS2 host matrixes. The calcd. band gap energy of Mn2+ doped FeS2 thin films showed a red shift of absorption edge compared to undoped FeS2 thin film. EIS indicated that Mn2+ doped FeS2 thin films showed lower charge transfer resistance with better cond. nature compared to undoped sample. Moreover, the photo electrochem. measurements carried out for the optimized Mn2+ doped FeS2 thin film which revealed the faster migration of photo-induced charge-carriers. Electro catalytic activity of Mn-doped FeS2 thin films were studied for the redox reaction of iodide/triiodide (I-/I3-) by using cyclic voltammetry measurement.

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60. 60

    Tonpe, D.; Gattu, K.; More, G.; Upadhye, D.; Mahajan, S.; Sharma, R. In Synthesis of CuFeS₂ Thin Films from Acidic Chemical Baths, AIP Conference Proceedings; AIP Publishing, 2016; p 020676.

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    Aup-Ngoen, K.; Thongtem, T.; Thongtem, S.; Phuruangrat, A. Cyclic microwave-assisted synthesis of CuFeS2 nanoparticles using biomolecules as sources of sulfur and complexing agent. Mater. Lett. 2013, 101, 9– 12,  DOI: 10.1016/j.matlet.2013.03.055

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    Cyclic microwave-assisted synthesis of CuFeS2 nanoparticles using biomolecules as sources of sulfur and complexing agent

    Aup-Ngoen, Kamonwan; Thongtem, Titipun; Thongtem, Somchai; Phuruangrat, Anukorn

    Materials Letters (2013), 101 (), 9-12CODEN: MLETDJ; ISSN:0167-577X. (Elsevier B.V.)

    CuFeS2 nanoparticles were prepd. by a 300 W cyclic microwave radiation, exposing onto ethylene glycol contg. Cu(CH3COO)2, FeCl3.·6H2O or FeCl2.4H2O and L-cysteine biomols. X-ray diffraction (XRD), field emission SEM (FE-SEM), TEM, Raman spectrometry, and XPS revealed the presence of pure tetragonal chalcopyrite CuFeS2 nanoparticles with valence states of Cu+, Fe3+, and S2- and four Raman shifts at 215.0-218.6, 280.2-281.4, 394.4-394.9, and 472.2-473.4 cm-1. A formation mechanism of the products was also proposed according to the exptl. results.

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    Ito, K.; Nakazawa, T. Electrical and optical properties of stannite-type quaternary semiconductor thin films. Jpn. J. Appl. Phys. 1988, 27 (11R), 2094,  DOI: 10.1143/JJAP.27.2094

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    Electrical and optical properties of stannite-type quaternary semiconductor thin films

    Ito, Kentaro; Nakazawa, Tatsuo

    Japanese Journal of Applied Physics, Part 1: Regular Papers, Short Notes & Review Papers (1988), 27 (11), 2094-7CODEN: JAPNDE; ISSN:0021-4922.

    Quaternary stannite-type semiconductor films of Cu2CdSnS4 and Cu2ZnSnS4 with (112) orientation were deposited on heated glass substrates using atom beam sputtering. These p-type films showed resistivities which were decreasing functions of the substrate temp. up to 240°. The films had an absorption coeff. >1 × 104 cm-1 in the visible wavelength range. The direct optical band gaps of the (112)-oriented polycryst. films were estd. as 1.06 and 1.45 eV for Cu2CdSnS4 and Cu2ZnSnS4, resp.

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63. 63

    Shi, C.; Shi, G.; Chen, Z.; Yang, P.; Yao, M. Deposition of Cu2ZnSnS4 thin films by vacuum thermal evaporation from single quaternary compound source. Mater. Lett. 2012, 73, 89– 91,  DOI: 10.1016/j.matlet.2012.01.018

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    Deposition of Cu2ZnSnS4 thin films by vacuum thermal evaporation from single quaternary compound source

    Shi, Chengwu; Shi, Gaoyang; Chen, Zhu; Yang, Pengfei; Yao, Min

    Materials Letters (2012), 73 (), 89-91CODEN: MLETDJ; ISSN:0167-577X. (Elsevier B.V.)

    Cu2ZnSnS4 (CZTS) thin films were successfully deposited using vacuum thermal evapn. from single quaternary CZTS semiconducting material powder source, followed by annealing at 300° for 40 min under high purity N2 atmosphere. X-ray diffraction (XRD) patterns indicated that as-deposited CZTS thin films transformed from amorphous state into cryst. state with kesterite structure after annealing. Energy dispersive x-ray spectroscopy (EDS) detd. the compns. of the CZTS thin films were Zn-poor, Sn-rich, and S-rich. Scanning electron microscope (SEM) images, UV-visible-near IR (UV-Vis-NIR) spectra and the Hall measurements showed the annealed CZTS thin film exhibited a smooth, densely packed and homogeneous surface, a direct band gap of 1.55 eV and a p-type cond. The fabricated photovoltaic device obtained a conversion efficiency of 0.36%, open-circuit voltage of 493 mV, short-circuit c.d. of 1.76 mA·cm- 2, and fill factor of 0.42.

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64. 64

    Vanalakar, S.; Agawane, G.; Shin, S. W.; Suryawanshi, M.; Gurav, K.; Jeon, K.; Patil, P.; Jeong, C.; Kim, J.; Kim, J. A review on pulsed laser deposited CZTS thin films for solar cell applications. J. Alloys Compd. 2015, 619, 109– 121,  DOI: 10.1016/j.jallcom.2014.09.018

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    64

    A review on pulsed laser deposited CZTS thin films for solar cell applications

    Vanalakar, S. A.; Agawane, G. L.; Shin, S. W.; Suryawanshi, M. P.; Gurav, K. V.; Jeon, K. S.; Patil, P. S.; Jeong, C. W.; Kim, J. Y.; Kim, J. H.

    Journal of Alloys and Compounds (2015), 619 (), 109-121CODEN: JALCEU; ISSN:0925-8388. (Elsevier B.V.)

    A review. Cu2ZnSnS4; commonly abbreviated as CZTS is a promising material for low cost thin film solar cells, because of its suitable band gap energy of around 1.5 eV and large absorption coeff. of over 104 cm-1. All the constituents of this material are abundant in the earth's crust, and they are not toxic making it a smarter choice. Since 1996, after the initial success of the CZTS based solar cell (with its light to elec. conversion efficiency of 0.6%), significant progress in this research area has been achieved, esp. in the last five years. Now-a-days, the conversion efficiency of the CZTS thin film solar cell has improved to 12%. Over 600 papers on CZTS have been published since 2001, and the majority of these discuss the prepn. of CZTS thin films by different methods. So far, many phys. and chem. techniques have been employed for prepg. CZTS thin films. Among them, the pulsed laser deposition (PLD) is a versatile deposition method. PLD is a simple, but multipurpose, exptl. method that finds use as a means of modeling a very diverse range of materials, and in extensive areas of thin film deposition and multi-layer research. This technique is suitable for depositing high quality films with complex compns. because of its influencing properties such as harmonious transfer of species from the target to substrate, enrichment in crystallinity, clean deposition, and simplicity and flexibility in the engineering design. On the occasion of the 25th anniversary of PLD, this manuscript, reviews the synthesis of CZTS semiconductor thin films fabricated by PLD. This review begins with a description of the PLD system, and then introduces the CZTS and prepn. of the CZTS target for PLD deposition. A survey of pulsed laser deposited CZTS thin films and their solar cell performance is discussed in detail. Finally, we present perspectives for further developments of PLD for a CZTS based solar cell absorber layer.

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65. 65

    Araki, H.; Mikaduki, A.; Kubo, Y.; Sato, T.; Jimbo, K.; Maw, W. S.; Katagiri, H.; Yamazaki, M.; Oishi, K.; Takeuchi, A. Preparation of Cu₂ZnSnS₄ thin films by sulfurization of stacked metallic layers. Thin Solid Films 2008, 517 (4), 1457– 1460,  DOI: 10.1016/j.tsf.2008.09.058

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    65

    Preparation of Cu2ZnSnS4 thin films by sulfurization of stacked metallic layers

    Araki, Hideaki; Mikaduki, Aya; Kubo, Yuki; Sato, Tatsuhiro; Jimbo, Kazuo; Maw, Win Shwe; Katagiri, Hironori; Yamazaki, Makoto; Oishi, Koichiro; Takeuchi, Akiko

    Thin Solid Films (2008), 517 (4), 1457-1460CODEN: THSFAP; ISSN:0040-6090. (Elsevier B.V.)

    Stacked precursors of Cu, Sn, and Zn were fabricated on glass/Mo substrates by electron beam evapn. Six kinds of precursors with different stacking sequences were prepd. by sequential evapn. of Cu, Sn, and Zn with substrate heating. The precursors were sulfurized at temps. of 560° for 2 h in an atm. of N2 and sulfur vapor to fabricate Cu2ZnSnS4 thin films for solar cells. The sulfurized films exhibited x-ray diffraction peaks attributable to Cu2ZnSnS4. Solar cells using Cu2ZnSnS4 thin films prepd. from six kinds of precursors were fabricated. As a result, the solar cell using a Cu2ZnSnS4 thin film produced by sulfurization of the Mo/Zn/Cu/Sn precursor exhibited an open-circuit voltage of 478 mV, a short-circuit current of 9.78 mA/cm2, a fill factor of 0.38, and a conversion efficiency of 1.79%.

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66. 66

    Scragg, J. J.; Dale, P. J.; Peter, L. M. Towards sustainable materials for solar energy conversion: Preparation and photoelectrochemical characterization of Cu₂ZnSnS₄. Electrochem. Commun. 2008, 10 (4), 639– 642,  DOI: 10.1016/j.elecom.2008.02.008

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    Towards sustainable materials for solar energy conversion: Preparation and photoelectrochemical characterization of Cu2ZnSnS4

    Scragg, Jonathan J.; Dale, Phillip J.; Peter, Laurence M.

    Electrochemistry Communications (2008), 10 (4), 639-642CODEN: ECCMF9; ISSN:1388-2481. (Elsevier B.V.)

    The feasibility of a new fabrication route for films of the attractive solar absorber Cu2ZnSnS4 (CZTS) has been studied, consisting of electrodeposition of metallic precursors followed by annealing in sulfur vapor. Photoelectrochem. measurements using a Eu3+ contact have been used to establish that the polycryst. CZTS films are p-type with doping densities in the range (0.5-5) × 1016 cm-3 and band gaps of 1.49 ± 0.01 eV, making them suitable for terrestrial solar energy conversion. It has been shown that a somewhat Cu-poor compn. favors good optoelectronic properties.

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67. 67

    Olgar, M. A.; Tomakin, M.; Küçükömeroğlu, T.; Bacaksiz, E. Growth of Cu₂ZnSnS₄ (CZTS) thin films using short sulfurization periods. Mater. Res. Express 2019, 6, 056401,  DOI: 10.1088/2053-1591/aaff78

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    67

    Growth of Cu2ZnSnS4 (CZTS) thin films using short sulfurization periods

    Olgar, M. A.; Tomakin, M.; Kucukomeroglu, T.; Bacaksiz, E.

    Materials Research Express (2019), 6 (5), 056401CODEN: MREAC3; ISSN:2053-1591. (IOP Publishing Ltd.)

    In this study CZTS thin films were grown by a two-stage process that involved sequential sputter deposition of metallic Cu, Zn, and Sn layers on Mo coated glass substrates followed by RTP annealing at 530 and 560°C for various dwell times (1, 60, and 180 s). CZTS thin films obtained by reaction at different sulfurization temps. and reaction times were characterized employing XRD, Raman spectroscopy, SEM, EDX, and photoluminescence. It was obsd. that it is possible to obtain Cu-poor and Zn-rich CZTS thin films with short dwell time of reactions. XRD pattern and Raman spectra of the films showed formation of kesterite CZTS structure and some secondary phases such as CuS, SnS, SnS2. The full-width-at-half-max. (FWHM) values extd. from the (112) diffraction peaks of the CZTS thin films showed that extension of the sulfurization time provides better cryst. quality except for the CZTS560-60 thin film. SEM surface microstructure of the films displayed non-uniform, dense, and polycryst. structure. The optical band gap of the films as detd. by photoluminescence was found to be about 1.36-1.38 eV.

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68. 68

    Long, B.; Cheng, S.; Ye, D.; Yue, C.; Liao, J. Mechanistic aspects of preheating effects of precursors on characteristics of Cu₂ZnSnS₄ (CZTS) thin films and solar cells. Mater. Res. Bull. 2019, 115, 182– 190,  DOI: 10.1016/j.materresbull.2019.03.027

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    Mechanistic aspects of preheating effects of precursors on characteristics of Cu2ZnSnS4 (CZTS) thin films and solar cells

    Long, Bo; Cheng, Shuying; Ye, Dapeng; Yue, Chuang; Liao, Jie

    Materials Research Bulletin (2019), 115 (), 182-190CODEN: MRBUAC; ISSN:0025-5408. (Elsevier Ltd.)

    CZTS thin films are fabricated using sol-gel method following sulfurization. The material properties of the CZTS films which are prepd. under different preheating temps. and times are systematically investigated. The TGA-DTA anal. shows that the sulfides begin to be oxidized and the CZTS nanoparticles would be formed when the preheating temp. is above 300°C. Moreover, with increasing the preheating temp. and time, the crystallinity of the CZTS thin films becomes stronger firstly and then weaker. Morphol. characterizations show that the CZTS thin films deliver the best crystallinity under the preheating temp. of 250°C for 5 min. The Eg, resistivity, carrier concn., and mobility of the CZTS thin films is 1.45 eV, 3.56 Ω·cm, 2.47 × 1017 cm-3, 7.12 cm2·V-1·s-1, resp. The solar cells with the efficiency of 1.51% is successfully configured.

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69. 69

    Benachour, M.; Bensaha, R.; Moreno, R. Annealing duration influence on dip-coated CZTS thin films properties obtained by sol–gel method. Optik 2019, 187, 1– 8,  DOI: 10.1016/j.ijleo.2019.05.015

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    69

    Annealing duration influence on dip-coated CZTS thin films properties obtained by sol-gel method

    Benachour, M. C.; Bensaha, R.; Moreno, R.

    Optik (Munich, Germany) (2019), 187 (), 1-8CODEN: OTIKAJ; ISSN:0030-4026. (Elsevier GmbH)

    The effect of annealing duration on structural and optical properties of dip-coated cryst. CZTS thin films was studied. The obtained samples were investigated by several techniques such as XRD, Raman spectroscopy, SEM, UV-vis spectroscopy and Photoluminescence. Being confirmed by Raman spectroscopy, XRD anal. reveals the formation of kesterite tetragonal phase with preferential orientation along (112) direction. The grain size tends to increase as the annealing duration increases, a result confirmed by SEM. The last shows smooth, uniform, homogeneous and densely packed grains. Optical measurement anal. reveals that layers have relatively high absorption coeff. in the visible spectrum with a band gap redn. of 1.62-1.50 eV which is quite close to the optimum value for a solar cell. The photoluminescence distinguishes broad bands that have max. of intensity limited between 1.50 and 1.62 eV, corresponding to the optical band gap of the CZTS.

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70. 70

    Fernandes, P.; Salomé, P.; Da Cunha, A. Growth and Raman scattering characterization of Cu₂ZnSnS₄ thin films. Thin Solid Films 2009, 517 (7), 2519– 2523,  DOI: 10.1016/j.tsf.2008.11.031

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    Growth and Raman scattering characterization of Cu2ZnSnS4 thin films

    Fernandes, P. A.; Salome, P. M. P.; da Cunha, A. F.

    Thin Solid Films (2009), 517 (7), 2519-2523CODEN: THSFAP; ISSN:0040-6090. (Elsevier B.V.)

    The authors report the results of the growth, morphol. and structural characterization of Cu2ZnSnS4 (CZTS) thin films prepd. by sulfurization of d.c. magnetron sputtered Cu/Zn/Sn precursor layers. The adjustment of the thicknesses and the properties of the precursors were used to control the final compn. of the films. Its properties were studied by SEM/EDS, XRD and Raman scattering. The influence of the sulfurization temp. on the morphol., compn. and structure of the films was studied. With the presented method the authors were able to prep. CZTS thin films with the kesterite structure.

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