Solution-processed copper zinc tin sulfide thin films from metal xanthate precursors

Fischereder, Achim; Schenk, Alexander; Rath, Thomas; Haas, Wernfried; Delbos, Sébastien; Gougaud, Corentin; Naghavi, Negar; Pateter, Angelika; Saf, Robert; Schenk, Dorith; Edler, Michael; Bohnemann, Kathrin; Reichmann, Angelika; Chernev, Boril Stefanov; Hofer, Ferdinand; Trimmel, Gregor

doi:10.1007/s00706-012-0882-6

Cited by 28 publications

(27 citation statements)

References 65 publications

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“…p.a., Sigma-Aldrich), deuterated chloroform (CDCl 3 , 99.8 atom % D, VWR Chemicals), methanol (MeOH, puriss., C99.7%, Sigma-Aldrich), 2-propanol (99.9%, Sigma-Aldrich), toluene (C99.0%, VWR Chemicals). Potassium O-3,3-dimethylbutan-2-yl dithiocarbonate (KXa-C6) and potassium O-2,2-dimethylpentan-3-yl dithiocarbonate (KXa-C7) were prepared by the following previously published procedures [51,55].…”

Section: Experimental Materials and Methodsmentioning

confidence: 99%

“…1. Nickel xanthate precursors nickel (II) O-3,3-dimethylbutan-2-yl dithiocarbonate (NiXa-C6) and nickel (II) O-2,2-dimethylpentan-3-yl dithiocarbonate (NiXa-C7) were synthesized analogously to our previously published procedures for metal xanthates [51,55] and isolated in high yields. The obtained green powders are stable over an extended period of time under ambient conditions and exhibit high solubility in nonpolar organic solvents such as chloroform, toluene or chlorobenzene due to the branched alkyl side chains.…”

Section: Synthesis and Structural Analysismentioning

confidence: 99%

“…The attractive properties of metal xanthates, like their usually good stability (also in solution), relatively low decomposition temperature (below 200°C) and simplicity to tailor solubility and decomposition behavior by variation of their organic side chains, have ensured that they are widely employed in the preparation of various metal sulfide nanomaterials [35][36][37][38][39][51][52][53][54][55][56][57][58][59][60].…”

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confidence: 99%

“…A variety of binary (Bi 2 S 3 [52,61], CdS [53], CuS [36], HgS [36], MnS [36], ZnS [36], PbS [60], PdS [35], SnS [59], NiS [35][36][37][38][39]), ternary (copper indium sulfide [51], copper antimony sulfide [54]) and quaternary (copper zinc tin sulfide [55]) metal sulfide nanomaterials have already been synthesized via a thermally induced decomposition of the metal xanthates, proceeding via the Chugaev elimination mechanism [36,51]. Far less explored is the conversion of metal xanthates to metal sulfides at room temperature by photochemically induced decomposition using UV irradiation [56,57] or direct chemical reaction with primary amines.…”

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confidence: 99%

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Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

et al. 2017

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Nickel sulfide thin films and nanocrystals stabilized with oleylamine ligands are prepared from two different nickel xanthates as single-source precursors, which decompose at approx. 180°C, and are thereby converted into nickel sulfide. These nickel xanthates comprise branched alkyl moieties allowing the choice of a wide range of nonpolar organic solvents for the processing to nickel sulfide thin films as well as to nanoparticles. The crystal structures of both compounds show a typical square-planar coordination of the sulfur atoms of both xanthates to the nickel central atom. The thermal decomposition via the Chugaev reaction forming nickel sulfide was studied by thermal gravimetric analysis showing the reaction taking place at about 180°C. Consequently, by thermally converting spin-coated metal xanthate films directly on the substrates in the solid state, thin films consisting of hexagonal nickel sulfide are formed. If the nickel xanthates are heated in an oleylamine solution, oleylaminecapped nickel sulfide nanocrystals are obtained, exhibiting hexagonal NiS as main phase and Ni 3 S 4 as secondary phase. This is also reflected in a sulfur-rich composition of the synthesized nickel sulfide nanocrystals as observed from TEM-EDX analyses.

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Section: Experimental Materials and Methodsmentioning

confidence: 99%

Section: Synthesis and Structural Analysismentioning

confidence: 99%

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confidence: 99%

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Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

et al. 2017

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“…The decomposition of metallo-organic xanthates is known to take place via the relatively lowtemperature and clean Chugaev elimination reaction [19]. The use of the xanthate ligand in SSPs has permitted the formation of many metal sulfides, including, but not limited to, MoS 2 [20], CdS [21], NiS, PdS [22], and CZTS [23], at lower temperatures than those needed by their respective (N,N-dialklydithiocarbamato-) analogs. Recently, we have reported the preparations of PbS/polymer composites from both lead(II)xanthate and lead(II)dithiocarbamate complexes by a melt process [18,24], finding that the decomposition of Pb(S 2 CO n Bu) 2 in a polymer matrix produced pure cubic PbS nanocrystals at 150°C; significantly lower temperatures than 275°C are needed to decompose Pb(S 2 CN n Bu 2 ) 2 .…”

Section: Introductionmentioning

confidence: 99%

A facile method for the production of SnS thin films from melt reactions

et al. 2016

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Tin(II)O-ethylxanthate [Sn(S 2 COEt) 2 ] was prepared and used as a single-source precursor for the deposition of SnS thin films by a melt method. Polycrystalline, (111)-orientated, orthorhombic SnS films with controllable elemental stoichiometries (of between Sn 1.3 S and SnS) were reliably produced by selecting heating temperatures between 200 and 400°C. The direct optical band gaps of the SnS films ranged from 1.26 to 1.88 eV and were strongly influenced by its Sn/S ratio. The precursor [Sn(S 2 COEt) 2 ] was characterized by thermogravimetric analysis and attenuated total reflection Fourier-transform infrared spectroscopy. The as-prepared SnS films were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, powder X-ray diffractometry, Raman spectroscopy, and UV-Vis spectroscopy.

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Soluble Xanthate Compounds for the Solution Deposition of Metal Sulfide Thin Films

et al. 2014

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A series of soluble metal ethylxanthate compounds was synthesised as precursors for metal sulfide thin films to be deposited using solution‐based techniques. Initially, a range of air‐ and moisture‐stable organic ethylxanthate (EtXn) salts were synthesised (cation=Me4N (1), Et4N (2), Pr4N (3), Ph4P (4), guanidinium (5), NMeH3 (6), NMe2H2 (7), NMe3H (8), NH4 (9)). Thermogravimetric analysis (TGA) was used to examine their decomposition profiles, which in turn informed the decision of which counter cation was best suited for inclusion in the metal xanthate compounds. Periodic NMR spectroscopy studies and single‐crystal X‐ray diffraction (SXRD) were used to determine the role protic ammonium counter cations play in the detrimental conversion of xanthates to dithiocarbamate anions. The organic salts 1 and 4 were used to form the metal ethylxanthate compounds (Me4N)[M(EtXn)x] (x=3 for M=Cd (10 Cd), Ni (10 Ni), Zn (10 Zn); x=4 for M=La (11 La)) and (Ph4P)[M(EtXn)3] (M=Cd (12 Cd), Ni (12 Ni), Zn (12 Zn)). Solubility studies on these compounds were performed using a range of solvents to demonstrate the viability of using these compounds for solution‐based deposition methods for thin‐film formation. TGA of the metal xanthate compounds was used to examine their thermal‐decomposition profiles and the product resulting from thermolysis was found to be the respective metal sulfide. In addition, the coproducts of thermal decomposition were analysed by headspace gas‐chromatography mass spectrometry (HS GC–MS) to probe the decomposition mechanism of the precursors. In situ variable‐temperature synchrotron XRD studies on both bulk and thin‐film samples of 10 Cd and 12 Cd were used to examine metal sulfide crystalline phase formation. Decomposition of both precursors was found to give CdS in a hexagonal phase, with the addition of CdCl2 found to aid in increasing the crystallite size during crystallisation.

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Solution-processed copper zinc tin sulfide thin films from metal xanthate precursors

Cited by 28 publications

References 65 publications

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

A facile method for the production of SnS thin films from melt reactions

Soluble Xanthate Compounds for the Solution Deposition of Metal Sulfide Thin Films

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