Pyridine Adducts of Nickel(II) Xanthates as Single-Source Precursors for the Aerosol-Assisted Chemical Vapor Deposition of Nickel Sulfide

Alam, Naveed; Hill, Michael S.; Kociok‐Köhn, Gabriele; Zeller, Mat­thias; Mazhar, Muhammad; Molloy, Kieran C.

doi:10.1021/cm801330v

Cited by 87 publications

(59 citation statements)

References 23 publications

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“…49:51 at % (films prepared from NiXa-C7). The formation of a mixture of a-NiS and b-NiS phase by thermal decomposition of nickel xanthates and dithiocarbamates is common and has also already been reported in other publications [30,33,37,39].…”

Section: Preparation Of Nickel Sulfide Thin Filmssupporting

confidence: 61%

“…Numerous single-source precursor compounds, which already contain a nickel sulfur bond, such as nickel dithiocarbamate [28][29][30][31][32][33][34], dithiocarbonate (xanthate) [35][36][37][38][39][40], thiolate [10,41], dithiooxamide [42], thiourea [43], thiobenzoate [44], thiobiuret [45], mercaptobenzothiazole [46], thiosemicarbazide [47], polysulfide [48], imidodiphosphinate [49] or dithiophosphate [50], have already been investigated for the fabrication of various nickel sulfide nanostructures.…”

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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%

“…Considering the attractive potential of metal xanthates as SSPs for the production of metal sulfide nanomaterials, it is surprising that there are only a few reports dealing with the thermal conversion of nickel xanthate complexes [35][36][37][38][39]. Therefore, in this contribution we demonstrate the potential of the two novel 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), as SSP for the preparation of nickel sulfide nanostructures.…”

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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: Preparation Of Nickel Sulfide Thin Filmssupporting

confidence: 61%

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confidence: 99%

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confidence: 99%

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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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Flexible Molecular Precursors for Selective Decomposition to Nickel Sulfide or Nickel Phosphide for Water Splitting and Supercapacitance

Ayom

Khan

Ingsel

et al. 2020

Chemistry A European J

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Herein, the synthesis of three nickel(II) dithiophosphonate complexes of the type [Ni{S2P(OR)(4‐C6H4OMe)}2] [R=H (1), C3H7 (2)] and [Ni{S2P(OR)(4‐C6H4OEt}2] [R=(C6H5)2CH (3)] is described; their structures were confirmed by single‐crystal X‐ray studies. These complexes were subjected to surfactant/solvent reactions at 300 °C for one hour as flexible molecular precursors to prepare either nickel sulfide or nickel phosphide particles. The decomposition of complex 2 in tri‐octylphosphine oxide/1‐octadecene (TOPO/ODE), TOPO/tri‐n‐octylphosphine (TOP), hexadecylamine (HDA)/TOP, and HDA/ODE yielded hexagonal NiS, Ni2P, Ni5P4, and rhombohedral NiS, respectively. Similarly, the decomposition of complex 1 in TOPO/TOP and HDA/TOP yielded hexagonal Ni2P and Ni5P4, respectively, and that of complex 3 in similar solvents led to hexagonal Ni5P4, with TOP as the likely phosphorus provider. Hexagonal NiS was prepared from the solvent‐less decomposition of complexes 1 and 2 at 400 °C. NiS (rhom) had the best specific supercapacitance of 2304 F g−1 at a scan rate of 2 mV s−1 followed by 1672 F g−1 of Ni2P (hex). Similarly, NiS (rhom) and Ni2P (hex) showed the highest power and energy densities of 7.4 kW kg−1 and 54.16 W kg−1 as well as 6.3 kW kg−1 and 44.7 W kg−1, respectively. Ni5P4 (hex) had the lowest recorded overpotential of 350 mV at a current density of 50 mA cm−2 among the samples tested for the oxygen evolution reaction (OER). NiS (hex) and Ni5P4 (hex) had the lowest overpotentials of 231 and 235 mV to achieve a current density of 50 mA cm−2, respectively, in hydrogen evolution reaction (HER) examinations.

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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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Pyridine Adducts of Nickel(II) Xanthates as Single-Source Precursors for the Aerosol-Assisted Chemical Vapor Deposition of Nickel Sulfide

Cited by 87 publications

References 23 publications

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

Flexible Molecular Precursors for Selective Decomposition to Nickel Sulfide or Nickel Phosphide for Water Splitting and Supercapacitance

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

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