Synthesis of rare pure phase Ni3S4 and Ni3S2 nanoparticles in different primary amine coordinating solvents

Gervas, Charles; Mlowe, Sixberth; Akerman, Matthew P.; Ezekiel, Itegbeyogene P.; Moyo, T.; Revaprasadu, Neerish

doi:10.1016/j.poly.2016.11.014

Cited by 40 publications

(16 citation statements)

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“…8b) [30,33,34]. In these studies, the role of the primary amine as reaction component, besides its function as solvent and stabilizing agent, is demonstrated, whereby the decomposition mechanism or rather phase composition can be tuned by the nature of the amine.…”

Section: Preparation Of Nickel Sulfide Nanoparticlesmentioning

confidence: 99%

“…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%

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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 Nanoparticlesmentioning

confidence: 99%

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confidence: 99%

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

et al. 2017

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“…However, the synthesis of phase pure nickel sulfide nanomaterials from single molecular precursors are limited, mixed-phase systems are normally generated. For instance, Gervas et al employed a solvothermal route for the synthesis of Ni 3 S 4 and Ni 3 S 2 nanoparticles from dithiocarbamate precursors in which a mixture of other phases of nickel sulfide were also obtained 38 . Ghezelbash et al, carried out the solventless thermolysis of nickel thiolate precursors which resulted in a mixed phase system of NiS and Ni 3 S 4 39 .…”

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confidence: 99%

Direct solvent free synthesis of bare α-NiS, β-NiS and α-β-NiS composite as excellent electrocatalysts: Effect of self-capping on supercapacitance and overall water splitting activity

Shombe

Khan

Zequine

et al. 2020

Sci Rep

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Nickel sulfide is regarded as a material with tremendous potential for energy storage and conversion applications. However, it exists in a variety of stable compositions and obtaining a pure phase is a challenge. this study demonstrates a potentially scalable, solvent free and phase selective synthesis of uncapped α-niS, β-niS and α-β-niS composites using nickel alkyl (ethyl, octyl) xanthate precursors. Phase transformation and morphology were observed by powder-X-ray diffraction (p-XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The comparative efficiency of the synthesized samples was investigated for energy storage and generation applications, in which superior performance was observed for the niS synthesized from the short chain xanthate complex. A high specific capacitance of 1,940 F/g, 2,150 F/g and 2,250 F/g was observed at 2 mV/s for bare α-niS, β-niS and α-β-NiS composite respectively. At high current density of 1 A/g, α-niS showed the highest capacitance of 1,287 F/g, with 100% of Coulombic efficiency and 79% of capacitance retention. In the case of the oxygen evolution reaction (oeR), β-NiS showed an overpotential of 139 mV at a current density of 10 mA/cm 2 , with a Tafel slope of only 32 mV/dec, showing a fast and efficient process. It was observed that the increase in carbon chain of the synthesized self-capped nickel sulfide nanoparticles decreased the overall efficiency, both for energy storage and energy generation applications. As a step towards the implementation of sustainable energy development strategies, research on the design of high-performance energy storage and conversion systems is gathering renewed momentum 1-3. Sodium ion batteries (SIBs), lithium-ion batteries (LIBs), and supercapacitors (SCs) are examples of the most studied energy storage devices 4,5. Energy conversion systems on the other hand, constitute a series of electrochemical reactions occurring in an electrolytic cell or in a hydrogen-oxygen fuel cell 3. Hydrogen is a clean and sustainable energy carrier, currently regarded as the best alternative fuel of the future 6,7. Its generation via the electrocatalytic splitting of water is a commonly investigated energy conversion technology 8. The performance of both energy storage devices and energy conversion systems is largely influenced by the type of electroactive material employed. Generally, for energy conversion systems the goal is to develop low cost, earth-abundant and efficient electrocatalysts that will replace Pt-, Ir-and Ru-based compounds 9 , while for energy storage devices, the goal is to develop advanced electrode materials that can deliver high energy and power densities 10. Carbon-based materials 11 , conductive polymers 12 , transition metal oxides 13 , nitrides 14 , carbides 14 , phosphides 15 , and sulfides 5 are among the materials investigated for both energy storage and generation applications. Owing to their low cost, high electrochemical activity as well as mechanical and thermal stability, transition

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“…The FTIR spectrum of the complex show ν(C–N) (thioureide) peak at 1489 cm −1 . The position of this band, typical of dithiocarbamates, indicated a partial double bond character [ 42 ]. The bond energy falls between the single (1350–1250 cm −1 ) and double (1690–1650 cm −1 ) bond energies.…”

Section: Resultsmentioning

confidence: 99%

Morphological variations in Bi2S3 nanoparticles synthesized by using a single source precursor

Onwudiwe

Nkwe

2020

Heliyon

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A simple solvothermal decomposition of bismuth dithiocarbamate complex in oleylamine, oleic acid, and hexadecylamine at 180 °C, yielded bismuth sulphide nanomaterials of different morphologies represented as Bi 2 S 3 (OAm), Bi 2 S 3 (OAc) and Bi 2 S 3 (HDA) respectively. The bismuth complex, used as the single source precursor, was synthesized and characterised by elemental analysis, FTIR, and NMR spectroscopic techniques. The spectroscopic and micro analysis confirmed the proposed compound, while the as-prepared nanoparticles were characterized using UV-visible spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive spectrometer (EDS). The effects of the different solvent media on the structural properties of the obtained Bi 2 S 3 were investigated. An orthorhombic phase bismuthinite of varying intensities were obtained, with an indication that a bias of orientations existed in the (2 1 1) crystallographic planes in the Bi 2 S 3 (OAm) compared to the characteristic (1 3 0) diffraction peak of Bi 2 S 3 . The microscopic analysis showed a correlation between the nanoparticles' morphology and the type of solvent used, which also implied that the properties of Bi 2 S 3 were affected by the solvent medium.

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Synthesis of rare pure phase Ni3S4 and Ni3S2 nanoparticles in different primary amine coordinating solvents

Cited by 40 publications

References 39 publications

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

Nickel sulfide thin films and nanocrystals synthesized from nickel xanthate precursors

Direct solvent free synthesis of bare α-NiS, β-NiS and α-β-NiS composite as excellent electrocatalysts: Effect of self-capping on supercapacitance and overall water splitting activity

Morphological variations in Bi2S3 nanoparticles synthesized by using a single source precursor

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