Conversion of single crystals of a nickel(II) dithiocarbamate complex to nickel sulfide crystals

Angeloski, Alexander; Cortie, Michael B.; Scott, John; Bordin, Dayanne Mozaner; McDonagh, Andrew M.

doi:10.1016/j.ica.2018.12.014

Cited by 10 publications

(20 citation statements)

References 70 publications

(82 reference statements)

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“…These values match well with the expected 1:1 nickel to sulfur molar ratio. The calculated weight percentages also agree with the reported values determining the formation of αor β-NiS www.nature.com/scientificreports www.nature.com/scientificreports/ phase 52,53 . Elemental mapping of the samples indicate a homogeneous distribution of the two elements in the samples (Figure S7, ESI).…”

Section: Resultssupporting

confidence: 87%

“…The reversibility might be influenced by the content of Ni and S present in the system at a specified temperature. It has been reported that, the β-NiS phase is formed when the ratio of Ni:S is in the 64:36-67:33 wt% range, and the α-NiS phase is formed when the ratio of Ni:S is in the 63:37-64:34 wt% range 52,53 . The intricate stoichiometric difference between the two phases makes it very challenging to obtain pure phases in the absence of any surface stabilizing reagents.…”

Section: Resultsmentioning

confidence: 99%

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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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Section: Resultssupporting

confidence: 87%

Section: Resultsmentioning

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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“…Recent insight into this decomposition process comes from in situ X-ray diffraction studies. 177 Single crystals of [Ni(S 2 CN i Pr 2 ) 2 ] decompose in a single step at ca. 250 °C to give α-NiS exclusively, with no β-NiS phase detected.…”

Section: Groupmentioning

confidence: 99%

“…595 Later, the solvothermal decomposition of a related precursor, [Ni(S 2 CNBz 2 ) 3 ][FeCl 4 ], in EN was reported to give iron−nickel sulfide nanoparticles, however, broad PXRD peaks meant their phase could not be determined. 177 Recently, Hogarth and co-workers carried out a detailed study of the solvothermal decomposition of [Fe(S 2 CN i Bu 2 ) 3 ] and [Ni-(S 2 CN i Bu 2 ) 2 ] in OLA, products varying as a function of temperature and SSP concentration. 588 The latter was found to be a key variant.…”

Section: Ternary Metal Sulfidesmentioning

confidence: 99%

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Dithiocarbamate Complexes as Single Source Precursors to Nanoscale Binary, Ternary and Quaternary Metal Sulfides

2021

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Nanodimensional metal sulfides are a developing class of low-cost materials with potential applications in areas as wide-ranging as energy storage, electrocatalysis, and imaging. An attractive synthetic strategy, which allows careful control over stoichiometry, is the single source precursor (SSP) approach in which well-defined molecular species containing preformed metal–sulfur bonds are heated to decomposition, either in the vapor or solution phase, resulting in facile loss of organics and formation of nanodimensional metal sulfides. By careful control of the precursor, the decomposition environment and addition of surfactants, this approach affords a range of nanocrystalline materials from a library of precursors. Dithiocarbamates (DTCs) are monoanionic chelating ligands that have been known for over a century and find applications in agriculture, medicine, and materials science. They are easily prepared from nontoxic secondary and primary amines and form stable complexes with all elements. Since pioneering work in the late 1980s, the use of DTC complexes as SSPs to a wide range of binary, ternary, and multinary sulfides has been extensively documented. This review maps these developments, from the formation of thin films, often comprised of embedded nanocrystals, to quantum dots coated with organic ligands or shelled by other metal sulfides that show high photoluminescence quantum yields, and a range of other nanomaterials in which both the phase and morphology of the nanocrystals can be engineered, allowing fine-tuning of technologically important physical properties, thus opening up a myriad of potential applications.

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Gold Microstructures by Thermolysis of Gold(III) Di‐isopropyldithiocarbamate Complexes

Angeloski,

Flower‐Donaldson,

Matar

et al. 2024

ChemNanoMat

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Elemental gold was formed by thermolysis of gold(III) dithiocarbamate single‐source precursors, which exist as two isomers. The isomers were readily synthesised from the reaction between chloroauric acid and sodium di‐isopropyldithiocarbamate and could be isolated from each other. The thermal decomposition processes were evaluated using thermogravimetry and electrical resistance measurements. The structure and purity of the resultant gold was examined using scanning electron microscopy. The resultant gold materials were drastically different and dependent on the thermolysed isomer.

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Conversion of single crystals of a nickel(II) dithiocarbamate complex to nickel sulfide crystals

Cited by 10 publications

References 70 publications

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

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

Dithiocarbamate Complexes as Single Source Precursors to Nanoscale Binary, Ternary and Quaternary Metal Sulfides

Gold Microstructures by Thermolysis of Gold(III) Di‐isopropyldithiocarbamate Complexes

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