Synthesis of nickel and cobalt sulfide nanoparticles using a low cost sonochemical method (original) (raw)
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Synthesis of Nickel Sulfide Thin Films and Nanocrystals from the Nickel Ethyl Xanthate Complex
Advances in Materials Science and Engineering
Nickel sulfides have unique and diverse structural features, making them ideal for energy conversion and storage. This research focuses on the synthesis and characterization of nickel sulfide thin films and nanocrystals from nickel ethyl xanthate complex using spin-coating and solventless methods. The nickel ethyl xanthate complex (C6H10S4NiO2) was characterized using Fourier-transformed infrared (FT-IR), ultraviolet-visible (UV-Vis), and nuclear magnetic resonance (NMR) spectroscopies as well as thermogravimetric analysis (TGA). The NiS thin films and nanoparticles were analyzed with energy dispersive X-ray (EDX) spectroscopy and X-ray diffraction (XRD). Nickel ethyl xanthate was synthesized in an 81.2% yield. The bandgaps of the nickel sulfide obtained from the spin-coating method ranged from 4.35–4.88 eV. For the solventless method, the bandgap of the nickel sulfide ranged from 3.93–3.96 eV. The crystal phase observed from the spin-coating and solventless methods was α-NiS (hexag...
Preparation and characterization of Cu and Ni sulfides nanoparticles
In the present work we aimed to prepare two metal sulfides nanoparticles [copper monosulfide (CuS) and nickel monosulfide (NiS)] using two different sulfur sources (Potassium N 0-[4-(N 0-dithiocarboxy-hydra zino)-4-oxo-butyryl]-hydrazine carbodithionate (I) and thiourea (II)) by a simple chemical method in an aqueous ethanolic solution. The effect of the used sulfur source on the optical and structural properties of the prepared metal sulfides was investigated. The synthesized sulfides were characterized using X-ray diffraction (XRD), UV-visible spectrophotometry, Transmission Electron Microscope (TEM) and elemental analysis. The yield, lattice parameters, crystallite sizes, microstrains and the band gap energy of the prepared CuS and NiS nanoparticles were evaluated and compared. Using the organic salt (I) leads to obtaining single phase structure of CuS and NiS, while using thiourea lead to obtaining mixed phases structure. By using the organic salt (I) we obtained CuS nanoparticles having greater potential for solar cell applications and NiS nanoparticles very interesting for photo catalysis applications.
Nanostructured Nickel Sulfides with Different Stoichiometries Prepared by Mechanochemical Synthesis
2018
By reactions between nickel and sulfur, products with different stoichiometries can be obtained, from the nickel rich compounds like Ni3S2, over NiS to sulfur rich compounds like Ni3S4 and NiS2. Nickel sulfides have been recently used in many applications, like solar cell materials, catalysts and cathode material for lithium batteries. In this paper, we present the synthesis of different nanosized nickel sulfides by high – energy milling of nickel powder with elemental sulfur in different molar ratios, using milling times between 1h and 8h. The products were characterized by X-ray powder diffraction, TEM including EDX analysis, elemental analysis and UV – Vis spectroscopy. Following products have been obtained in good yield: by milling a Ni : S mixture in molar ratio 1: 1, NiS1.03 was obtained after 8h milling time. Using a Ni : S mixture in molar ratio 1 : 2, NiS2 was obtained after 8h. Finally, from a Ni : S = 3 : 2 mixture, nanosized Ni3S2 can be obtained after 2h.
Chalcogenide Lett, 2010
Hierarchical nanostructureds of β-NiS were successfully prepared by hydrothermal treatment of Ni(NO 3 ) 2 .6H 2 O and thioglycolic acid (TGA) at 180 • C. The as prepared β-NiS hierarchical nanostructureds were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), ultraviolet-visible (UV-vis) absorption spectroscopy, photoluminescence (PL) spectroscopy and Fourier transform infrared (FT-IR) spectra. The hierarchical nanostructureds, with an average diameter of ~600 nm, were composed of short nanorods with a diameter of ~30 nm and a length of about 150 nm. On the basis of the experimental results and corresponding literatures, a possible growth mechanism of the NiS hierarchical nanocrystals is discussed. The obtained products have relatively high surface area, which favors the application in catalysis.
Polyhedron, 2012
Convenient and environmentally friendly synthesis of Co 9 S 8 /PVA, Co x S y /EG and Co x S y /3-MPA nanocomposites were carried out in the presence of ultrasonic irradiation by the liquid phase synthesis of the sonochemical method. For the synthesis, cobalt acetate tetrahydrate [Co(CH 3 COO) 2 •4H 2 O] and sodium sulfide (Na 2 S•9H 2 O) were used as a cobalt and sulfur precursor, respectively. Polyvinyl alcohol (PVA), ethylene glycol (EG) and 3-mercaptopropionic acid (3-MPA) were used as a capping agent and surfactant. The structural, optical properties and morphology of nanocomposites were characterized using X-ray diffractometer (XRD), Ultraviolet/Visible Spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The optical band gap of Co 9 S 8 /PVA is 1.81 eV and for Co x S y /EG is 2.42 eV where the direct band gap of bulk cobalt sulfide is (0,78-0,9 eV). The wide band gap indicates that synthesised nanocomposites can be used in the fabrication of optical and photonic devices. The growth mechanisms of the Co 9 S 8 , CoS 2 and Co 3 S 4 nanoparticles were discussed by the reactions. The effects of sonication time and annealing temperature on the properties of the nanoparticles have been studied in detail.
Mixed Ni/Co Hydroxide Nanoparticles Synthesized by Sonochemical Method
Journal of Nanoscience and Nanotechnology, 2007
Nickel hydroxide nanoparticles with different amounts of cobalt atoms in the structure forming a unique material, were synthesized by using ultrasonic radiation. The particles of 5 nm diameter were prepared and characterized by X-Ray diffraction, Raman and Infrared spectroscopies, and thermogravimetry. The incorporation of cobalt leads to distinct crystalline planes, showing an opened and disarranged structure, indicating the stabilization of the -Ni(OH) 2 phase.
Nickel Sulfide and Copper Sulfide Nanocrystal Synthesis and Polymorphism
Nickel sulfide and copper sulfide nanocrystals were synthesized by adding elemental sulfur to either dichlorobenzene-solvated (copper sulfide) or oleylamine-solvated metal(II) precursors (nickel sulfide) at relatively high temperature to produce the metal sulfide. Nickel sulfide nanocrystals are cubic Ni3S4 (polydymite) with irregular prismatic shapes, forming by a two-step reduction-sulfidation mechanism where Ni(II) reduces to Ni metal before sulfidation to Ni3S4. Despite extensive efforts to optimize the Ni3S4 nanocrystal size and shape distributions, polydisperse nanocrystals are produced. In contrast, copper sulfide nanocrystals can be obtained with narrow size and shape distributions. The copper sulfide stoichiometry depended on the Cu:S mole ratio used in the reaction: Cu:S mole ratios of 1:2 and 2:1 gave CuS (covellite) and Cu1.8S (digenite), respectively. CuS nanocrystals formed as hexagonal disks that assemble into stacked ribbons when cast from solution onto a substrate. CuS, Cu1.8S, and Ni3S4 differ from the Cu2S and NiS nanocrystals obtained by solventless decomposition of metal thiolate single source precursors, in terms of stoichiometry for copper sulfide, and both stoichiometry and morphology for nickel sulfide
Crystals, 2022
Cyclohexylammonium hexaisothiocyanatonickelate(II) dihydrate, (C6H11NH3)4[Ni(NCS)6]·2H2O, was synthesized, for the first time, by a four-step method in a yield of 95%. The compound was fully characterized by elemental microanalysis, Fourier transform infrared (FTIR), ultraviolet-visible-near infrared (UV-Vis-NIR), and nuclear magnetic resonance (NMR) spectroscopy and thermogravimetry. A single crystal X-ray diffraction (SXRD) gave the monoclinic space group P21/c with a = 15.8179 (5) Å, b = 10.6222 (3) Å, c = 13.8751 (4) Å, β = 109.362 (1)°, V = 2199.45 (11) Å3, Z = 2 (T = 293 K) for this novel hybrid organic–inorganic compound. The title compound was employed as a single-source precursor for the synthesis of mesoporous, high surface area nickel oxide (53 Å; 452 m2/g) and nickel sulfide (46 Å; 220 m2/g) via pyrolysis under air at 550 °C or helium atmosphere at 500 °C, respectively. X-ray powder diffraction (XRPD) demonstrated the nanocrystalline nature of both NiO and NiS with an av...