Cyclohexylammonium Hexaisothiocyanatonickelate(II) Dihydrate as a Single-Source Precursor for High Surface Area Nickel Oxide and Sulfide Nanocrystals

Cyclohexylammonium hexaisothiocyanatonickelate(II) dihydrate, (C6H11NH3)(4)[Ni(NCS)(6)]center dot 2H(2)O, 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 P2(1)/c with a = 15.8179 (5) angstrom, b = 10.6222 (3) angstrom, c = 13.8751 (4) angstrom, beta = 109.362 (1)degrees, V = 2199.45 (11) angstrom(3), 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 angstrom; 452 m(2)/g) and nickel sulfide (46 angstrom; 220 m(2)/g) via pyrolysis under air at 550 degrees C or helium atmosphere at 500 degrees C, respectively. X-ray powder diffraction (XRPD) demonstrated the nanocrystalline nature of both NiO and NiS with an average crystallite size of 16 and 54 nm, respectively. Scanning electron microscope (SEM) indicated the formation of agglomerated, quasi-spherical particles of nickel oxide and agglomerated flake-like structures of nickel sulfide. The high surface area, porosity, and nanocrystallinity of both NiO and NiS, obtained via this approach, are promising for a wide spectrum of applications.

Automated summary

Cyclohexylammonium hexaisothiocyanatonickelate(II) dihydrate was synthesized and fully characterized. It was used as a single-source precursor for the synthesis of mesoporous, high surface area nickel oxide and nickel sulfide via pyrolysis. The obtained NiO and NiS exhibited nanocrystalline nature, high surface area, porosity, and showed great potential for various applications.