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Ni/NiO nanopowders have been prepared by using thermal decomposition of aqua solutions of nickel acetate ammine complexes in air at the annealing temperature range of 300°C to 500°C, time of decomposition from 30 to 180 min, and ammonia content in initial complex 3.6 to 9.55 mol/mol Ni 2+ . Chemical composition of obtained powders has been characterized by chemical and thermal analysis. Phase analysis and particle size of powders have been investigated by X-ray diffraction method, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The powders’ pore structure has been determinated by low-temperature nitrogen adsorption method.  Products of decomposition were represented as agglomerates of nanoparticles of Ni, NiO, and hydroxy-containing precursors. Mean agglomerate size depended on ammonia content in initial complex, annealing temperature, and duration and has grown from 30 to 40 to 400 to 520 nm. Mean nanoparticle size of hydroxy-containing precursors was invariable with ammonia concentration in initial complex, annealing temperature, and duration and has grown 5 nm. Mean nanoparticle size of Ni depended on annealing temperature and has grown from 40 to 60 to 40 to 70 nm at temperatures 400°С and 500°С, respectively. Mean nanoparticle size of NiO increased with temperature rising from 5 nm at 350°С to 20 to 25 nm at 500°С.

Obtaining of Ni/NiO nanopowder from aqua solutions of Ni(CH3COO)2 ammonia complexes