Effect of Synthesis Conditions on the Phase Composition and Structure of Nickel-Based Microspheres Prepared by Exothermic Synthesis from a Glycine–Nitrate Solution

— We report our findings on the influence of composition and reaction temperature on the phase composition and structure of nickel-based microspheres prepared by combining exothermic synthesis and spray pyrolysis from a glycine–nitrate solution. It has been shown that, at the optimal reductant-to-oxidant ratio and reaction temperature, the microspheres consist of Ni, Ni 3 N, and NiO, and the nickel content reaches 98%. The synthesized material has the form of microspheres 0.5 to 1.5 μm in average diameter and 10 to 15 nm in crystallite size.