The use of metal powders produced by mechanical treatment in various fields, such as catalysis or gas absorption, is often limited by the low specific surface area of the resulting particles. One of the possible solutions for increasing the particle fineness is hydrogen treatment; however, its effect on the structure of mechanically treated powders remains unexplored. In this work, for the first time, a metal-oxide nanocomposite powder was produced by mechanical alloying (MA) in a high-energy planetary ball mill from commercial powders of Zr and Co in the atomic ratio Co:Zr = 53:47 in an inert atmosphere, followed by high-pressure hydrogenation at room temperature. The initial powders and products of alloying and hydrogenation were studied by XRD, 59Co Internal Field NMR, SEM, and HRTEM microscopy with EDX mapping, as well as Raman spectroscopy. MA resulted in significant amorphization of the powders, as well as extensive oxidation of zirconium by water according to the so-called “Fukushima effect”. Moreover, an increase in hcp Co sites was observed. 59Co IF NMR spectra revealed the formation of magnetically single-domain cobalt particles after hydrogenation. The crystallite sizes remained unchanged, which was not observed earlier. The pulverization of Co and an increase in hcp Co sites made this nanocomposite suitable for the synthesis of promising Fischer–Tropsch catalysts.
