The effect of nickel content in Mg 1−x Ni x (OH) 2 nanoparticles produced by reverse co-precipitation on their structural characteristics, morphology and size parameters of crystallites and particles has been studied. The plate-shaped nanoparticles were shown to be predominantly single crystals. It has been determined that when the nickel content x in the hydroxide solid solution is not less than 0.4, the particle size sharply decreases and the number of stacking faults increases. The dependence of the dehydration temperature of Mg 1−x Ni x (OH) 2 nanoparticles on the nickel content has been revealed. KEYWORDS magnesium hydroxide, nickel hydroxide, layered double hydroxide, nanoparticles.