Abstract: Metallic nickel was electrochemically dissolved in absolute ethanol and acetylacetone solution in the presence of Bu4NBr(as electronconductive additive). The electrolyte solution containing the precursor was then directly hydrolyzed to obtain nanocrystalline NiO. The precursor was characterized by FTIR、1HNMR、Raman spectra and the nanopowder was characterized by XRD and TEM. The results showed that the NiO powder after hydrolysis was amorphous but formed the cubic NaCl structure when calcined at 350 ℃,the NiO powder have a narrow size distribution of 5～10 nm after annealed at 600 ℃. Characterization of the electrochemical product revealed that Ni(OEt)2(acac)2 was formed by anode dissolution of nickel in ethanol and acetylacetone mixed solution. The experiments also showed that the precursor of the nanocrystalline NiO prepared by this method can be dissolved in ethanol solution when temperature increase to 40～50 ℃ region.

Key words: Electrolysis, Nickel anode, Sol-gel, Nanocrystalline NiO, Raman spectrum