Abstract: A process for preparing a LiCoO.sub.2 or LiNiO.sub.2 powder comprising the steps of dissolving lithium nitrate, lithium acetate or lithium hydroxide and cobalt nitrate, cobalt acetate, cobalt oxide or cobalt hydroxide; or dissolving lithium nitrate, lithium acetate or lithium hydroxide, and nickel nitrate, nickel acetate, nickel oxide or nickel hydroxide to produce a mixed solution, sufficiently mixing the mixed solution with a chelating agent, polyacrylic acid, malic acid or polyvinyl butyral, slowly heating the above to produce a sol, continuously and slowly heating the sol to produce a gel precursor, heating the gel precursor to produce a precursor powder, and calcining the precursor powder to produce a LiCoO.sub.2 or LiNiO.sub.2 powder is simple and economic. The particles of the powder produced by the process are so microscopic and have a high specific surface area that cathode material of a lithium based secondary cell using the powder shows preferable properties.