Abstract:Submicro-porous nickel wafers were prepared by a molding-decomposition-sintering method, using nickel oxalate nano-rods which were synthesized via a liquid phase precipitation process as precursors, keeping the decomposition temperature of 360?C for 10 minutes, and sintering temperature of 420, 450，480 and 510℃ for 10 minutes respectively, in a tubular oven filled with Ar gas. The study of Infrared spectroscopy (IR) indicated that the precursor as-prepared was pure nickel oxalate. The studies of X-Ray Diffractions (XRD) indicated that the grey wafers as-treated were nickel, which has face-centered cubic crystal structure. The images of Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) showed that the morphology of metal nickel wafers were obvious porous structure. The structure of holes was irregular with 100-1000 nm in diameters, and the hole walls were fiber-like nickel with 100-300 nm in diameters.