Abstract: Titanium nickelide intermetallic compounds have been prepared by means of coprecipitation-reduction followed by diffusion processes, in order to obtain the cathodic material with improved hydrogen absorbing character.Titanium-nickel hydroxides are first precipited by NaOH from mixed solution of NiCl₂ and TiCl₄. After dehydration at 600℃, the mixed hydroxide is reduced by CaH₂ to give hydrided TiNi and Ti₂Ni.The coprecipitation-reduction and diffution process has been discussed in detail. The lattice parameters of TiNiH_1.14 and TiNiH_2.56 are 24.85Å and 11.91Å.The temperature-composition dissociation isobars at 1 atm. for the product and potential-time plots of TiNi and Ti₂Ni electrodes have been drawn respectively. The discharge capacities were determined as 262.2 mAh/g for TiNiH_1.14 and 169.9 mAh/g for Ti₂NiH_2.56.Since the product has higher specific surface and excellent electro-catalytic activity, electrodes made from the product have much important effect on decreasing the polarization and increasing the cycle life.