Hydrogen storage in metal hydrides has been received lots of attentions, recently. However, lack of enough absorbtion/desorbtion capacity and good kinetic properties in these materials have limited its application. Making ultrafine and nanostructures materials by some methods like mechanical alloying and melt spinning can improve the metal hydrides properties. In this research, vacuum plasma spraying was employed as a new method to produce hydrogen storage materials. The properties of the produced materials were compared to the materials produced by vacuum induction melting and mechanical alloying. Ti 1-x Zr x Mn 2-y-z V y Cr z alloy was used and its composition was optimized by design experimental method. The optimum stoichiometric coefficients were z=0, y=0.6 and x=0.28. XRD, SEM analysis on the samples, produced by induction melting, plasma spraying, and ball milling showed that all samples consisted of two main crystallographic phases; lave and V-base BCC solid solution phase. The amount of C14 Lave phase in plasma sprayed sample was twice compared to other samples. The amount of BCC solid solution in the induction melted sample was the highest. The results of galvanostatic tests showed that the capacity of all samples decreased with increasing the number of cycle. The electrochemical capacity of the induction melted sample was higher which could be due to the higher amount of V-base solid solution. The plasma sprayed sample showed the highest cyclic stability. The result of Electrochemical Impedance Spectra (EIS), potentiostatic and High Rate Discharge (HRD) tests showed that the kinetic properties of the plasma sprayed sample was much better than those for two other samples. The improvement of the kinetic properties of the plasma sprayed sample could be attributed to the presence of the highest amount of C14 Lave and amorphous phases. The Seivert tests on the melted and ball milled samples showed that the highest capacity of storage can be achieved at 150 o C. Keywords: Characterization, Hydrogen storage, Ti-base alloys, Vacuum plasma spray, Ball milling, Vacuum induction melting, Ultra fine grain, Rapid solidification