Hydrogen storage is one of the important steps in the implementation of the hydrogen economy; metal hydrides are a promising way to achieve this goal. We present in this work the use of Rietveld analysis to characterize structurally TiCr-based alloys that are able to store hydrogen. TiCruV09, TiCrL1V0.45Nb0.45, TiCr1.1V0.2 Nb0.8, TiCr1.1Nb0.9 alloys were synthesized in an arc furnace under argon atmosphere. The analysis of phases was developed by X-Ray Diffraction (XRD) for further refinement of both the two lattice parameters and the percentage of the phases. Our results confirmed that a structure bcc, mostly combined with a small percentage of Laves phases, leads to obtain important properties in this area. Rietveld analysis was performed by the Fullprof program and this program allows us to obtain the different structural parameters.