In this paper, we report the results obtained from different phases of metal hydrides. The synthesis and characterization of tantalum hydrides were obtained “in situ” during mechanical milling. Elemental Ta with purity of 99.8% was used in this investigation to obtain the hydrides. A highenergy ball milling technique was utilized to prepare hydrogenated phases. Ta hydrides and oxides were formed as function of milling process time. Milling times of 5, 10 and 20 hours were programmed, and the ball-to-powder weight ratio was 10:1. The material was first characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Before and after hydrogenation process the material was also analyzed by TGA. X-ray diffraction analysis demonstrated that only tantalum hydrides (Ta2H and TaH0.5) were obtained after 20 h of milling. We will discuss the effect of the ball-milling process about formation “in situ” of nanometric tantalum hydrides with methanol as a hydrogen source.
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