In this paper, we report the microstructure and first hydrogenation properties of TiFe cast with 4 wt.% of Zr. Measurements were made in as-cast state and after processing by ball milling and cryomilling. It was found that ball milling and cryomilling significantly reduced the particle/crystallite sizes with most of the reduction occurring during the first 15 min of milling. While the cryomilled sample did not absorb any hydrogen, ball milling improved the initial kinetics of processed powders compared with the as-cast sample. However it also reduced the hydrogen storage capacity. The observed increased kinetics was likely caused by the reduction of crystallite sizes with longer ball milling times. However, the longer ball milling times might also be the reason of the capacity loss due to formation of new grain boundaries. Faster kinetics was not due to a change in the rate-limiting step, as all kinetics curves were fitted with the 3D growth, diffusion controlled with decreasing interface velocity model.
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