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Mg-Ni nanoparticles were synthesized by a physical vapor condensation method (DC arc-discharge) in a mixture of argon and hydrogen atmosphere, using compressed mixture of micro powders as the raw materials. The crystal phases, morphology, and microstructures of nanoparticles were analyzed by means of X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). It was found that the intermetallic compounds of Mg₂Ni and MgNi2 formed with existence of phases of Mg, Ni, and MgO in Mg-Ni nanoparticles. After one cycle of hydrogen absorption/desorption process (activation treatment), Mg-Ni nanoparticles exhibited excellent hydrogen absorption properties. Mg₂Ni phase became the main phase by aphase transformation during the hydrogen treatments. The phenomenon of refinement of grain size in the nanoparticle was also observed after the hydrogen absorption/desorption processes, which was attributed to the effect of volume expansion/shrinkage and subsequent break of nanoparticles. Maximum hydrogen absorption contents are 1.75, 2.21 and 2.77 wt.% at 523, 573 and 623 K, respectively.

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