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Ni and Ni-Cu,Co nanopowders have been synthesized by chemical reduction method. It was demonstrated early that hydrogenation properties are critically dependent from the structure of particles. Therefore the crystal structure of Ni-based nanopowders has been studied precisely by SEM, XRD and SAXS methods. X-ray diffraction and SEM analysis showed that the size of the obtained nickel nanoparticles covered the range from 20 to 200 nm. The particles consist from crystallites, which are characterized by the size about 5-20 nm. The complicated structure of the particles was confirmed by SAXS method.