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We present a structural investigation on Co-Ni alloy nanoclusters obtained by sequential ion implantation in silica slides. The study is based on small angle X-ray scattering for obtaining the cluster size distribution and volume fraction and on X-ray diffraction for nanocrystalline structures, both performed in grazing incidence mode to enhance the cluster signal. A systematic comparison with cluster size distribution obtained from transmission electron microscopy points out the potential of the technique for investigating these composite glasses. The nanocrystal structure turns out to depend on the relative Co/Ni dose: the ccp structure is preferred at low Ni content, while the hcp structure predominates when increasing the Co content.

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