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We report the results of the Ni-based bulk metallic glass structuralevolution and crystallization behavior in situ investigation. The X-raydiffraction (XRD), transmission electron microscopy (TEM), nano-beamdiffraction (NBD), differential scanning calorimetry (DSC), radial distributionfunction (RDF) and scanning probe microscopy/spectroscopy (STM/STS) techniqueswere applied to analyze the structure and electronic properties of Ni63.5Nb36.5glasses before and after crystallization. It was proved that partial surfacecrystallization of Ni63.5Nb36.5 can occur at the temperature lower than for thefull sample crystallization. According to our STM measurements the primarycrystallization is originally starting with the Ni3Nb phase formation. It wasshown that surface crystallization drastically differs from the bulkcrystallization due to the possible surface reconstruction. The mechanism ofNi63.5Nb36.5 glass alloy 2D-crystallization was suggested, which corresponds tothe local metastable (3x3)-Ni(111) surface phase formation. The possibility ofdifferent surface nano-structures development by the annealing of theoriginally glassy alloy in ultra high vacuum at the temperature lower, than thecrystallization temperature was shown. The increase of mean square surfaceroughness parameter Rq while moving from glassy to fully crystallized state canbe caused by concurrent growth of Ni3Nb and Ni6Nb7 bulk phases. The simpleempirical model for the estimation of Ni63.5Nb36.5 cluster size was suggested,and the obtained values (7.64 A, 8.08 A) are in good agreement with STMmeasurements data (8 A-10 A).

In situ visualization of Ni-Nb bulk metallic glasses phase transition