The structure, crystallization processes and products of electroless Ni-Fe-P alloy deposits at various heat treatment temperature were studied, with prepared and composition. The deposits were amorphous structure with NaH2PO2 concentration from 18 g/L to 48 g/L. The surface of the deposited specimens was smooth, bright and homogeneous. Heating these deposits from 200 to 700 degree(s)C produces structural changes. A two-step process of crystallization was observed for the amorphous alloys. At first, the crystallization phases were (gamma) -(Fe,Ni) solid solution phases and Ni3Fe, then Ni3P, Fe3P and (Ni,Fe) solid solution phases for high temperature in the films.
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