In this research, NixTiy compound was prepared by thermal treatment of Ni-plated Ti powder. For this purpose, Ti powder was plated in an electroless Ni bath for various times (120, 225, 300, and 720min). Hydrazine hydrate was used as a reductant for the deposition of pure Ni on the Ti particles. The plated powder (225min) was heat treated under argon atmosphere to achieve NixTiy powder. Finally, the heated/plated powder was pressed by CIP followed by sintering at 980 degrees C for prepare the NixTiy bulk sample. The plated powders as well as sintered one were characterized using scanning electron microscopy, energy dispersive spectrometer, X-ray fluorescence, X-ray diffraction and differential scanning calorimetric. The NiTi2, NiTi, and Ni3Ti phases were detected in the XRD patterns of heated/plated Ti powder. According to DSC data, the heated/plated Ti powder showed reversible martensitic transformation at temperature range of -38.0 degrees C to +38.1 degrees C, while sintered/heated/plated Ti powder displayed reversible transformation at temperature range of 16.0 degrees C-15.4 degrees C.