This is the first report discussing the synthesis of hydrophobic alloy powders consisting of Ni and transition metal nitride (vanadium nitride (VN)) at different proportions through mechanical alloying. The milled alloy powder showed very good resistance to wetting when it was placed in a beaker containing water. The maximum contact angle of 150° with water was recorded for the alloy composition of Ni-75 (wt.%) VN when the powder was loosely sprayed on a glass slide. Few working examples also elucidated the hydrophobic nature of the as-prepared alloy powder. The optimised alloyed powder composition and its phase and morphology as well as the time of milling for maximum hydrophobicity were established with the help of X-ray diffraction (XRD) and field emission scanning electron microscope (FE-SEM) for phase and morphology analysis, respectively. The unique chemistry of toluene with elemental Ni and transition metal nitride VN as characterized by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy led to the development of hydrophobicity in the ball milled powder. © 2019 The Society of Powder Technology Japan