Usually, heat-treated electroless NiP deposits (NiP) were cooled using air quenching (AQ) process for enhancing its surface properties. As of now, no research work reported the surface characteristics of heat-treated NiP followed by water quenching (WQ) process. Hence, a novel attempt has been made to report the preliminary investigation on the properties of WQ-NiP. The deposits were heat treated (400°C, 500°C, 600°C and 700°C) at the rate of 0.5°C/s followed by air and water cooling. Comparative investigations have been made between the as-plated, AQ-NiP, WQ-NiP in terms of phase structure, crystallite size, residual stress, rockwell hardness, microstructure, and work of adhesion. Additionaly, the failure mechanisms of various heat-treated NiP during indentation were investigated and reported in this article. There is a restriction observed in the growth of crystallite for WQ-NiP as compared to the as-plated and AQ-NiP. The solubility of the intermediate phases has induced compressive residual stress for both AQ-NiP and WQ-NiP at 600°C and 700°C. Nickel oxide precipitate was observed in the microstructure of AQ-NiP and WQ-NiP heat treated at 700°C. The work of adhesion is considerably increased for WQ-NiP as compared to AQ-NiP. Maximum hardness of about 53.7 HRC was obtained for WQ-NiP treated at 400°C. © 2021