The present study describes the synthesis of electroless Ni-P (nickel-phosphorous) coatings on mild steel substrate and optimization of the coating process parameters for minimum friction and wear in acidic (1M H2SO4) solution using Taguchi based grey relation analysis. The study is carried out using different combinations of four coating process parameters, namely, concentration of nickel source, concentration of reducing agent, deposition temperature and annealing temperature with three levels each. The tribological tests are conducted with a pin-on-disk tribometer. Analysis of variance reveals that annealing temperature has the maximum contribution in controlling the friction and wear characteristics of Ni-P coating. The coating is characterized using scanning electron microscopy, energy dispersive X-ray and XRD analysis, respectively. It is found that Ni-P coating is amorphous in as-deposited condition but gradually turns crystalline with heat treatment. Moreover the wear mechanism is found to be abrasive in nature.