Ternary Ni-Co-P and binary Ni-P alloy coatings were deposited on mild steel panels from an alkaline bath in the presence and absence of cobalt sulfate using an electroless process. The effects of heat treatment on surface topography and crystal orientation of Ni-Co(11.17%)-P(3.49%) alloy coatings were studied in contrast to that of Ni-P ones. It was found that the as plated Ni-Co-P alloy is a supersaturated solid solution of P and Co dissolved in a microcrystalline Ni matrix with [111] preferred direction. Heat treatment induces structural changes. The formation of Ni3P phase precipitates and recrystallization of nickel occur when the sample is treated at > 400 degreesC for one hour. It is observed that the Ni diffraction lines of treated Ni-Co-P alloy at > 400 degreesC are shifted to lower angles as compared to those of treated Ni-P or as plated Ni-Co-P alloys. The surface topography of Ni-Co-P alloy also changes with heat treatment temperature. The surface topography and crystal orientation were characterized by means of scanning electron microscopy and X-ray diffraction, respectively. The hardness and corrosion resistance, in 5 wt % NaCl solution, of heat treated Ni-Co-P samples were studied.