The present paper aims to study the formation of electroless Ni-B coatings and evaluation of its structural and thermal characteristics, hardness, corrosion and wear resistance. An alkaline bath having nickel chloride as the source of nickel and borohydride as the reducing agent was used to prepare the electroless Ni-B deposits. XRD pattern reveals that Ni-B deposit of the present study is amorphous in as-plated condition and undergoes phase transformation to crystalline nickel and nickel borides upon heat-treatment. DSC trace exhibit two exothermic peaks around 300 and 420°C, corresponding to their transformation to crystalline'nickel and Ni3B phases and the higher phase compound to Ni3B and Ni2B, respectively. TEM microstructures strongly support the occurrence of phase transitions at these temperatures. The hardness increases with increase in heat-treatment temperature and exhibit two maxima in the hardness-annealing temperature curve. The Ni-B deposits demonstrate a moderate corrosion resistance in 3.5% sodium chloride solution. Heat treatment decreases the corrosion resistance. The wear resistance of electroless Ni-B coatings is governed by the adhesive wear mechanism. The ability of electroless Ni-B coatings to offer high hardness, improved wear resistance and moderate corrosion resistance justifies its role in surface engineering of industrial components. Copyright © 2004 by Society for Advancement of Heat Treatment & Surface Engineering (SAHTSE),.