In the present talk, mechanistic aspects of the electroless nickel-phosphorus (Ni-P) deposition process using sodium hypophosphite as reducing agent will be discussed. We will focus primarily on the mechanism of hydrogen evolution during electroless Ni-P deposition. The role of pH and reducing agent concentration on the kinetics of hydrogen evolution will be discussed. A combination of volumetric analysis of the hydrogen evolved, titration analysis of the hypophosphite consumed and compositional gas analysis when using D₂O and H₂O as solvents shows that hydrogen evolution proceeds primarily via hydrolysis of the reducing agent rather than electrolysis of water. Mechanistic aspects of the reductant hydrolysis reaction will be investigated using a rotating disc electrode to unravel the role of surface kinetics and mass transport on the hydrogen generation process. Findings will be incorporated into a simple mathematical process model. Implications of the present study to improved process design for electroless deposition of amorphous alloys will be discussed.