Abstract: Electrochemical behavior of hypophosphite was studied with cyclic voltammogram in acidic solution(pH = 4.6) at 80℃. Two anodic peaks were observed on gold electrode at -0.44V and -0.59 V (SCE),respectively, and no corresponding cathodic peaks were obtained. The one at -0.44 V wits ascribed to the oxidation of tautomeric form of hypophosphite, the other at -0.59 V was due to the oxidation of absorbed form of hypophosphite. The two oxidation reactions were believed to be the electron source of nickel ion reduction in electroless nickel processes.