The deactivation of nickel hydroxide to the electrooxidation of hypophosphite on a nickel electrode was studied by means of in situ UV-Vis subtractive reflectance spectroscopy. The experimental results show that when the potential is lower than -1.0 V (SCE), the surface on nickel electrode is free of nickel hydroxide, on which hypophosphite is active. When the potential moves positively to about -0.75V, two absorbency bands around 300 nm and 550 nm, which were ascribed to the formation of α-nickel hydroxide, were observed, nickel is oxidized t...