The activation process of Ni(OH)(2) used as the positive electrode active material of Ni/MH batteries was studied by a single particle microelectrode method thanks to an improved apparatus. The images of the Ni(OH)(2) particle during the charge process were collected. The electrochemical properties of Ni(OH)(2) were studied by cyclic voltammetry and galvanostatic charge/discharge of a single particle. The charge efficiency (eta) of the single particle was as high as 94%. The normalized output rate (NOR) was proposed as a parameter to evaluate the output performance of the electrode material. The NOR value varied with the electrode potential value. But the NOR value remained constant at fixed electrode potential value during the activation process. This implies that the activation process did not improve the reaction rate of the particle, although the capacity kept increasing during the activation process. The intrinsic nature of the activation of Ni(OH)(2) was deduced as the formation of dispersed Ni(III) in the active mass. The Ni(III) phase was formed during the charge process and some remained unreduced during the discharge process. The remaining Ni(III) resulted in a much higher electronic conductivity of Ni(OH)(2). Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.