Electrochemical properties were studied for a single particle of active material of hydrogen storage alloy $(MmNi_{3.55}Co_{0.75}Mn_{0.4}Al_{0.3})$ and nickel hydroxides $(NiOH)_2$ for the secondary Nickel Metal Hydride (Ni-MH) batteries using the microelectrode, which was manipulated to make electrical contact with an active material particle for cyclic voltammograms (CV) and potential-step experiments. As a result of CV test, it was found that three kinds of hydrogen oxidation peaks at -0.9, -0.75 and -0.65 V and hydrogen evolution peak at -0.98 V for hydrogen storage alloy were separately observed and two kinds of peaks of proton oxidation/reduction at 0.45 and 0.32 V and oxygen evolution reaction (OER) at 0.6 V for nickel hydroxides were also more clearly observed. Furthermore hydrogen diffusion coefficient within a single particle was also found to vary the order between $10^{-9};and;10^{-10}cm^2/s$ over the course of hydrogenation and dehydrogenation process for potential-step experiments.