Electrochemical impedance spectroscopy (EIS) was applied for a single mesocarbon microbead (heat-treated at 1000°C) of 30 μm diameter during Li-ion insertion and extraction using a stainless tip-microelectrode in the electrolyte of 1 M LiClO4/propylene carbonate+ethylene carbonate. Obtained spectra were analyzed with an equivalent circuit model. Kinetic parameters such as the charge transfer resistance, and the apparent chemical diffusion coefficient of Li-ion in the particle were evaluated without interference of organic binders. The charge transfer resistance decreased and chemical diffusion coefficient of Li-ion increased as the electrode potential was made more negative. The chemical diffusion coefficient varied within 10−12–10−6 cm2 s−1.