Abstract: In our reseach,paste electrode and powder microelectrode of NiOOH have been fabricated and their electrochemical property have been examined by cyclic voltammetry.The results show that there are one oxidation peak and one reduction peak for the powder microelectrode and only reduction peak for the paste electrode.It indicates that powder microelectrode has better reversibility than the paste electrode.As for the powder microelectrode,its potential and current of the oxidation peak and reduction peak will become stable eventually.It demonstrates the NiOOH sample is very stable.Moreover,the minimum among all △E values is 0.131 V and is smaller than the paste electrode.It illustrates that the powder microelectrode is better than the other electrode for cyclic voltammetry, the NiOOH sample has very stable crystal lattice and better reversibility.Furthermore, the reason for the cyclic voltammetry measurement results difference between paste electrode and powder microelectrode was studied in this paper.