A new single micro-particle electrode(SMPE)fabrication technique the inlaid SMPE technique was introduced in this paper.The preparation procedure of an alloy SMPE was described in detail.Based on the SMPE technique,the electrochemical behavior of LaNi_ 4.7Al_ 0.3 spherical particles with two different radii was investigated.The results of CV study showed that more detailed electrochemical information of the alloy can be provided on the alloy SMPE as compared with that on the composite alloy electrode.The results of potential step study depict that H diffusion coefficient in LaNi_ 4.7Al_ 0.3 keeps almost constant when the size of the alloy particle changes,and the diffusion coefficient measured on the alloy SMPE[(2.5—2.6)×10-9 cm 2/s] is about one order larger than that detected on the composite alloy electrode.