The fabrication of alloy microelectrodes by electrochemical-etching method is presented. The surface morphology of micro-electrodes is characterized by scanning electron microscopy (SEM) and the effective radius is estimated. Micro-electrode cyclic voltammetry analysis is performed by electrochemical workstation at room temperature. Characterization results show that the best performance of micro-electrode is reached at the conditions of 0.1 mol/L KCl reaction solution and 5 V voltage with the effective radius of 5 m or less. The cyclic voltammetry response curves show that the prepared electrode has good conductivity and good stablity