Using urea and alkali as precipitators,a series of carbonate pillared Ni/Al hydrotalcite were synthesized by hydrothermal methods.The crystal structure and morphology of Ni/Al hydrotalcite were characterized by XRD、FT-IR and TEM.The electrochemical properties of Ni/Al hydrotalcite modified electrode in 0.5 mol/L NaOH electrical media was investigated by cyclic voltammetry and alternating current impedance measurements.The results indicate that the obtained samples synthesized using two different precipitators have the typical layered structure ordering of hydrotalcite and nice crystal forms;Moreover,layered double hydroxides synthesized by homogeneous precipitation through urea hydrolysis have better crystallization than samples using alkali as precipitator;Furthermore,electrochemical reaction in 0.5 mol/L NaOH electrical media occurs under semi-infinite linear diffusion conditions,the stability and the cyclic capability of hydrotalcite modified electrode are related to its crystallinity,the higher the crystallinity is,the better the stability and the cyclic capability are.