Zirconium 1,4-butylenediphosphonate[Zr(BDPA)] multilayers on a 3-mercaptopropylphosphonate-coated gold electrode were prepared by the conventional layer-by-layer method.The stability of the Zr(BDPA) multilayers in different supporting electrolyte solutions was studied by cyclic voltammetry (CV) and X-ray photoelectron spec-troscopy(XPS) measurements.The results show that the Zr(BDPA) multilayers are very stable in 0.2 mol·L-1 KCl,0.2 mol·L-1 KNO3 and low concentration phosphate buffer solution(PBS) with low pH values(c≤0.05 mol·L-1,pH≤ 6.8).While in high concentration 0.2 mol·L-1 PBS(pH=5.2~7.4),the Zr(BDPA) multilayers will be partially desorbed within two days,possibly due to the formation of more stable zirconium phosphate.