Ti4 was selected to modified PbZrO3, and sol-gel method was used to prepare PZ and PZT (95/5) dried gel powder. XRD results showed that the calcination temperature of PZ is 900℃ with single perovskite structure, while that for PZT (95/5) is 750℃. SEM results showed that PZ is sintered into ceramic when calcined at 900℃ and the grain boundary is obvious. However, the particle size of PZT(95/5) is about 150nm after calcined at 750℃. TEM and EDS results indicated that PZT (95/5) nano-powder with single perovskite structure is antiferroelectric material. The content of Ti4 was determined by ICP-OES.DSC-TGA results illustrated that a large number of Ti4 hydroxyl substances was formed because of the addition of Ti4 . And with the decomposition of Ti4 hydroxyl substances, a large amount of heat was released, which is conducive to the crystallization of PZT(95/5).