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A new type of phosphate compound with different chemical composition but the same framework belonging to NaZr2(PO4)3(NZP) family were synthesized by chelating sol-gel route. The factor that influence on the physical phase was investigated in this paper. The physical phase and pore structure of the synthesized powder materials were characterized by X-ray diffraction (XRD) and N2 adsorptiondesorption respectively. The results showed that the crystalline NZP family compounds CaZr4(PO4)6 and KZr2(PO4)3 which is occupied by Ca2+ and K+ respectively at lattice site of MIcan be prepared by sol-gel route followed with calcinations at 700-800°C for 2h, but when the gel precursor of CaZr4(PO4)6 was treated by hydrothermal crystallization at 160°C for 24h, the obtained powder was NH4Zr2(PO4)3 instead of CaZr4(PO4)6.