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Mono-disperse and micron of porous zirconia spheres were synthesized by the improved process of polymerization-induced colloid aggregation (PICA).In this process,ZrOC12·8H2O was used as raw material with formaldehyde and urea as solidified agents, acetyl acetone was used as stabilizing agent, the optimum process parameters were determined by experiments.Porous zirconia particles obtained after vacuum drying and sintering which had a narrow particle size distribution and appropriate aperture、 pore structure.Phase compositions were mainly tetragonal and monoclinic.Porous zirconia microspheres were also strong enough to withstand the packing of a HPLC column.