Ammonia gas was blown into the solution of zirconium ion to induce precipitation of supersaturated zirconium ion at gas-liquid interface with increase in pH. The influence of pH on the phase and particle size of precipitate and calcined powders has been investigated. At pH 4.5 of zirconium solution, maximum yield of 98.7% was obtained. Above pH 4.5, there was no more increase of yield. Above pH 5.5, large aggregates consisting of primary particles were observed in precipitate and calcined powders. At pH 4.5, almost aggregate-free fine spherical zirconia powders were obtained.