Y2O3 nano-phase powders were prepared by polyacrylamide gel method. The mechanism of polyacrylamide gel process and its calcinations procedure were analyzed. The high purity yttria powders can be produced by polyacrylamide gel method at the calcination temperature of 850°C, which is about 100°C lower than prepared by precipitation method. The microstructure of yttria powders prepared in different proportion of monomer and network agent was investigated. When the mole proportion of monomer and network agent is 5:1, the average size of grains is less than 20nm. Some grains grow abnormally if the proportion deviate from this value and there are a lot agglomerates. Development of such an inexpensive and easy technique for synthesis of high purity yttria nano-phase powders can be of commercial significance.