A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous to crystal phase was about 850℃. The grain size was increased with the raising of calcine temperature. The alcohol-water ratio did not affect the formation of main crystal phases, but affected the agglomeration of nanoparticles based on the results of TEM. When alcohol-water ratio was 5:1, the dispersion of nanoparticles was good. When there was not alcohol, the dispersion of nanoparticles was poor because there was only pure co-precipitation reaction and the speed of co-precipitation reaction was too high to have enough time of PEG. dispersing particles.