Gd3Ga5O12(GGG) precursor was synthesized by a co-precipitation method using ammonium hydrogen carbonate as precipitator. TG-DTA and IR spectra indicated that the precursor was alkaline and the weight loss during calcination was 28.06%. The results of XRD analysis indicated that the polycrystalline powder was well-crystallized after calcination at 1000℃ for 3h. Compared with the solid-state reaction, the carbonate co-precipitation had the merits of short reaction period, well-crystallization, low calcining temperature, and less volatilization. As a result, the volatilization and disproportion of Gd2O3 and Ga2O3 could be well controlled during crystal growth and the optical quality of single crystal was also improved.