To research mixing uniformity of precursor was helpful to improve the quality of the powder late processing. Layered problems of the precursor comprised of aluminium source and of carbon source were well solved by the polymer network method. High quality raw precursor was synthesized by new process which contained polyacrylamide-gel method and carbothermal process. The synthesized precursor was investigated to obtain porous structure precursor. The results showed that sucrose was more suitable for the preparation of AlN precursor. The effect of reaction temperature and heating time on the phase composition of AlN powder were also studied. In this work, ultrafine nano-sized AlN powder was prepared at low temperature.