Abstract: Gelcom bustion method has been widely used for synthesizing ultrafine powder because of its advantages of low synthesis temperature and good dispersity.Polycrystalline neodymium doped yttrium aluminum garnet (Nd:Y₃Al₅O₁₂,Nd:YAG) powders were prepared via gel combustion method with metal nitrates as starting materials Four different kinds of fuels (urea glycine glycol citric acid) were investigated. SEM morphologies showed that the resultant powder dispersed best with citric acid as the fuel The evolution of phase composition and morphology of the powders prepared with citric acid were specially characterized by TG-DTA,X-ray powder diffraction and scanning electron microscopy (SEM). The results indicated that nano一sized Nd; YAG powders with an average particle size of approximately 40nm could be directly obtained by calcining the precursor at 850℃ for 2h. No any intermediate phases were formed.The particle size of the Nd; YAG powders became larger with rising of calcining temperature Nd:YAG powders with approximate particle size 60nm could be obtained as calcining the precursor at 1000℃ for 2h.