The synthesis of Nd 3+ doped lithium lanthanide tetraphosphate (LiLaP 4 O 12 ) nanocrystalline powders was presented. Their structure, morphology and spectroscopic properties are determined. The luminescence properties of LiLa 1− x Nd x P 4 O 12 nanocrystalline powders were studied as a function of concentration of Nd 3+ ions. The fluorescence branching ratio of 4 F 3/2 → 4 I J transitions were strongly dependent on Nd 3+ concentration what was associated with self-absorption of the resonant fluorescence R 1 →Z 1 transition. It was found that the fluorescence quenching rate has demonstrated a linear concentration dependence.