The crystallite and particle sizes, morphology and corresponding photoluminescence (PL) properties of nanocrystalline phosphors Y 2 O 3 :Eu 3+ and LaPO 4 :Ce 3+ , Tb 3+ , produced by combustion synthesis, co-precipitation, hydrothermal reaction, sol-gel, spray pyrolysis, and solid-state reaction protocols, are compared. In general, phosphors particles with a relatively large crystallite size with a spherical and agglomerated morphology are favored for emitting the highest PL intensity. However, spray-pyrolyzed particles with a uniform spherical morphology and narrow size distribution produced the lowest PL emission intensity, which is attributed to the small crystallite size. For both compositions, the PL emission intensity increased with increasing crystallite size, but was not dependent on the particle size.