Using rare earth coordination polymers with salicylic acid as precursors for the luminescence species Y x Gd 2−x SiO 5 :Eu 3+ , composing the polyvinyl alcohol (PVA) as dispersing media, nanophosphors of Y x Gd 2−x SiO 5 :Eu 3+ (x=0.10,0.25,0.50,0.75,0.90) with different molar ratio of Y and Gd were synthesized by the sol-gel process. Both X-ray diffraction and scanning electronic microscope show that these materials have the nanometer size of 100–200nm. These nanometer materials exhibit red emission at 612nm. When x=0.5, Y 0.5 Gd 1.5 SiO 5 :Eu 3+ shows the strongest emission intensity comparing with other molar ratio of Y to Gd.