Here, we report the preparation of Ce(3+) and Tb(3+) co-doped sodium yttrium fluoride nanorods and NaYF(4):Ce(3+)/Tb(3+) core-shell nanoparticles by the emulsion method. The core-shell nanoparticles are confirmed by X-ray diffraction study and transmission electron microscopy (TEM) analysis. The hexagonal crystal phase of Ce(3+)-doped sodium yttrium fluoride nanocrystals is converted to the cubic polymorph after surface coating by TbF(3). Cell volume, cell parameters and lattice strain have been modified due to core-shell structure. The decay times are found to be 8.4 ms and 5.4 ms for doped nanorods and core-shell nanoparticles, respectively, which reveals that non-radiative decay is higher in the case of core-shell nanoparticles than doped nanorods. Energy transfer efficiencies from Ce(3+) to Tb(3+)are 65% and 45% for doped Na(Y(1.5)Na (0.5))F(6):Ce:Tb material and NaYF(4):Ce/Tb core-shell materials, respectively. Quantum yields are found to be 75% and 42% for doped and core-shell samples, respectively.