Nanocrystals of CePO4:Tb were prepared by reacting the corresponding metal chlorides, phosphoric acid and trioctylamine at 200 °C in tris(2-ethylhexyl) phosphate (TEHP). The samples were characterized by X-ray diffraction and scanning electron microscopy (SEM). The photoluminescence (PL) and the absorption spectra of CePO4:Tb nanoparticles will be presented. The PL spectra are described by using the well-known 5D4 - 7FJ transitions (J = 6, 5, 4, 3 ⋯) of Tb3+ ions with the strongest emission at 543 nm for J = 5. The dependence of PL intensity on Tb3+ concentration has been investigated.