Cubic nanocrystalline Yb:Lu 2O 3 in the size range of 50–100 nm were synthesized by modified Pechini sol–gel method. Differential thermal analysis and thermogravimetric analysis (DTA–TG) were used to study the thermal evolution of the precursor powder. Moreover, together with the results of X-ray powder diffraction (XRD) indicated that the nanocrystals began to crystallize at 773 K. To observe the morphology and the size of the particle, we used the electronic microscopy (SEM and TEM). The optical spectroscopy of the trivalent ytterbium ion in cubic Lu 2O 3 nanocrystals was also measured and discussed.