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Single crystal scintillators are widely applied in many areas of science and technology. Production of single crystal scintillators is a rather complex, long-standing and power-intensive process. As an alternative to single crystals scintillation ceramic materials made of nanocrystalline powders were being considered. Sol-gel and co-precipitation methods have been used for establishing possibilities of fabricating rare earth metal ion-doped scintillators. By these methods, if modified, it is possible to regulate sizes of powder particles. Finely dispersed powders of single-phase lutetium silicates, titanates, aluminates, tungstates, molybdates and other materials were synthesized. Main goal of the present work was to study the influence of different factors on purity of LSO and LPS phases. Pyrolysis procedure of amorphous gels promoted formation of phase mixtures (LSO, LPS, Lu2O3 and SiO2) due to disturbance of the Lu:Si ratio under the influence of fluorine- and chlorine-containing compounds. Optimum modes for preparing nanophase powders of Ce3+-doped lutetium silicates (LSO, LPS) were defined. The synthesized samples were studied by using X-ray diffraction, electron microscopic and thermal analysis methods. LPS luminescence characteristics were established.