During the last 10 years the number of works related to the development of new light-emitting nanoparticles has increased. One of the research interest based on new materials is substitution of organic dyes in the tunable laser systems with inorganic fluorophore such as lanthanide compounds that can be more stable host material. Within this direction, nanostructured Bi-3d metal mixed-oxides of bismuth-transition display increasing interest. This work deals with photoluminescent properties of two most perspective oxides Bi1.854Pr0.146O3 and BiTbO3 from earlier studied Bi(III)-Ln(III) heterometallic oxides [1]. The phases were obtained by decomposing the solid precursors in two stages. This synthesis method made possible the preparation of nano-sized particles in a short time and at relatively low temperature (~ 700 °C). Bi1.854Pr0.146O3 oxide was obtained upon thermal treatment of PrBi(cdta)(NO3)2·7H2O and PrBi(dtpa)NO3·10H2O precursors (cdta4- = 1,2-cyclohexane-N,N'-diaminetetraacetate and dtpa5- = diethylenetriaminepentaacetate ions) while BiTbO3 oxide was obtained by decomposing TbBi(dtpa)NO3·10H2O coordination compound. The powdered materials have been studied in shape of compressed tablets. The dimensions of some of the particles were of about tens nanometers. The photoluminescence spectra of Bi1.854Pr0.146O3 and BiTbO3samples were investigated in the visible and near infrared spectral regions at room temperature. Luminescence was excited by the solid-state laser YAG: Nd, λex = 0,532 μm. The used sensors was photomultiplier FAU-62 and photo resistor PbS. The exciting radiation was focused on the sample to obtain the density power from 0.5 to 5.5 kW/cm2. Physical properties of the materials proved to be closely related to their size and morphology. The results of the investigation demonstrated distinct dependence of the emitting properties of hetero-metal oxide systems from the initial organic ligand. The samples Bi1.854Pr0.146O3 displayed intense photoluminescence in the near infrared region having a complex PL spectrum. On the short-wave decay besides the intensity of the peak at 1095 nm there is a feature at the 900 nm (curve 1.).In the IR spectrum except intense line at 1555nm is observed maxima at 1361nm and 1780nm (curve 2). It was found that the luminescence intensity depends greatly on the time of irradiation. When the power density of exciting laser radiation is 5.5 kW/cm2, the luminescence intensity decreased at about 8-10 times within 3 minutes of irradiation, leaving after that a stable level of intensity. However such a decrease of the luminescence intensity was not observed when the laser irradiation intensity was reduced 3 times. Thus this effect has a threshold character. The phenomena of decreasing in emitting intensity may be caused by the re-organization of the oxides nanostructure, change of their size or the order of structure as a result of heating during intense laser radiation.All the spectra were recorded after five minutes of irradiation of oxides with power density of about 1.5 kW/cm2. The study of luminescent spectra of heterometal oxide systems with rare earth elements is very interesting due to their light emissive properties. These materials can be used in the new class of device structures based on transparent polymers that may be ideal candidates for the role of the host material in the photoactive particles.