Photodynamic therapy (PDT) is a promising modern method for treatment of oncological, bacterial, fungal and viral diseases. However, its application is limited to diseases with superficial localization since the body tissues are not transparent for visible light. To address this problem and extend PDT application to abdominal diseases, an enhanced method of X-ray photodynamic therapy (XRPDT) is suggested, involving X-ray radiation easily penetrating the body tissues. The implementation of this approach requires the development of a pharmacological drug including a photosensitizer stimulated by visible light to yield active oxygen and a nanosized phosphor converting X-ray radiation into visible light with the wavelength required for the photosensitizer activation. This study is aimed at obtaining X-ray stimulated phosphors with nanosized particles suitable for XRPDT application. For this purpose, Y2O3:Eu phosphors were synthesized via hydrothermal processing of the corresponding mixed acetate followed by annealing. To prevent from the undesirable agglomeration of the particles in the course of hydrothermal synthesis and subsequent annealing, different techniques were used, including rapid thermal annealing (RTA), microwave annealing and addition of finely dispersed pyrogenic silica (aerosil) to the phosphor. The microwave annealing was carried out using a special installation including a resonance chamber for maintaining a standing wave of microwave radiation. The performed research allowed the determination of hydrothermal processing optimal duration affording the synthesis of phosphors with the highest luminescence brightness. The application of microwave annealing is found to provide phosphors with a more perfect crystal structure compared with RTA. The developed method of Y2O3:Eu phosphor synthesis involving pyrogenic silica addition to the autoclave allowed the preparation of samples with the amorphous structure and significantly reduced the particle size without a considerable decrease in the luminescence brightness. The particle size of the phosphor synthesized with aerosil addition is less than 100 nm that allows its implementation in pharmacological drugs for XRPDT.