Abstract—: Gd₂(WO₄)₃ and Gd₂(WO₄)₃:0.5% Tm³⁺, 10% Yb³⁺ nanopowders have been prepared by the Pechini method and solid-state sintering. According to X-ray diffraction results, the materials prepared by the Pechini method are more uniform in phase composition. Optimal synthesis conditions were defined: t = 900°C and τ = 1 h for Gd₂(WO₄)₃ and t = 950°C and τ = 3 h for Gd₂(WO₄)₃:0.5% Tm³⁺, 10% Yb³⁺. The surface morphology of the materials has been studied by scanning electron microscopy. The samples prepared by solid-state sintering have been found to be highly agglomerated, and large agglomerates have been shown to persist even after ultrasonic processing. The average size of the doped and undoped nanoparticles prepared by the Pechini method has been determined to be 44.0 and 47.6 nm, respectively. Luminescence spectra of Gd₂(WO₄)₃:0.5% Tm³⁺, 10% Yb³⁺ were measured and compared the intensities of the Tm³⁺¹G₄ → ³H₆, ¹G₄ → ³F₄, ³F_1,2→³H₆, and ³H₄ → ³H₆ radiative transitions in the materials prepared by both methods. The data obtained in this study demonstrate that the Pechini process is a preferable and promising method for the synthesis of Gd₂(WO₄)₃ and Gd₂(WO₄)₃:Tm³⁺,Yb³⁺ nanopowders.