In this research, we report on the characterization of La1−xTbxMn0.9Zn0.1O3+d (LTMZ) (0.0≤x≤0.32). Nanoparticles with high surface area were synthesized by the polymerized complex method based on the Pechini-type reaction. High-quality nanopowders with controlled stochiometry and microstructure were prepared in the temperature range of 700–800 °C for 6 h, with mean particle sizes of approximately 18.35 nm. The synthesized materials were characterized by X-ray powder diffraction, fourier transform infrared spectrometry and photoluminescence (PL). PL measurements showed the characteristic green emission of Tb3+ ions in crystalline LTMZ powders due to the 5D 4→7F J transitions of the 4f electrons of Tb3+ ions. The structure, homogeneity and particle size of the obtained compounds during different stages were investigated by scanning electron microscopy.