New compounds of rare earth complex oxides with perovskite structure in a combination of La with Eu ions and Mn with Zn ions, La1−xEuxMn0·9Zn0·1O3+d (LEMZ) (0·0 ≤ x ≤ 0·32) in A and B sites, respectively were synthesized. X-ray powder diffraction (XRD), fourier transform infrared spectroscopy (FT-IR) and photoluminescence spectra (PL) were used to characterize the resulting nanoparticles. The powder X-ray diffraction peaks could be indexed as a rhombohedral cell. The results of FT-IR spectra were in agreement with those of XRD. High-quality nanopowders with controlled stoichiometry and microstructure were prepared at a temperature range of 700–800°C for 6 h, with mean particle sizes of ∼ 17·5 nm. Photoluminescence measurements showed Eu3+ ions characteristic red emission in crystalline LEMZ powders due to the 5D0 → 7FJ (J = 0–6) transitions of the 4f electrons of Eu3+ ions. The structure, homogeneity and particle size of the obtained compounds during different stages were investigated by scanning electron microscopy (SEM).