Autocombustion of citric acid gel was employed to prepare ReFeO 3 (Re = Gd, Nd) nanocrystalline powders. The phase identification and lattice parameters were investigated by the X-ray diffraction (XRD). Fieldemission scanning electron microscopy (FESEM) investigations were carried out to examine the morphology and average size of these powders. Several one phonon lines, two-magnon excitation, and two-phonon scattering have been assigned in their Raman spectra. Both NdFeO 3 and GdFeO 3 nanocrystalline powders were single ReFeO 3 phase, which are agglomerated with average crystallite size of 70-90 nm. The investigations indicated that the autocombustion of citric acid gel method is an effective technology to prepare ReFeO 3 nanocrystalline powders.