In this work, a series of GdFeO 3 nanopowders was successfully synthesized via a reverse co-precipitation technique at different solution temperatures (0, 25 and 50 • C) followed by thermal treatment. Co-precipitated hydroxides and heat treatment products were analyzed using EDXS, DTA-TGA, PXRD, ASA and LD methods. It was shown that the formation temperature of GdFeO 3 nanoparticles varies in the range of 737.5-758.8 • C and total weight loss varies in the range of 23.6-26.4% depending on the temperature of initial solutions. The specific surface areas of nanopowders were found to be strongly dependent on the factor mentioned above and belong to 2.5-16.3 m 2 /g values interval. The hierarchical structure of the obtained nanopowders was established and the effect of co-precipitation temperature on the average crystallite (21.4-34.3 nm), aggregate (46.2-301.2 nm) and agglomerate (33.5-40.9 µm) sizes was discussed in detail.