Magnetic ceramic nanoparticles system xNd2O3-(1-x)α-Fe2O3 (x = 0.1, 0.3 and 0.5) was synthesized by mechanochemical activation starting from hematite and neodymium oxide precursors and characterized by X-ray diffraction (XRD) and Mӧssbauer spectroscopy. Rietveld refinement of XRD data evidenced the formation of neodymium orthoferrite NdFeO3 as an end-product with a particle size of about 22 nm, determined using the Scherrer method for x = 0.5. The Mӧssbauer spectra were typically analyzed considering 2 sextets, corresponding to hematite and neodymium orthoferrite and a doublet, representing superparamagnetic particles (SPM). The recoilless fractions were determined using our dual absorber method and were found consistent with a decrease in particle size as consequence of the ball milling process performed.