Yttrium orthoferrite (YFeO 3 ) powder was prepared by a mechanochemical synthesis from a mixture of Y 2 O 3 and α-Fe 2 O 3 powders in a planetary ball mill for 2.5 h. The obtained YFeO 3 powder sample was characterized by X-ray diffraction (XRD), Raman and infrared spectroscopy. The average crystallite size calculated by the Scherrer equation was 12 nm. The Mössbauer spectroscopy at room temperature confirms the superparamagnetic character of YFeO 3 orthoferrite sample.