Nickel ferrite (NiFe2O4) and manganese ferrite (MnFe2O4) have been prepared by a soft mechanochemical route from mixture of (1) Ni(OH)2 and α-Fe2O3 and (2) Mn(OH)2 and α-Fe2O3 powders in a planetary ball mill. The mixture was activated for varying duration. Soft mechanochemical reaction leading to formation of the NiFe2O4 and MnFe2O4 spinel phases were followed by X-ray diraction, Raman and infrared spectroscopy, scanning and transmission microscopy. The spinel phase formation was rst observed after 4 h of milling (case 1) and after 3 h (case 2) and its formation was completed after 25 h in both cases. The synthesized NiFe2O4 and MnFe2O4 ferrites have a nanocrystalline structure with a crystallite size of about 30 and 40 nm for cases (1) and (2), respectively. There are ve Raman and four IR active modes. In order to understand better the whole process of phase formation, the Mössbauer measurements were done.

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