Nanoparticles, bulk and thin films of NiFe2 O4 compounds are studied by micro-Raman spectroscopy. The effect of varying the incident laser power up to 40 mW was studied in all forms of the samples. The spectra showed a large magnitude of red shift and line broadening as a result of high incident laser power. It is shown that the inverse spinel structure remains robust, and no trace of laser-induced oxidation was observed. The low-temperature study of the bulk and nanoparticles has also been carried out for elucidating thermal effects due to the high incident laser power. The rise in temperature for maximum incident laser power of 40 mW was estimated to be ∼625 °C. Copyright © 2010 John Wiley & Sons, Ltd.