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Fe(3)O(4) nanoparticles with a size range of 4-8 nm were formed by the spontaneous redox reaction between Fe(3 + ) and multi-walled carbon nanotubes (MWCNTs). Cyclic voltammetry, Raman spectroscopy and x-ray photoelectron spectroscopy were employed to study the thermodynamic and dynamic conditions for the Fe(3)O(4)/MWCNTs formation. It is found that the high defect density of MWCNTs was thermodynamically favorable for the spontaneous reduction of Fe(3 + ) ions and a reaction time of above 2.5 h should be guaranteed. As the catalysts for benzene hydroxylation to phenol, the as-obtained Fe(3)O(4)/MWCNTs exhibit superior catalytic performance to those prepared by the hydrothermal method. Therefore, the spontaneous redox between the Fe(3 + ) and MWCNTs supplies an attractive facile route for the preparation of Fe(3)O(4) nanoscale catalysts.