Effect of the Support on the Formation of FeCo Alloy Nanoparticles in an SBA-16 Mesoporous Silica Matrix: An X-ray Absorption Spectroscopy Study

A series of nanocomposites consisting of FeCo alloy nanoparticles supported on a three-dimensional cubic mesoporous silica matrix (SBA-16) were prepared by wet impregnation of the matrix with a solution of Fe and Co nitrates. Fe Co alloy nanoparticles were obtained by heat treatment at 800 degrees C in reducing atmosphere of the impregnated SBA-16 previously calcined at 500 degrees C. Three different SBA-16 types were used as a support of the nanophase. The influence of the matrix on the absorption of Fe and Co ions was investigated using X-ray diffraction and X-ray absorption spectroscopy. In particular, extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES) techniques at the Fe and Co K-edges were used in order to identify the intermediate products before reduction and to study the formation of the bcc FeCo alloy, which cannot be assessed unambiguously using X-ray diffraction. An important influence of the matrix has been observed in the phases formed before reduction, in the size of nanoparticles, and in the oxidation of the FeCo alloy nanoparticles.