The selectivity of the EXAFS (extended x-ray absorption fine structure) technique was used in order to gain insights on the structural evolution of the Fe and Co environment at different stages of the preparation of FeCo-Al 2O3 aerogels and xerogels. The gels, which were prepared using aluminium tri-sec-butoxide, iron nitrate and cobalt nitrates as precursors, were dried using different procedures in order to obtain xerogels and aerogels, respectively. After drying, the samples are treated either in air up to 900°C or in hydrogen up to 800°C
