A series of FeCo-SiO2 granular films of different FeCo atomic concentration (33-54%) have been prepared by fast atom beam sputtering technique and post-annealed in inert (Ar) and reducing (H2) gas environments. Fe and Co K-edge XANES analysis of as-deposited films indicate that both Fe and Co are present mainly in their elemental (Fe 0 , Co 0 ) state. A partial oxidation of Fe and Co is observed, as the FeCo alloy content decreases (54 to 33%) due to reduced particle size. XANES/XAFS analysis shows the formation of FeCo alloy with bcc Fe structure in H2 environment annealed films. The XRD and Raman analysis of Ar environment annealed films suggest the formation of Co3O4 and CoFe2O4 phases. The Ar environment is found not to be effective reducing medium to stabilize the FeCo alloy phase, while H2 environment annealing (450-700 o C) leads to formation of bcc FeCo alloy.