Metallic thin films Fe/V/Fe/V.../V sequentially deposited under vacuum have been annealed half an hour in room atmosphere. The samples have been characterised by X-rays diffraction (XRD), scanning electron microscopy (SEM), microprobe analysis (EDX), X-ray photoelectron spectroscopy (XPS) and optical absorption. The annealing temperature and the under layer material have been taken as parameters. The results have shown that triclinic phase of FeVO4, homogeneous thin films can be synthesised by this technique. The best results have been obtained when the glass substrate used was coated with SnO2 thin film. The results were improved when, before air-annealing, a first annealing under vacuum was proceeded in order to homogenise the metal distribution in the sample.