FeVO 4 was synthesised using a low temperature, aqueous precipitation reaction. The material prepared directly from this synthesis was found to be predominantly amorphous and required a thermal treatment. The resultant material was characterised using XRD, FT-IR, Raman spectroscopy and magnetic susceptibility measurements. Materials annealed above 600°C were found to consist mainly of FeVO 4 , although traces of hematite were found following annealing at higher temperatures. Diffuse-reflectance UV spectroscopy and subsequent Tauc plots revealed a band gap of ca. 2.00eV corresponding to an indirect transition. Photocurrent–voltage characteristics recorded under simulated solar illumination indicate that photocurrents are sensitive to annealing temperature and the number of layers deposited on an electrode surface.