Mixed oxides nanocomposites of the type xCr 2 O 3 -(1-x)α-Fe 2 O 3 (x = 0.0-1.0) were synthesized using hydrothermal technique and characterized by X-ray diffraction (XRD) and Mössbauer spectroscopy. The same characterization methods were applied to a set of samples annealed at 600 • C for 2 h. High chromium content correlated with occurrence of amorphization effects and onset of superparamagnetism in the as-obtained samples. The structure and properties of the thermally annealed samples, however, are dominated by the equilibrium of two phases, Cr:Fe 2 O 3 and Fe:Cr 2 O 3 . The final (x = 1.0) particle size of the nanocomposite is close to 19 nm.