Fe-doped In2O3 nanocubes were synthesized by a solvothermal method. The lattice constant a decreases linearly as Fe doping concentration increases, and Raman scattering measurement proves the incorporation of Fe ions into the In2O3 crystal lattice. Mössbauer spectra show the presence of mixed valence of Fe ions instead of Fe3O4, while the sample is superparamagnetic. The products with an average diameter of 80 nm have a single-crystalline phase and appear as a square shape. Magnetic measurements confirm the superparamagnetic properties of the nanocubes, and electron paramagnetic resonance studies indicate Fe ions occupy different sites in the In2O3 matrix.