A facile aqueous solution route has been employed to synthesize Ba x Sr 1-x SO 4 (0 ≤ x ≤ 1) solid solution nanocrystals at room temperature without using any surfactants or templates. The as-synthesized products were characterized by means of X-ray diffraction (XRD), X-ray fluorescence spectrometer (XRF), scanning electron microscopy (SEM), and differential scanning calorimetry-thermogravimetry (DSC-TG).The Ba x Sr 1-x SO 4 solid solution nanocrystals exhibit an orthorhombic structure and an ellipsoidal-shaped morphology with an average size of 80-100 nm. The lattice parameters of Ba x Sr 1-x SO 4 solid solution crystals increase with increasing x value. However, they are not strictly coincident with the Vegard's law, which indicates that the as-obtained products are non-ideal solid solutions. The Ba x Sr 1-x SO 4 solid solution nanocrystals have an excellent thermal stability from ambient temperature to 1300°C with a structural transition from orthorhombic to cubic phase at about 1111°C.