Calcium sulfate nanorods, nanowires, nanobelts and sheets had been synthesized via a facile solution reaction of CaCl2 and H2SO4 in mixed solvents of ethanol/N, N-dimethylformamide and deionized water at 35°C. The results indicated that well-crystallized CaSO4 nanomaterials with different morphology were obtained by adjusting the volume ratio of ethanol/N, N-dimethylformamide to deionized water and the reaction time. Samples prepared at 35°C in mixed solvents of 50 mL ethanol and 30 mL water for 1 min and 2 h showed nanowire and sheet morphology, respectively. While increasing the volume ratio of ethanol to deionized water to 78/2, only nanorods were obtained. When N, N-dimethylformamide was employed to substitute ethanol, the sample heating at 35°C for 2 h was composed of nanowires in 50 mL N, N-dimethylformamide and 30 mL water. Higher volume ratio of N, N-dimethylformamide to deionized water caused the formation of nanorods.