Magnesium hydroxide sulfate hydrate whiskers (, abbreviated 513 MHSH) were prepared using hydrothermal reaction with magnesium oxide (MgO) and magnesium sulfate () as the starting materials. The effects of the molar ratio of /MgO and amount of were studied. As a result, 513 MHSH whiskers co-existed with hexagonal plate at low concentration of . The molar ratio of /MgO was 7:1, uniform 513 MHSH whiskers were formed without impurity such as . Appropriate amount of has affected to formation of high quality MHSH. Their morphologies and structures were determined by powder X-ray diffraction (XRD) scanning electron microscopy (SEM) and thermo-gravimetric analyzer (TGA).