Different types magnesium hydroxide groups have been obtained using the hydrothermal precipitation technique from magnesium sulfate and calcium carbonate solution. The Mg atom coordinated around O atom of SO42- in another layer to form a multi-layer structure crystal. The influence of synthesis parameters on the morphological characteristics and size of magnesium hydroxide groups precipitated in aqueous were investigated such as different of additive and pH. Magnesium hydroxide groups were decomposed gradually and converted finally to MgO particles after heated in air temperature up to 1050℃. The particle size and it's distribution morphology, crystal phase and thermal behavior of the samples were characterized through XRD, SEM, EDS, and TG/DTA.