Abstract: A new surfactant——the surfactant Gemini in the series of alkanediyl α,ω bis (dimethylalkyl ammonium bromide) C18 H37 N +(CH3)2(CH2)10 N +(CH3)2C18 H37 ·2Br -, was used as a template in the synthesis of MCM 48 applying microwave radiation. The effect of different factors, such as ratio of raw materials, pH value of reaction medium, power and duration of microwave radiation employed in crystallization and removal of organic template process up on the morphology of the products was investigated. The resulting samples were characterized with such techniques as XRD. The results showed that the reaction time and energy required in the synthesis of MCM 48 mesoporous molecular sieve by the microwave radiation method were greatly reduced in contrast with those needed by the hydrothermal method, and the samples, having pore diameters of around 3 5 nm, displayed a three dimentional mesoporous structure with a short range order.