Mesoporous material MCM-41 with hexagonal arrangement is obtained by microwave treatment of precursor gel at 100-120 degrees C for 1 h or less, a very short period of time compared with the hydrothermal method. In addition to shorter synthesis time, microwave radiation in the synthesis of MCM-41 provides a way to control its crystallinity and morphology. Especially the addition of small amount of ethylene glycol (EG) in synthetic mixture contributes to improving crystallinity, forming homogeneous particle shape and reducing particle size of MCM-41 under microwave radiation. Attenuated total reflectance (ATR)/FTIR and photoluminescence (PL) spectroscopy have been used to monitor intermediate step of microwave preparation of MCM-41.