Mayenite (Ca(12)Al(14)O(33)) is an important material, being used as a transparent conductive oxide (TCO), catalysts for VOCs cleaning and ionic conductor. Unfortunately, the material has a very low BET surface area, generally below 10 m(2)/g and requires higher calcination temperature for the formation of mayenite phase. In this study, a new synthesis method, namely hydrothermal method, was employed for the synthesis of mayenite with higher BET surface area of about 70 m(2)/g, and also the calcination temperature decreased from over 1000 to just 400 degrees C. It was found that mayenite from different method shows different shapes. (C) 2011 Elsevier Ltd. All rights reserved.