In order to comprehensively utilize coal gangue as the main raw material in cementitious materials, improving its cementitious activity is a question of fundamental importance. In this paper, we present a new compound mechanical-hydro-thermal activation (CMHTA) technology to investigate the activation effect of coal gangue, and the traditional mechanical-thermal activation (TMTA) technology was used as reference. The purpose of this study is to give a detailed comparison between these two methods with regard to the mineral composition, crystal structure and microstructure, by XRD, IR, MAS NMR, XPS and mechanical property analysis. The prepared coal gangue based blended cement, containing 52% of activated coal gangue C (by CMHTA technology), has a better mechanical property than activated coal gangue T (by TMTA technology) and raw coal gangue. The results show that both of the TMTA and CMHTA technologies can improve the cementitious activity of raw gangue greatly. Moreover, compared with TMTA, the mineral phases such as feldspar and muscovite in raw coal gangue were partially decomposed, and the crystallinity of quartz decreased, due to the effect of adding CaO and hydro-thermal process of CMHTA technology. (C) 2010 Elsevier B.V. All rights reserved.