Coal gangue was activated by means of calcination in seven temperature ranges. Systematic research was made about activation mechanism and structural evolution. Glycerin-ethanol method, SEM, MIP and XRD were used to determine the variation of structure and activation of coal gangue during the calcination. The experimental results show that because of heat treatment in the range of calcination temperature, mineral composition and microstructure of coal gangue are changed. In addition, its activity is improved evidently. The amount of lime absorbed by the sample calcined at 700 °C is 2-4 times that by uncalcined coal gangue in the course of hydration. When NaOH is added to coal gangue-lime system, hydration reaction of the system is sped up and the microstructure of hydrating samples of coal gangue is improved. © 2007 Wuhan University of Technology and Springer-Verlag Berlin Heidelberg.