In order to investigate the reaction in the system of fly ash-sulfuric acid-calcium hydroxide the hydrates were produced by the addition of Ca(OH)2 to fly ash activated with sulfuric acid at various temperatures. And then they were characterized by XRD. SEM and TG-DTA. It was found that in the reaction of fly ash with sulfuric acid fly ash was not decomposed but Al2O3 and SiO2 component in it were activated. The addition of calcium hydroxide into this system resulted in the formation of ettringite and calcium silicate hydrate (C-S-H) As the concentration of sulfuric acid and reaction temperature increased the amount of calcium hydroxide decreased fast. At this time gypsum produced by the reaction calcium hydroxide with sulfuric acid was consumed to form ettringite. Accordingly the formation of ettringite increased with calcium hydroxide and reaction time. And it showed faster than the formation of C-S-H.