Silicon (Si) fertilizer is of great signi cance to modern agricultural production; the citrate-soluble silicon fertilizer based on coal gangue is one way to protect the environment and meet the agricultural needs of China. In this study, we produced high-e ciency coal-gangue based silicon fertilizer by calcining a mixture of coal gangue, calcium carbonate (CaCO 3 ) and corn stalk powder at high-temperature (i.e., high-temperature activation technology); the effect of temperature and mixing ratio on the available-Si content of activated coal gangue was studied, followed by an analysis of the mechanism of available-Si formation. The results showed that the layered structure of coal gangue was severely damaged above 600 ℃, and the kaolin began to transform into metakaolin and other substances, where the available-Si content was not high (less than 10%). When CaCO 3 alone was added, the peak intensity of quartz and muscovite in coal gangue decreased signi cantly with the increase of CaCO 3. However, CaCO 3 mainly played a catalytic role in the entire calcination and activation process, forming only a small amount of calcium silicate on the contact surface with coal gangue; however, the available-Si content was still below 12.60%. When corn stalk powder alone was added, the oxides of the corn stalk ash participated in the chemical reaction involving coal gangue, forming nepheline (K(Na, K) 3 Al 4 Si 4 O 16 ) and other silicates, and the available-Si content was signi cantly higher than that with CaCO 3 . When coal gangue, CaCO 3 , and corn stalk powder were mixed and calcined, the available-Si content was as high as 22.97% under the synergistic effect of CaCO 3 and corn stalk powder; the concentration of harmful heavy metals was below 0.025 mg/L. The above is in line with the requirements of silicon fertilizer for use in agriculture, thus con rming the preparation of coal gangue-based silicon fertilizer in an e cient manner.