Geopolymers of metakaolin and sodium silicate were synthesized respectively with the ratios of the amount of SiO2 in the sodium silica solution to that of Al2O3 in metakaolinite equal to 1.0, and 0.66. The geopolymeric structures of the products were investigated by 27Al and 29Si solid-state nuclear magnetic resonances with magic-angle spinning (MAS NMR), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), differential scanning colorimetry (DSC) and scanning electron microscopy (SEM). The reaction of the Al-O sheet in meakaolinite with low-order polymerized Si-O tetrahedral units such as monomer of SiO4 yields three-dimensional structures with the Q3 Si-O tetrahedral structure and the coordination of Al(IV) in the Al-O tetrahedral structure. The geopolymers are essentially X-ray amorphous. The assays by 27Al and 29Si NMR, FTIR confirm that the active structure in the metakaolinite is the sheet of Al-O with three coordination states.
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