Calcium carbide residue (CCR) is a solid waste resulting from acetylene gas production. In this study, CCR was used as an alkali activator to prepare fly ash (FA)-based geopolymers without any alkali supplementation. We studied the factors (FA/CCR ratio, curing temperature, and water/binder ratio) influencing the mechanical property of FA/CCR-based geopolymers. The compressive strength results showed that, by optimizing these three factors, the FA/CCR mixture has great potential for use as a cementitious material and geopolymer with a dense microstructure having a maximal compressive strength of 17.5 MPa. The geopolymers’ chemical structure, microstructure, and chemical composition were characterized and determined by a combination of techniques. All these results revealed that amorphous C-(A)-S-H (calcium (aluminate) silicate hydrate) gels mainly formed after geopolymerization resulting from the reaction of FA and CCR. In addition, some crystallines, such as ettringite and monosulfate, were also formed. Further, geopolymers prepared with a suitable FA/CCR ratio (1:1 or 1:2) possessed a compact microstructure because of their sufficient reactive SiO₂ and Al₂O₃ and high-enough alkalinity, responsible for higher content of C-(A)-S-H formation and better mechanical property. Too high curing temperature or water content induced the formation of a loosely bound geopolymer matrix that strongly weakens its mechanical property.

As 1:1 dioctahedral clay minerals, kaolinite and halloysite have similar chemical compositions. However, halloysite often possesses a nanotubular structure and special surface reactivity compared to platy kaolinite. The objective of this current work was to determine the effect of the SiO₂/Al₂O₃ ratio on the microstructure and properties of geopolymers derived from two kinds of kaolin: platy kaolinite and nanotubular halloysite. The chemical structures and compositions of the geopolymers obtained were characterized through X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy, and nuclear magnetic resonance (NMR), whereas the microstructural analysis was performed by scanning electron microscopy (SEM), the Brunauer–Emmett–Teller (BET) method, and N₂ physisorption analysis. The results indicated that calcined halloysite showed greater geopolymerization reactivity than calcined kaolinite. In addition, the mechanical properties of the clay-based geopolymers depended not only on the SiO₂/Al₂O₃ ratio but also on the morphology of the clay. Crystalline zeolite A and geopolymer were produced after alkali-activation of kaolin with a SiO₂/Al₂O₃ ratio of 2.5; these products possessed porous and heterogeneous microstructures having poor compressive strength. As SiO₂/Al₂O₃ ratios increased to >2.5, geopolymers with compact microstructure and high compressive strength were produced after alkali-activation of kaolin. Notably, at a given condition, halloysite-based geopolymers exhibited greater early compressive strength, more compactness, and more homogeneous microstructure than kaolinite-based geopolymers. This can be attributed to the nanotubular microstructure of halloysite, which can release more Si and Al during alkali activation than platy kaolinite. These results indicated that the various morphologies and microstructures among clays have significant impact on the microstructure and compressive strength of geopolymers.