Characterization and Selection of Metakaolin for Reproducible Geopolymer Matrices: A Thermal Evolution Approach

The HYPEX® process is a novel method for conditioning spent ion exchange resins from nuclear power plants, aiming to reduce final waste volume and carbon emissions by stabilizing the resins in metakaolin-based geopolymers. This study addresses the challenge posed by the natural variability of commercial metakaolin and defines a testing strategy to ensure consistent performance of the final matrix. The reactivity of two batches of metakaolin, characterized by comparable chemical composition and BET surface area, was evaluated by monitoring temperature evolution during geopolymerization at varying water-to-solid ratios. The resulting geopolymers were tested for compressive strength, water permeability, and strontium leachability to assess correlations between precursor properties and final matrix performance. Despite similar compositions, the two batches showed marked differences in compressive strength that could be linked to early thermal behavior. These findings demonstrate that conventional precursor characterization is insufficient to guarantee reproducibility and that thermal profiling is useful to predict mechanical performance. The results suggest the implementation of thermal response monitoring as a quality control tool to ensure the reliability of geopolymer wasteforms in nuclear applications. A simplified analytical model for the thermal evolution during geopolymerization was also developed, matching qualitatively the measured evolution, to suggest scale-up rules from laboratory specimens to full-scale drums, which should be achieved while preserving the thermal evolution.