Synthesis of porous hierarchical geopolymer monoliths by ice-templating

Hierarchical geopolymers with mesoporous matrices and lamellar macro-porosities were produced for the first time by ice-templating (freeze-casting) technique in a water-based sol-gel system. Starting from an aqueous solution of metakaolin and potassium silicate, geopolymerization was triggered through a maturation step without reaching complete consolidation. Different amounts of water (20, 50, 70 vol.%) were then mixed with the geopolymer paste to induce lamellar ice growth by unidirectional freezing. The consolidation was completed during freeze-casting and drying. Ice-templated hierarchical geopolymers had 53-83% total porosity and N<inf>2</inf> BET specific surface area values from 4 to 46 m² g^-1, depending on the amount of water added. A broad mesopore Barret Joyner Halenda distribution was detected between 4 and 100 nm with maxima from 5 to 7 nm, while macropores in the 1-to-100 ?m range were identified by Hg intrusion porosimetry. Lamellar monoliths (height 25 mm) were produced with a selected composition (50 vol.% of additional water) in order to assess the reproducibility of the ice-templating technique combined with geopolymerization.