Insights into freeze-cast hierarchical water–glass foams via in situ time-lapse phase-contrast enhanced microcomputed tomography: Correlating composition, microstructure, and compression failure

Abstract

We demonstrate how continuous freeze-casting without post-treatment sintering may be successfully employed using a pure water–glass (WG) solution to fabricate hierarchically porous foams lacking a morphology gradient along the freeze direction. By adjusting the water content (dilution) and/or the alkali ratio of the solution, we achieved lamellar structures with sub-features or cellular structures, with porosities spanning ∼65% to 83%. The WG foams exhibit astounding mechanical properties; notably, foams with a relatively low density of ∼0.33 g/cm3 demonstrated the highest compressive strength (5 MPa), due to their microstructure and pore morphology. In situ uniaxial compression tests combined with phase-contrast enhanced micro-computed tomography in a synchrotron revealed bending, buckling, fracture and splitting of the lamellar structures as main failure mechanisms. Our newly developed approach of continuous freeze-casting of pure WG solutions with an improved understanding of the relationship between composition, structure, and failure mechanisms provide a basis for a customized design and manufacture of a wide range of freeze-cast WG-based materials for applications ranging from biomedicine to energy generation and storage.

Keywords

• Water glass
• Continuous directional freeze casting
• Microstructure
• Hierarchical porosity
• In situ mechanical testing
• Phase contrast-enhanced tomography