Cracking during freeze‐drying in dense freeze cast ceramics: Role of drying rate

Abstract

AbstractCracks can form during the freeze‐drying of freeze cast ceramic suspensions while attempting to produce dense ceramics. The suspensions contain alumina particles dispersed in cyclohexane. The rate of drying is controlled by the pressure and temperature during drying (slow drying at atmospheric pressure and −15°C and fast drying under vacuum while the temperature slowly increases from −80°C to room temperature). X‐Ray micro‐computed tomography was used to characterize internal crack formation. Cracks were found to occur during freeze‐drying rather than during freezing. Both slow and fast drying produced cracks, although two different morphologies were observed. Mechanistic models are proposed for the formation of both types of cracks. The rate of freezing was found to influence the formation of cracks. Slow freezing tended to reduce the formation of drying cracks because the slower freezing produced a more heterogeneous distribution of particles and porous regions, which tends to allow stress to be relieved by opening up existing pores rather than forming cracks in the more homogeneous fast frozen bodies.