Investigation of structural collapse in unidirectionally freeze cast collagen scaffolds

Though unidirectional freeze casting is a facile method for the production of structurally anisotropic biomedical scaffolds, challenges exist in optimizing the drying process that are often overlooked. In particular, structural collapse may occur if the material's frozen-state glass transition temperature (Tg') is exceeded. It was discovered that unidirectionally freeze cast collagen matrices were highly deformed following lyophilization, rendering them incapable of further use. In this study, modulated differential scanning calorimetry was performed to identify Tg's of unidirectionally freeze cast collagen scaffolds, and product temperatures during sublimation were recorded. It was observed that cast matrices from 0.5 to 0.05 M acetic acid (HAc) sublimed at a lyophilizer shelf temperature of -25 °C underwent structural collapse and exceeded their Tg's for the majority of the drying cycle. The use of a low pH suspension (0.5 M HAc) promoted the formation of a non-porous surface, which in turn contributed to the increase of the product temperature above its Tg' during drying. This study has revealed that use of a low shelf temperature (-40 °C) and a low HAc concentration (0.05 M) is effective in maintaining product temperatures under Tg' thereby preventing collapse in unidirectionally freeze cast collagen scaffolds.