Freeze-drying with structured sublimation fronts-visualization with neutron imaging

The particular structure of the sublimation front in vacuum freeze-drying of porous media is, in most situations, not accessible at the pore scale. The classical measurement techniques access the process only globally. Knowledge about the structure of the front, however, is necessary for prescriptive analysis of freeze-drying, as it dictates not only drying velocity, drying time, and overall energy consumption, but also the material properties after drying. This is especially relevant in situations in which the freeze-drying process is carried out close to the collapse temperature of the product. We, therefore, study the sublimation of ice with neutron tomography and analyze the spatial formation of the dry space using the example of frozen cylindrical maltodextrin with drying parameters at the limit of material collapse. We show that the sublimation front forms unique fractal structures that differ strongly from the usual form of a flat front. Distinct dry fingers covering the sample, in addition to a fractal peripheral sublimation front, were observed. The findings are important for the understanding of freeze-drying processes and will serve as a basis for the development of microscale models of freeze-drying.