Pore shape matters – In-situ investigation of freeze-drying kinetics by 4D XCT methods

Freeze-drying is a commonly employed method in the food industry to extend shelf life of products. However, this process remains time and energy consuming. While higher shelf temperatures accelerate the process, they also pose the risk of product damage. The microstructure of the product, influencing heat and mass transport, is a critical factor. This study aims to understand the impact of 3-dimensional (3D) structural parameters (pore size, shape and orientation) on local primary freeze-drying kinetics. Freeze-drying experiments were conducted with maltodextrin solutions (c₁ = 0.05, c₂ = 0.15 and c₃ = 0.3 w/w) at different shelf temperatures (T₁ = -11, T₂ = -15 and T₃ = –33 °C) with the use of a freeze-drying stage that allows in-situ visualization of the process inside a 4D-X-Ray computed tomography (XCT). The findings show the importance of understanding the microstructure in detail to optimize the sublimation time during the freeze-drying process. It is shown that for longitudinal pores, the orientation is a crucial parameter.