The effect of gelation on statically and dynamically freeze-cast structures

Freeze-casting is a technique used to produce structures with anisotropic porosity in the form of well-defined microchannels throughout a sample. Here, this technique is used on the magnetocaloric ceramic La0.66Ca0.26Sr0.07 Mn1.05O3. We show that a dynamic freezing profile, where the temperature is decreased continuously at -10 K/min, results in homogeneous, lamellar channels with widths of similar to 15 mu m, while static freezing, where the temperature is kept constant at 177 K, results in channels of increasing size away from the initial ice crystal nucleation site. The effect of gelation before freeze-casting is also investigated. Gelation inhibits ice crystal growth, which significantly changes the morphology by making channel cross sections less elongated, while additionally introducing more dendrites and ceramic bridges in the structure. The latter significantly dominates the flow path through the gelated structures, affecting the calculated tortuosity, which increases to tau approximate to 4 when compared to non-gelated samples where calculated tortuosities are in the range of similar to 1.3 to similar to 3. Finally, we present a systematic and automatic approach for evaluating channel and wall sizes and calculating tortuosities. This is based on analysis of images obtained by scanning electron microscopy using a continuous particle size distribution method and the TauFactor application in MATLAB (R).