Multiphase imaging of freezing particle suspensions by confocal microscopy

Ice-templating is a well-established processing route for porous ceramics. Because of the structure/properties relationships, it is essential to better understand and control the solidification microstructures. Ice-templating is based on the segregation and concentration of particles by growing ice crystals. What we understand so far of the process is based on either observations by optical or X-ray imaging techniques, or on the characterization of ice-templated materials. However, in situ observations at particle-scale are still missing. Here we show that confocal microscopy can provide multiphase imaging of ice growth and the segregation and organization of particles. We illustrate the benefits of our approach with the observation of particles and pore ice in the frozen structure, the dynamic evolution of the freeze front morphology, and the impact of PVA addition on the solidification microstructures. These results prove in particular the importance of controlling both the temperature gradient and the growth rate during ice-templating.Comment: 20 pages, 9 figure

The Freezing Rotation Illusion

The freezing rotation illusion arises when a figure is continuously rotating in front of a back and forth rotating ground. The term “freezing rotation” designates the decrease in the perceived rotation speed of a figure when the figure and the ground are turning in equal directions. Subjects had to estimate the rotation speed of a continuously turning figure while the ground was either turning opposite to or with the figure. Their estimations of the figure’s speed were significantly lower, when the ground was moving in the same direction as the figure. In control experiments subjects had to estimate the ground’s speed while the figure was turning opposite to or with the ground. Overall, their estimations of the rotational speed of the ground were not significantly influenced by the rotational direction of the figure

Particle-scale structure in frozen colloidal suspensions from small angle X-ray scattering

During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has mostly concentrated on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle-scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small angle X-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by any standard inter-particle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium or steady-state densification processes

Boundary-induced inhomogeneity of particle layers in the solidification of suspensions

When a suspension freezes, a compacted particle layer builds up at the solidification front with noticeable implications on the freezing process. In a directional solidification experiment of monodispersed suspensions in thin samples, we evidence a link between the thickness of this layer and the sample depth. We attribute it to an inhomogeneity of particle density induced by the sample plates. A mechanical model enables us to relate it to the layer thickness with a dependency on the sample depth and to select the distribution of particle density that yields the best fit to our data. This distribution involves an influence length of sample plates of about nine particle diameters. These results clarify the implications of boundaries on suspension freezing. They may be useful to model polydispersed suspensions since large particles could play the role of smooth boundaries with respect to small ones.Comment: 16 pages, 13 figure