Aerogels are attracting
increasing interest due to their functional
properties, such as lightweight and high porosity, which make them
promising materials for energy storage and advanced composites. Compressive
deformation allows the nano- and microstructure of lamellar freeze-cast
aerogels to be tailored toward the aforementioned applications, where
a 3D nanostructure of closely spaced, aligned sheets is desired. Quantitatively
characterizing their microstructural evolution during compression
is needed to allow optimization of manufacturing, understand in-service
structural changes, and determine how aerogel structure relates to
functional properties. Herein we have developed methods to quantitatively
analyze lamellar aerogel domains, sheet spacing, and sheet orientation
in 3D and to track their evolution as a function of increasing compression
through synchrotron phase contrast X-ray microcomputed tomography
(μCT). The as-cast domains are predominantly aligned with the
freezing direction with random orientation in the orthogonal plane.
Generally the sheets rotate toward flat and their spacing narrows
progressively with increasing compression with negligible lateral
strain (zero Poisson’s ratio). This is with the exception of
sheets close to parallel with the loading direction (
Z
), which maintain their orientation and sheet spacing until ∼60%
compression, beyond which they exhibit buckling. These data suggest
that a single-domain, fully aligned as-cast aerogel is not necessary
to produce a post-compression aligned lamellar structure and indicate
how the spacing can be tailored as a function of compressive strain.
The analysis methods presented herein are applicable to optimizing
freeze-casting process and quantifying lamellar microdomain structures
generally.