X-ray has the ability to reveal intrinsic sub-nanoscale patterns as the polydispersity of particles in a cluster affects scattering . SAXS measures the X-ray scattering intensity I(q) as a function of the scattering vector q, i.e., I(q) ∝ q -τ , where τ is the scattering exponent. By combining the analyses done by SEM-local thickness, SAXS, and DVS, this experiment aims to establish a reliable method to probe porosity, morphology, and to further the understanding of the porosity of CNC-based cryogels as renewable, biocompatible, and biodegradable porous materials. The CNC suspension used in this experiment was a carboxylated entity obtained from Anomera Inc., produced by oxidation with dilute hydrogen peroxide of dissolving pulp from black spruce. The CNC was used without further purification.