AbstractFoam‐aerogel composites are synthesized in polymeric, hybrid, and ceramic states by completing the open cells of the foam with a solution forming a wet gel, carbon dioxide (CO2) supercritically dried, and pyrolyzed. Thermal diffusivity measurements are conducted using the laser flash, and for mechanical performance, cold crushing tests are done to obtain compressive strengths. Samples possess a range of specific surface area (SSA) values up to ∼650 m2/g contingent upon the material state, that is, polymeric, hybrid, or ceramic. While SSA values can be deliberately altered, almost all samples demonstrated a total porosity of ∼90 vol%, with superb specific compressive strength reaching around 2 MPa. In addition to adjustable surface characteristics granting hydrophobic and hydrophilic features, the study revealed the potential use of these foam‐aerogel composites as thermal insulators with low thermal conductivities of 0.02 W·m−1·K−1 at RT and 0.05 W·m−1·K−1 at 500°C. When exposed directly to a butane flame gun with a flame temperature reaching ∼1200°C, from the backside of a 5 mm‐thick foam‐aerogel composite, only ∼200°C is recorded, which is lower than a comparable commercial insulator panel tested under the same conditions.
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