Silicon-containing arylacetylene resins with rigid conjugated structures in the main chain often exhibit poor processability and low mechanical properties.

Two novel bridged silsesquioxane (BSQ) precursors, 1,4-bis(trimethoxysilylpropylthioethenylphenoxy)benzene and 1,3-bis(trimethoxysilylpropylthioethenyl)benzene, were synthesized from arylacetylenes and 3-mercaptopropyltrimethoxysilane through the thiol-yne click reaction. Then, bridged polysilsesquioxane aerogels were prepared from BSQ precursors alone or together with tetramethoxysilane (TMOS) as a co-precursor through the sol–gel method. The resulted aerogels were characterized by scanning electron microscopy, mercury intrusion porosimetry, thermogravimetric analysis, transient hot-wire method, and water contact angle tests. Their mechanical properties were evaluated by unidirectional compression tests. The properties of the aerogels are strongly affected by precursor content, mass ratio of BSQ to TMOS, and the structures of BSQ. The obtained aerogels do not break even when compressive strain is up to 55% and show high compressive modulus (≥2.46 MPa) and hydrophobicity (water contact angle ≥130°).

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