This study introduces a new synthesis route for obtaining homogeneous chitosan (CS)-silica hybrid aerogels with CS contents up to 10 wt%, using 3-glycidoxypropyl trimethoxysilane (GPTMS) as coupling agent, for tissue engineering applications. Aerogels were obtained using the sol-gel process followed by CO₂ supercritical drying, resulting in samples with bulk densities ranging from 0.17 g/cm³ to 0.38 g/cm³. The textural analysis by N₂-physisorption revealed an interconnected mesopore network with decreasing specific surface areas (1230–700 m²/g) and pore sizes (11.1–8.7 nm) by increasing GPTMS content (2–4 molar ratio GPTMS:CS monomer). In addition, samples exhibited extremely fast swelling by spontaneous capillary imbibition in PBS solution, presenting swelling capacities from 1.75 to 3.75. The formation of a covalent crosslinked hybrid structure was suggested by FTIR and confirmed by an increase of four hundred fold or more in the compressive strength up to 96 MPa. Instead, samples synthesized without GPTMS fractured at only 0.10–0.26 MPa, revealing a week structure consisted in interpenetrated polymer networks. The aerogels presented bioactivity in simulated body fluid (SBF), as confirmed by the in vitro formation of hydroxyapatite (HAp) layer with crystal size of approximately 2 µm size in diameter. In vitro studies revealed also non cytotoxic effect on HOB^® osteoblasts and also a mechanosensitive response. Additionally, control cells grown on glass developed scarce or no stress fibers, while cells grown on hybrid samples showed a significant (p < 0.05) increase in well-developed stress fibers and mature focal adhesion complexes.

This work introduces a new synthesis procedure for obtaining homogeneous silica hybrid aerogels with carbon nanotube contents up to 2.50 wt.%. The inclusion of nanotubes in the highly porous silica matrix was performed by a two-step sol–gel process, resulting in samples with densities below 80 mg/cm³. The structural analyses (N₂ physisorption and SEM) revealed the hierarchical structure of the porous matrix formed by nanoparticles arranged in clusters of 100 and 300 nm in size, specific surface areas around 600 m²/g and porous volumes above 4.0 cm³/g. In addition, a relevant increase on the mechanical performance was found, and an increment of 50% for the compressive strength and 90% for the maximum deformation were measured by uniaxial compression. This reinforcement was possible thanks to the outstanding dispersion of the CNT within the silica matrix and the formation of Si–O–C bridges between nanotubes and silica matrix, as suggested by FTIR. Therefore, the original synthesis procedure introduced in this work allows the fabrication of highly porous hybrid materials loaded with carbon nanotubes homogeneously distributed in the space, which remain available for a variety of technological applications.

Silica (SiO₂)/chitosan (CS) composite aerogels are bioactive when they are submerged in simulated body fluid (SBF), causing the formation of bone-like hydroxyapatite (HAp) layer. Silica-based hybrid aerogels improve the elastic behavior, and the combined CS modifies the network entanglement as a crosslinking biopolymer. Tetraethoxysilane (TEOS)/CS is used as network precursors by employing a sol-gel method assisted with high power ultrasound (600 W). Upon gelation and aging, gels are dried in supercritical CO₂ to obtain monoliths. Thermograms provide information about the condensation of the remaining hydroxyl groups (400–700 °C). This step permits the evaluation of the hydroxyl group’s content of 2 to 5 OH nm⁻². The formed Si-OH groups act as the inductor of apatite crystal nucleation in SBF. The N₂ physisorption isotherms show a hysteresis loop of type H3, characteristic to good interconnected porosity, which facilitates both the bioactivity and the adhesion of osteoblasts cells. After two weeks of immersion in SBF, a layer of HAp microcrystals develops on the surface with a stoichiometric Ca/P molar ratio of 1.67 with spherulite morphology and uniform sizes of 6 μm. This fact asserts the bioactive behavior of these hybrid aerogels. Osteoblasts are cultured on the selected samples and immunolabeled for cytoskeletal and focal adhesion expression related to scaffold nanostructure and composition. The initial osteoconductive response observes points to a great potential of tissue engineering for the designed composite aerogels.