Nowadays the sol–gel process is used by an increasing number of researchers for the preparation of various products, including bulk materials, films, membranes or fibers. The application of ultrasound (sonocatalysis) to the precursors gives rise to materials with new properties, known as sonogels. The absence of additional solvent and, mainly, the effects of ultrasonic cavitation create a unique environment for sol–gel reactions leading to particular features in the resulting gels: high density, fine texture, homogeneous structure etc. These properties determine the evolution of sonogels on further processing and the final material structure. In this sense, the full exploitation of sonocatalysis requires a thorough understanding of the processes involved and their sensitivity to reaction parameters. For this purpose, we have used diverse techniques to investigate the microstructural evolution during different steps in the sonogel process. The results of these studies are reported here. Finally, we present an overview of some applications for which the mechanical, textural and optical characteristics of sonogels are quite useful. Copyright © 1999 John Wiley & Sons, Ltd.
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.
Here we show the suitability of nanoindentation to study in detail the micromechanical response of silica colloidal crystals (CCs). The sensitivity to displacements smaller than the submicrometer spheres size, even resolving discrete events and superficial features, revealed particulate features with analogies to atomic crystals. Significant robustness, long-range structural deformation, and large energy dissipation were found. Easily implemented temperature/rate-dependent nanoindentation quantified the paramount role of adsorbed water endowing silica CCs with properties of wet granular materials like viscoplasticity. A novel “nongranular” CC was fabricated by substituting capillary bridges with silica necks to directly test water-independent mechanical response. Silica CCs, as specific (nanometric, ordered) wet granular assemblies with well-defined configuration, may be useful model systems for granular science and capillary cohesion at the nanoscale.
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