High-pressure cryogelation of nanosilica and surface properties of cryosilicas

• Effects of pressure and concentration on characteristics of silica cryogels.
• Confined space effects on the interfacial behavior of water bound to cryosilicas.
• Effects of cryosilica structure on co-adsorption of water with organics and inorganics.

Silica cryogels (cryosilicas) in a powder state were synthesized with different concentrations of fumed silica A-300 (CA-300 = 5–20 wt%), sonicated in aqueous suspension, then frozen at −14 °C at different pressures in a high-pressure stainless steel reactor (a freezing bomb), and dried in air at room temperature. To analyze the effects of low temperature and high pressure, samples were also prepared at −14 °C or room temperature and standard pressure. The structural and adsorption properties of the powder materials were studied using nitrogen adsorption, high-resolution transmission electron microscopy, infrared spectroscopy, thermogravimetry, low-temperature 1H NMR spectroscopy and thermally stimulated depolarization current. The structural, textural, adsorption and relaxation characteristics of high-pressure cryogel hydrogels and related dried powders are strongly dependent on the silica content in aqueous suspensions frozen at 1450 or 1000 atm and then dried. The largest changes are found with CA-300 = 20 wt% which are analyzed with respect to the interfacial behavior of nonpolar, weakly polar and polar adsorbates using low temperature 1H NMR spectroscopy.

Characteristics of cryosilica powders depend strongly on precursor concentration and pressure during cryogelation.Figure optionsDownload as PowerPoint slide