A simple nonaqueous sol-gel processing led to ionogels, resulting in the confinement of an ionic liquid within a silica-like network. In the case of a non-water-soluble ionic liquid, ionogels were made stable toward water immersion by the presence of hydrophobic methyl groups in the solid network. A set of ionogels with different ionic liquid content was studied by DSC and 1 H NMR spectroscopy. The nanometric level of the confinement of the ionic liquid turned out to significantly modify the phase transitions, while still allowing some molecular mobility. Moreover, ionogels were found to keep the high conducting performances of the ionic liquid.
The confinement of ionic liquids within a porous silica matrix was performed by a one-step non-hydrolytic sol-gel route, leading to hybrid materials (called "ionogels") featuring both the mechanical and transparency properties of silica gels and the high ionic conductivity and thermal stability of ionic liquids.
Bacterial cellulose produced by the gram-negative bacterium Gluconacetobacter xylinum was found to be an excellent native starting material for preparing shaped ultra-lightweight cellulose aerogels. The procedure comprises thorough washing and sterilization of the aquogel, quantitative solvent exchange and subsequent drying with supercritical carbon dioxide at 40 degrees C and 100 bar. The average density of the obtained dry cellulose aerogels is only about 8 mg x cm(-3) which is comparable to the most lightweight silica aerogels and distinctly lower than all values for cellulosic aerogels obtained from plant cellulose so far. SEM, ESEM and nitrogen adsorption experiments at 77 K reveal an open-porous network structure that consists of a comparatively high percentage of large mesopores and smaller macropores.
The development of functional materials by taking advantage of the physical properties of nanoparticles needs an optimal control over their size and crystal quality. In this context, the synthesis of crystalline oxide nanoparticles in water at room temperature is a versatile and industrially appealing process but lacks control especially for "large" nanoparticles (>30 nm), which commonly consist of agglomerates of smaller crystalline primary grains. Improvement of these syntheses is hampered by the lack of knowledge on possible intermediate, noncrystalline stages, although their critical importance has already been outlined in crystallization processes. Here, we show that during the synthesis of luminescent Eu-doped YVO4 nanoparticles a transient amorphous network forms with a two-level structuration. These two prestructuration scales constrain topologically the nucleation of the nanometer-sized crystalline primary grains and their aggregation in nanoparticles, respectively. This template effect not only clarifies why the crystal size is found independent of the nucleation rate, in contradiction with the classical nucleation models, but also supports the possibility to control the final nanostructure with the amorphous phase.
Ultra-lightweight cellulose aerogels can be obtained in three steps: (1) preparation of a cellulose solution in molten N-methylmorpholine-N-oxide monohydrate (NMMO·H2O) at 110–120°C and casting of the viscous mass into moulds; (2) extraction of the solidified castings with ethanol to initiate cellulose aggregation and to remove NMMO·H2O so that the fragile, fine-porous texture of cellulose II is largely retained; and (3) drying of the lyogel using supercritical carbon dioxide (scCO2). According to this approach, cellulosic aerogels were prepared from eight commercial cellulosic materials and pulps and analysed for selected chemical, physicochemical and mechanical parameters. The results reveal that all aerogels obtained from 3% cellulose containing NMMO·H2O melts had a largely uniform mesoporous structure with an average pore size of ∼9–12 nm, surface area of 190–310 m2 g-1, and specific density of 0.046–0.069 g cm-3, but rather low mechanical stability expressed as compressive yield strain of 2.9–5.5%. All samples showed viscoelastic behaviour, with Young's modulus ranging from ∼5 to 10 N mm-2. Doubling the cellulose content in the NMMO·H2O melt from 3% to 6% increased Young's modulus by one order of magnitude. Shrinkage of the fragile cellulose bodies during scCO2 drying was still considerable and is subject to further investigations. Influencing parameters such as scCO2 pressure, cellulose content, regenerating solvent and the number of regenerating baths were optimised.
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