Aqueous metal oxide sols

The direct intercalation of metal oxide sols (DIMOS) according to Pinnavaia is a good technique to achieve stable oxide pillars [31]. Aqueous oxide sols with uniform particle sizes of 20-80 A can be used to create mesoporous pillared clays. The materials are also called supergallery PILCs, a term covering all substrates with an interlayer distance substantially larger than the thickness of the host layers. Ti-sol prepared from Ti-alkoxides results in Ti-PILCs with interlayer free spacings of 13 A and surface areas of 300 m /g. 

The 3M Company manufactures a continuous polycrystalline alurnina—sihca—boria fiber (Nextel) by a sol process (17). Aluminum acetate is dissolved in water and mixed with an aqueous dispersion of colloidal sihca and dimethylform amide. This mixture is concentrated in a Rotavapor flask and centrifuged. The viscous mixture is then extmded through spinnerettes at 100 kPa (1 atm) the filaments are collected on a conveyor and heat-treated at 870°C to convert them to metallic oxides. Further heating at 1000°C produces the 10-p.m diameter aluminum borosihcate fibers, which are suitable for fabrication into textiles for use at temperatures up to 1427°C. 

With Acyl Halides, Hydrogen Halides, and Metallic Halides. Ethylene oxide reacts with acetyl chloride at slightly elevated temperatures in the presence of hydrogen chloride to give the acetate of ethylene chlorohydrin (70). Hydrogen haUdes react to form the corresponding halohydrins (71). Aqueous solutions of ethylene oxide and a metallic haUde can result in the precipitation of the metal hydroxide (72,73). The haUdes of aluminum, chromium, iron, thorium, and zinc in dilute solution react with ethylene oxide to form sols or gels of the metal oxide hydrates and ethylene halohydrin (74). 

Baek, S., et ah, A one-pot microwave-assisted non-aqueous sol-gel approach to metal oxide/graphene nanocomposites for Li-ion batteries. RSC Advances, 2011.1(9) p.1687-1690. 

In contrast to aqueous methods, the polyol approach resulted in the synthesis of metallic nanoparticles protected by surface-adsorbed glycol, thus minimizing the oxidation problem The use of polyol solvent also reduces the hydrolysis problem of ultrafine metal particles, which often occurs in aqueous systems. Oxide nanoparticles can be prepared, however, with the addition of water, which makes the polyol method act more like a sol—gel reaction (forced hydrolysis). For example, 5.5-nm CoFe204 has been prepared by the reaction of ferric chloride and cobalt acetate in 1,2- propanediol with the addition of water and sodium acetate. 

The sol-gel technique uses mild conditions to prepare a cross-linked, robust metal oxide gel. Gelation of silanes, such as tetraethoxysilane (TEOS) or sodium silicate, involves the use of aqueous solutions, sometimes containing alcohol, with a slight adjustment of pH to catalyse the condensation polymerisation. The cross-link density, material porosity and homogeneity of functionalised sites, are dependent on the solution pH, extent of ageing, method of solvent evaporation, water content in solution and type of catalyst, all of which provide a number of handles to modify the material of interest. 

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