Solvent-free synthesis of binary inorganic oxides

Hay, J. N.; Raval, Hema M.

doi:10.1039/a707549i

Cited by 44 publications

(37 citation statements)

References 17 publications

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“…They and others reported the synthesis of several metal oxide gels, including silica, alumina, titania, binary phases thereof, tin oxide, and various titanates. [53][54][55][56][57][58][59][60][61] At about the same time, Inoue et al and others worked on the preparation of oxidic powders using the reaction between metal alkoxides and alcohols [62][63][64] or inert organic solvents. [64][65][66] In particular, the glycothermal method involving the reaction of metal alkoxides or acetylacetonates in 1,4butanediol is a versatile approach to various metal oxides [67,68] and has recently been reviewed.…”

Section: Nonaqueous Sol-gel Chemistry For Metal Oxide Synthesismentioning

confidence: 99%

Organic Reaction Pathways in the Nonaqueous Synthesis of Metal Oxide Nanoparticles

Niederberger

Garnweitner

2006

Chemistry A European J

462

457

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Nonaqueous-solution routes to metal oxide nanoparticles are a valuable alternative to the known aqueous sol-gel processes, offering advantages such as high crystallinity at low temperatures, robust synthesis parameters and ability to control the crystal growth without the use of surfactants. In the first part of the review we give a detailed overview of the various solution routes to metal oxides in organic solvents, with a strong focus on surfactant-free processes. In most of these synthesis approaches, the organic solvent plays the role of the reactant that provides the oxygen for the metal oxide, controls the crystal growth, influences particle shape, and, in some cases, also determines the assembly behavior. We have a closer look at the following reaction systems in this order: 1) metal halides in alcohols, 2) metal alkoxides, acetates, and acetylacetonates in alcohols, 3) metal alkoxides in ketones, and 4) metal acetylacetonates in benzylamine. All these systems offer some peculiarities with respect to each other, providing many possibilities to control and tailor the particle size and shape, as well as the surface and assembly properties. In the second part we present general mechanistic principles for aqueous and nonaqueous sol-gel processes, followed by the discussion of reaction pathways relevant for nanoparticle formation in organic solvents. Depending on the system several mechanisms have been postulated: 1) alkyl halide elimination, 2) elimination of organic ethers, 3) ester elimination, 4) C--C bond formation between benzylic alcohols and alkoxides, 5) ketimine and aldol-like condensation reactions, 6) oxidation of metal nanoparticles, and 7) thermal decomposition methods.

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Section: Nonaqueous Sol-gel Chemistry For Metal Oxide Synthesismentioning

confidence: 99%

Organic Reaction Pathways in the Nonaqueous Synthesis of Metal Oxide Nanoparticles

Niederberger

Garnweitner

2006

Chemistry A European J

462

457

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“…Depending on the drying conditions the binary oxides could be obtained as aerogels, either by supercritical drying Pajonk et al [14], Dusi et al [15],or by silanization of the material previously to a conventional drying Sotelo et al [16].Additionally, non-hydrolytic sol-gel routes have been also reported in the literatureHay et al [17].…”

Section: Introductionmentioning

confidence: 97%

Synthesis of Titanium Dioxide Nanoparticles by Sol-Gel Technique

Devi¹,

Venckatesh²,

Sivaraj³

2014

IJIRSET

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Nanosized Titanium dioxide (TiO 2 ) powder was synthesized via sol-gel method using titanium tetraisopropoxide (TTIP) as the precursor. The as prepared nano powder was used for further characterization. The phase transformation was investigated by an X-ray diffractometer (XRD). The anatase structure of titanium dioxide was obtained after calcination. The microstructure was characterized by a Scanning Electron Microscope (SEM).

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“…The term NHSG reaction has not only been applied to systems that result in monolithic gels, but based on a common reaction mechanism also to precursors that yield precipitates. This method was later adapted to other complex oxide systems [73,74,75,76], as well as the preparation of hybrid organic-inorganic gels [77,78,79,80]. Our group has been exploring NHSG routes to negative thermal expansion (NTE) materials in the A 2 M 3 O 12 family (A = trivalent metal; M = Mo, W) [81,82,83].…”

Section: Non-hydrolytic Sol-gel Synthesis Of Metal Oxidesmentioning

confidence: 99%

Novel Materials through Non-Hydrolytic Sol-Gel Processing: Negative Thermal Expansion Oxides and Beyond

Lind

Gates

Pedoussaut³

et al. 2010

Materials

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Low temperature methods have been applied to the synthesis of many advanced materials. Non-hydrolytic sol-gel (NHSG) processes offer an elegant route to stable and metastable phases at low temperatures. Excellent atomic level homogeneity gives access to polymorphs that are difficult or impossible to obtain by other methods. The NHSG approach is most commonly applied to the preparation of metal oxides, but can be easily extended to metal sulfides. Exploration of experimental variables allows control over product stoichiometry and crystal structure. This paper reviews the application of NHSG chemistry to the synthesis of negative thermal expansion oxides and selected metal sulfides.

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Solvent-free synthesis of binary inorganic oxides

Cited by 44 publications

References 17 publications

Organic Reaction Pathways in the Nonaqueous Synthesis of Metal Oxide Nanoparticles

Organic Reaction Pathways in the Nonaqueous Synthesis of Metal Oxide Nanoparticles

Synthesis of Titanium Dioxide Nanoparticles by Sol-Gel Technique

Novel Materials through Non-Hydrolytic Sol-Gel Processing: Negative Thermal Expansion Oxides and Beyond

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