Investigation of some new hydro(solvo)thermal synthesis routes to nanostructured mixed-metal oxides

Journal Article · Sun Jun 01 00:00:00 EDT 2014 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2013.10.050· OSTI ID:22334240

Burnett, David L.; Harunsani, Mohammad H. ^[1]; Kashtiban, Reza J. ^[2]; Playford, Helen Y. ^[1]; Sloan, Jeremy ^[2]; Hannon, Alex C. ^[3]

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1. Department of Chemistry, University of Warwick, Coventry CV4 7AL (United Kingdom)
2. Department of Physics, University of Warwick, Coventry CV4 7AL (United Kingdom)
3. ISIS Facility, Rutherford Appleton Laboratory, Didcot OX11 0QX (United Kingdom)

We present a study of two new solvothermal synthesis approaches to mixed-metal oxide materials and structural characterisation of the products formed. The solvothermal oxidation of metallic gallium by a diethanolamine solution of iron(II) chloride at 240 °C produces a crystalline sample of a spinel-structured material, made up of nano-scale particles typically 20 nm in dimension. XANES spectroscopy at the K-edge shows that the material contains predominantly Fe{sup 2+} in an octahedral environment, but that a small amount of Fe{sup 3+} is also present. Careful analysis using transmission electron microscopy and powder neutron diffraction shows that the sample is actually a mixture of two spinel materials: predominantly (>97%) an Fe{sup 2+} phase Ga{sub 1.8}Fe{sub 1.2}O{sub 3.9}, but with a minor impurity phase that is iron-rich. In contrast, the hydrothermal reaction of titanium bis(ammonium lactato)dihydroxide in water with increasing amounts of Sn(IV) acetate allows nanocrystalline samples of the SnO{sub 2}–TiO{sub 2} solid solution to be prepared directly, as proved by powder XRD and Raman spectroscopy. - Graphical abstract: New solvothermal synthesis approaches to spinel and rutile mixed-metal oxides are reported. - Highlights: • Solvothermal oxidation of gallium metal in organic iron(II) solution gives a novel iron gallate spinel. • Hydrothermal reaction of titanium(IV) complex and tin(IV) acetate produces the complete SnO{sub 2}–TiO{sub 2} solid solution. • Nanostructured mixed-metal oxide phases are produced directly from solution.

• OSTI ID: 22334240
• Journal Information: Journal of Solid State Chemistry, Vol. 214; Conference: 7. international conference on materials for advanced technologies, Singapore (Singapore), 30 Jun - 5 Jul 2013; Other Information: Copyright (c) 2013 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
77 NANOSCIENCE AND NANOTECHNOLOGY
ABSORPTION SPECTROSCOPY
GALLIUM
HYDROTHERMAL SYNTHESIS
IRON
IRON IONS
NANOSTRUCTURES
NEUTRON DIFFRACTION
RAMAN SPECTROSCOPY
RUTILE
SOLID SOLUTIONS
SPINELS
TIN
TIN OXIDES
TITANIUM
TITANIUM OXIDES
TRANSMISSION ELECTRON MICROSCOPY
X-RAY DIFFRACTION
X-RAY SPECTROSCOPY