Please use this identifier to cite or link to this item: http://hdl.handle.net/1843/47196
Type: Artigo de Periódico
Title: Nanocrystalline transition-metal gallium oxide spinels from acetylacetonate precursors via solvothermal synthesis
Authors: Daniel Sean Cook
Reza J. Kashtiban
Klaus Wilhelm Heinrich Krambrock
Geraldo Magela de Lima
Humberto Osório Stumpf
Luciano Roni Silva Lara
José Domingos Ardisson
Richard I. Walton
Abstract: The synthesis of mixed-metal spinels based on substituted γ-Ga₂O₃ is reported using metal acetylacetonate precursors in solvothermal reactions with alcohols as solvents at 240 °C. New oxides of Cr, Mn and Fe have been produced, all of which are formed as nanocrystalline powders, as seen by high-resolution transmission electron microscopy (HR-TEM). The first chromium-gallium mixed oxide is thus formed, with composition 0.33Ga1.87Cr0.8O₄ ( = vacant site). X-ray absorption near-edge spectroscopy (XANES) at the chromium K-edge shows the presence of solely octahedral Cr3+, which in turn implies a mixture of tetrahedral and octahedral Ga3+, and the material is stable on annealing to at least 850 °C. An analogous manganese material with average chemical composition close to MnGa₂O₄ is shown to contain octahedral Mn2+, along with some Mn3+, but a different inversion factor to materials reported by conventional solid-state synthesis in the literature, which are known to have a significant proportion of tetrahedral Mn2+. In the case of iron, higher amounts of the transition metal can be included to give an Fe:Ga ratio of 1:1. Elemental mapping using energy dispersive X-ray spectroscopy on the TEM, however, reveals inhomogeneity in the distribution of the two metals. This is consistent with variable temperature 57Fe Mössbauer spectroscopy that shows the presence of Fe2+ and Fe3+ in more than one phase in the sample. Variable temperature magnetisation and electron paramagnetic resonance (EPR) indicate the presence of superparamagnetism at room temperature in the iron-gallium oxides.
Subject: Ferrita
Cristalização
Magnetismo
language: eng
metadata.dc.publisher.country: Brasil
Publisher: Universidade Federal de Minas Gerais
Publisher Initials: UFMG
metadata.dc.publisher.department: ICX - DEPARTAMENTO DE FÍSICA
ICX - DEPARTAMENTO DE QUÍMICA
Rights: Acesso Aberto
metadata.dc.identifier.doi: https://doi.org/10.3390/ma12050838
URI: http://hdl.handle.net/1843/47196
Issue Date: 12-Mar-2019
metadata.dc.url.externa: https://www.mdpi.com/1996-1944/12/5/838
metadata.dc.relation.ispartof: Materials
Appears in Collections:Artigo de Periódico

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