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Table · dataset · 2026

Data for Nanocrystalline transition-metal gallium oxide spinels from acetylacetonate precursors via solvothermal synthesis

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The synthesis of mixed-metal spinels based on substituted -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 (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 is in turn implies a mixture of tetrahedral and octahedral Ga3+, and the material is stable on annealing to at least 900 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+.

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In the case of iron, higher amounts of the transition metal can be included to give a 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.<br><br>Data are ascii format with names corresponding to the figures in the main paper, as follows: Figure1a powder XRD data Figure3a powder XRD data Figure5a powder XRD data Figure 7a magnetisation data Figure 7a magnetisation data Figure 8a Magnetic hysteresis data Figure 8b Magnetic hysteresis data Figure 9a EPR spectral data Figure 9b EPR spectral data Figure 10a Mossbauer spectral data Figure 10b Mossbauer spectral data Figure 10c Mossbauer spectral data Figure 10d Mossbauer spectral data

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