A Combined Neutron and Synchrotron X-ray Scattering Study of a MgAl-Layered Double Oxide Article Swipe
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· 2025
· Open Access
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· DOI: https://doi.org/10.1021/acs.inorgchem.5c03754
· OA: W4416602145
Owing to their vast chemical and structural flexibility, layered double hydroxides (LDHs) are among some of the most promising materials for many catalytic applications. Thermal decomposition below 700 °C leads to the formation of a complex semiamorphous mixed metal oxide (LDO). In this study, the product of calcination of aqueous miscible organic solvent-treated AMO-[Mg<sub>0.70</sub>Al<sub>0.30</sub>(OH)<sub>2</sub>](CO<sub>3</sub>)<sub>0.15</sub>·<i>y</i>H<sub>2</sub>O·<i>z</i>EtOH at 600 °C (AMO-Mg<sub>2.33</sub>Al LDO) has been investigated using a synergistic combination of high-resolution synchrotron X-ray and neutron scattering techniques, as well as high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), solid-state NMR (ssNMR), and thermogravimetric analysis coupled with mass spectrometry (TGA-MS). The local and extended structure of AMO-Mg<sub>2.33</sub>Al LDO has been modeled by reciprocal and real space X-ray and neutron scattering analyses and is consistent with a modified rock salt structure consisting of octahedrally coordinated layers containing a small number of vacancies and the tetrahedrally coordinated Al<sup>3+</sup> sites in contrast to previous reports.
