Abstract
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-[Mg0.70Al0.30(OH)2](CO3)0.15·yH2O·zEtOH at 600 °C (AMO-Mg2.33Al 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-Mg2.33Al 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 Al3+sites in contrast to previous reports.
| Original language | English |
|---|---|
| Pages (from-to) | 22720-22728 |
| Number of pages | 9 |
| Journal | Inorganic Chemistry |
| Volume | 64 |
| Issue number | 46 |
| DOIs | |
| State | Published - Nov 24 2025 |
Funding
F.Z.T.Y. acknowledges that the data collected for this work was facilitated by access to the I11 and I15-1 Beamlines at the Diamond Light Source. A portion of this research used resources at the Spallation Neutron Source, a DOE office of Science User Facility operated by the Oak Ridge National Laboratory on proposal number IPTS-311306. We thank Diamond Light Source for access and support in use of the electron Physical Science Imaging Centre (Instrument E02 and proposal number MG40887) that contributed to the results presented here. T.F. acknowledges support from the Royal Society in the form of a Newtown International Fellowship (NIF\R1\231784). F.Z.T.Y. acknowledges support from St Peter’s College, Oxford. F.Z.T.Y. acknowledges that the data collected for this work was facilitated by access to the I11 and I15-1 Beamlines at the Diamond Light Source. A portion of this research used resources at the Spallation Neutron Source, a DOE office of Science User Facility operated by the Oak Ridge National Laboratory on proposal number IPTS-311306. We thank Diamond Light Source for access and support in use of the electron Physical Science Imaging Centre (Instrument E02 and proposal number MG40887) that contributed to the results presented here. T.F. acknowledges support from the Royal Society in the form of a Newtown International Fellowship (NIF\R1\231784).