scholarly journals 17O solid-state NMR spectroscopy of A2B2O7 oxides: quantitative isotopic enrichment and spectral acquisition?

RSC Advances ◽  
2018 ◽  
Vol 8 (13) ◽  
pp. 7089-7101 ◽  
Author(s):  
Arantxa Fernandes ◽  
Robert F. Moran ◽  
Scott Sneddon ◽  
Daniel M. Dawson ◽  
David McKay ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Isotopic Enrichment ◽  
Ceramic Oxides ◽  
Solid State Nmr Spectroscopy

Investigation of the conditions required for quantitative isotopic enrichment and the acquisition of quantitative 17O NMR spectra of ceramic oxides.

Probing Interfaces in Complex Oxide Heterostructures via 17O Solid State NMR Spectroscopy

2020 ◽  
Author(s):  
Michael Hope ◽  
Bowen Zhang ◽  
Bonan Zhu ◽  
David M. Halat ◽  
Judith L. Driscoll ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Density Functional ◽  
Interfacial Structure ◽  
Atomic Scale ◽  
Random Structure ◽  
Isotopic Enrichment ◽  
Solid State Nmr Spectroscopy ◽  
Lift Off

The determination of the atomic-scale structure of a solid–solid interface is a major outstanding problem in the physical sciences, the structure controlling many properties including stability, ionic and electronic transport, magnetism, multiferroicity and superconductivity. NMR spectroscopy is sensitive to local structure but is not typically sufficiently sensitive or selective to observe solid–solid interfaces. In this work, CeO<sub>2</sub>–SrTiO<sub>3</sub> vertically aligned nanocomposite (VAN) thin films are studied and, by combining selective isotopic enrichment with a lift-off technique to remove the substrate, the <sup>17</sup>O NMR signal from single atomic layer interfaces can clearly be seen. The interfacial structure is solved by calculating the NMR parameters using density functional theory combined with random structure searching. By performing the isotopic enrichment at variable temperatures, the superior oxide-ion conductivity of the VAN films compared to the bulk materials is shown to arise in part from enhanced oxygen mobility at this interface; oxygen motion at the interface is further identified from <sup>17</sup>O relaxometry experiments. These results highlight the information that can be obtained on interfacial structure and dynamics with solid-state NMR spectroscopy, in this and other nanostructured systems, our methodology being generally applicable to overcome sensitivity limitations in thin-film studies.

Probing Interfaces in Complex Oxide Heterostructures via 17O Solid State NMR Spectroscopy

2020 ◽  
Author(s):  
Michael Hope ◽  
Bowen Zhang ◽  
Bonan Zhu ◽  
David M. Halat ◽  
Judith L. Driscoll ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Density Functional ◽  
Interfacial Structure ◽  
Atomic Scale ◽  
Random Structure ◽  
Isotopic Enrichment ◽  
Solid State Nmr Spectroscopy ◽  
Lift Off

The determination of the atomic-scale structure of a solid–solid interface is a major outstanding problem in the physical sciences, the structure controlling many properties including stability, ionic and electronic transport, magnetism, multiferroicity and superconductivity. NMR spectroscopy is sensitive to local structure but is not typically sufficiently sensitive or selective to observe solid–solid interfaces. In this work, CeO<sub>2</sub>–SrTiO<sub>3</sub> vertically aligned nanocomposite (VAN) thin films are studied and, by combining selective isotopic enrichment with a lift-off technique to remove the substrate, the <sup>17</sup>O NMR signal from single atomic layer interfaces can clearly be seen. The interfacial structure is solved by calculating the NMR parameters using density functional theory combined with random structure searching. By performing the isotopic enrichment at variable temperatures, the superior oxide-ion conductivity of the VAN films compared to the bulk materials is shown to arise in part from enhanced oxygen mobility at this interface; oxygen motion at the interface is further identified from <sup>17</sup>O relaxometry experiments. These results highlight the information that can be obtained on interfacial structure and dynamics with solid-state NMR spectroscopy, in this and other nanostructured systems, our methodology being generally applicable to overcome sensitivity limitations in thin-film studies.

scholarly journals The Study of Water Sorption with Hydrolysis Lignin by Solid-State NMR Spectroscopy

2019 ◽  
Vol 21 (4) ◽  
pp. 325
Author(s):  
S.L. Shestakov ◽  
Yu.A. Popova ◽  
A.Yu. Kozhevnikov ◽  
D.S. Kosyakov ◽  
S.A. Sypalov
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Water Sorption ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
13C Nmr Spectroscopy ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Hydrolysis Lignin ◽  
Solid State Nmr Spectroscopy

Hydrolysis lignin is formed as a by-product of cellulose production and has limited industrial application. The ability of hydrolysis lignin to absorb and retain some water is important aspect for the study of its properties and modification methods. The processes of water sorption by hydrolysis lignin were studied with solid-state NMR spectroscopy. The samples were humidified in desiccators containing different saturated salts solutions with different relative air humidity above them. The sorption capacity of the samples was determined by water sorbed from the air, and it was found that lignin absorbs the amount of water equal to 40% of sample weight at maximum relative humidity of the air. The cross-polarization (CP) and magic angle spinning (MAS) methods were used to register solid-state NMR spectra. Using the 1H-NMR spectra, it was found that the hydrolysis lignin is hydrated in the whole volume, and the water penetrates into the deep layers of polymer, however, the distribution of water at the likely sorption sites is uneven. It was obtained with use of 13C-NMR spectroscopy that hydrolysis lignin hydrates in both hydrophilic and hydrophobic regions of the macromolecule, and the bulk of sorbed water (~64%) concentrates around the hydroxyl and methoxyl groups of lignin and polysaccharide residues.

scholarly journals A New Methodological Approach to Correlate Protective and Microscopic Properties by Soft X-ray Microscopy and Solid State NMR Spectroscopy: The Case of Cusa’s Stone

2021 ◽  
Vol 11 (13) ◽  
pp. 5767
Author(s):  
Veronica Ciaramitaro ◽  
Alberto Spinella ◽  
Francesco Armetta ◽  
Roberto Scaffaro ◽  
Emmanuel Fortunato Gulino ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Methodological Approach ◽  
Polymer Chains ◽  
General Question ◽  
Protective Agent ◽  
Vapour Permeability ◽  
X Ray ◽  
Solid State Nmr Spectroscopy

Hydrophobic treatment is one of the most important interventions usually carried out for the conservation of stone artefacts and monuments. The study here reported aims to answer a general question about how two polymers confer different protective performance. Two fluorinated-based polymer formulates applied on samples of Cusa’s stone confer a different level of water repellence and water vapour permeability. The observed protection action is here explained on the basis of chemico-physical interactions. The distribution of the polymer in the pore network was investigated using scanning electron microscopy and X-ray microscopy. The interactions between the stone substrate and the protective agents were investigated by means of solid state NMR spectroscopy. The ss-NMR findings reveal no significant changes in the chemical neighbourhood of the observed nuclei of each protective agent when applied onto the stone surface and provide information on the changes in the organization and dynamics of the studied systems, as well as on the mobility of polymer chains. This allowed us to explain the different macroscopic behaviours provided by each protective agent to the stone substrate.

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