51. Single-Crystal 31P and 7Li NMR of the Ionic Conductor LiH2PO4
- Author
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Viktoria Kainz, Otto E. O. Zeman, and Thomas Bräuniger
- Subjects
Materials science ,7Li-NMR ,General Chemical Engineering ,Analytical chemistry ,31P-NMR ,Ionic bonding ,chemistry.chemical_element ,02 engineering and technology ,LDP ,010402 general chemistry ,01 natural sciences ,Inorganic Chemistry ,Crystal ,lcsh:QD901-999 ,General Materials Science ,Spectroscopy ,LiH2PO4 ,quadrupole coupling tensor ,021001 nanoscience & nanotechnology ,Condensed Matter Physics ,single-crystal NMR ,0104 chemical sciences ,NMR spectra database ,chemistry ,Quadrupole ,chemical shift tensor ,Lithium ,Orthorhombic crystal system ,lcsh:Crystallography ,0210 nano-technology ,Single crystal - Abstract
The electronic surroundings of phosphorus and lithium atoms in the ionic conductor lithium dihydrogen phosphate (LDP) have been studied by single-crystal nuclear magnetic resonance (NMR) spectroscopy at room temperature. From orientation-dependent NMR spectra of a large homegrown LDP single crystal, the full 31P chemical shift (CS) and 7Li quadrupole coupling (QC) tensor was determined, using a global fit over three rotation patterns. The resulting CS tensor is characterized by its three eigenvalues: &delta, 11 P A S = ( 67.0 ±, 0.6 ) ppm, &delta, 22 P A S = ( 13.9 ±, 1.5 ) ppm, and &delta, 33 P A S = ( &minus, 78.7 ±, 0.9 ) ppm. All eigenvalues have also been verified by magic-angle spinning NMR on a polycrystalline sample, using Herzfeld&ndash, Berger analysis of the rotational side band pattern. The resulting 7Li QC tensor is characterized by its quadrupolar coupling constant &chi, = Q 33 P A S = ( &minus, 71 ±, 1 ) kHz and the two eigenvalues Q 11 P A S = ( 22.3 ±, 0.9 ) kHz, and Q 22 P A S = ( 48.4 ±, 0.8 ) kHz. The initially unknown orientation of the mounted crystal, expressed by the orientation of the rotation axis in the orthorhombic crystal frame, was included in the global data fit as well, thus obtaining it from NMR data only.
- Published
- 2020
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