Crystal Structure of LiH<sub>2</sub>PO<sub>4</sub>Studied by Single-Crystal Neutron Diffraction

Oh, In Hwan; Lee, Kwang Sei; Meven, Martin; Heger, G.; Lee, Cheol Eui

doi:10.1143/jpsj.79.074606

Cited by 15 publications

(11 citation statements)

References 23 publications

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“…Thus, with high certainty, dipolar broadening can be identified as the only factor for the observed line broadening. While additional broadening mechanisms such as orientational disorder or lattice defects cannot be ruled out completely, their extent must be small, in accordance with the findings of a neutron diffraction study [6].…”

Section: P Nmr Of Ldpsupporting

confidence: 78%

“…Recently, the mechanism of the protonic conductivity of LDP has been investigated by 1 H NMR spectroscopy of powder samples under magic-angle spinning (MAS) [4,5]. However, not much attention has been paid to the electronic surroundings of the phosphorus and lithium atoms, which despite their light mass have been found to be quite immobile in the crystal structure at room temperature [6]. Since relatively large single crystals of LDP with several mm in diameter can be grown from aqueous solution [7], a good method to analyze the local surroundings of these nuclei is NMR of single crystals.…”

Section: Introductionmentioning

confidence: 99%

“…(b) Orthorhombic structure of LDP (space group Pna2 1 , No. 33), according to Reference [6], with the chosen view down the crystallographic [111] direction. All atoms in the unit cell are located at Wyckoff position 4a, with the lithium atoms (green) and the phosphorus atoms (purple) both tetrahedrally coordinated by oxygen (red).…”

Section: Introductionmentioning

confidence: 99%

“…The resulting 7 Li QC tensor is characterized by its quadrupolar coupling constant χ = Q PAS 33 = (−71 ± 1) kHz and the two eigenvalues Q PAS 11 = (22.3 ± 0.9) kHz, and Q PAS 22 = (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.Crystals 2020, 10, 302 2 of 12 with four formula units per unit cell [6]. The PO 4 tetrahedra build a three-dimensional framework connected by two different types of hydrogen bonds.…”

mentioning

confidence: 99%

“…Crystals 2020, 10, 302 2 of 12 with four formula units per unit cell [6]. The PO 4 tetrahedra build a three-dimensional framework connected by two different types of hydrogen bonds.…”

mentioning

confidence: 99%

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Single-Crystal 31P and 7Li NMR of the Ionic Conductor LiH2PO4

Zeman

Kainz²,

Bräuniger

2020

Crystals

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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 31 P chemical shift (CS) and 7 Li quadrupole coupling (QC) tensor was determined, using a global fit over three rotation patterns. The resulting CS tensor is characterized by its three eigenvalues: δ PAS 11 = (67.0 ± 0.6) ppm, δ PAS 22 = (13.9 ± 1.5) ppm, and δ PAS 33 = (−78.7 ± 0.9) ppm. All eigenvalues have also been verified by magic-angle spinning NMR on a polycrystalline sample, using Herzfeld-Berger analysis of the rotational side band pattern. The resulting 7 Li QC tensor is characterized by its quadrupolar coupling constant χ = Q PAS 33 = (−71 ± 1) kHz and the two eigenvalues Q PAS 11 = (22.3 ± 0.9) kHz, and Q PAS 22 = (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.Crystals 2020, 10, 302 2 of 12 with four formula units per unit cell [6]. The PO 4 tetrahedra build a three-dimensional framework connected by two different types of hydrogen bonds. The LiO 4 coordination tetrahedra are linked by their vertices forming [100] isolated chains and share each edge with the PO 4 units. All atoms in the unit cell are located at Wyckoff position 4a with the general site symmetry 1 − C 1 [7]. As a result, no symmetry constraints affect the algebraic form of the NMR interaction tensors, as will be explained in the following.Abstract: Last thing to be done...

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Section: P Nmr Of Ldpsupporting

confidence: 78%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

“…Crystals 2020, 10, 302 2 of 12 with four formula units per unit cell [6]. The PO 4 tetrahedra build a three-dimensional framework connected by two different types of hydrogen bonds.…”

mentioning

confidence: 99%

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Single-Crystal 31P and 7Li NMR of the Ionic Conductor LiH2PO4

Zeman

Kainz²,

Bräuniger

2020

Crystals

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Raman spectra in LiH₂PO₄ and KLi(H₂PO₄)₂: Mode assignment

Dekhili

Kauffmann

Aroui

et al. 2018

J Raman Spectroscopy

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We report and analyze Raman spectra recorded on crystals of LiH 2 PO 4 (LDP) and KLi(H 2 PO 4 ) 2 (KLDP). We provide a new and complete assignment of Raman lines in both crystals from their behavior as function of temperature. Among internal vibrations, we discern the modes within PO 4 tetrahedra, the modes related to Li-O bonds, and those due to the O-H vibrations. In the wavenumber range between 300 and 600 cm −1 , the lines associated with O-P-O or Li-O show different temperature dependencies. The bands of PO 4 are red-shifted with increasing temperature according to thermal dilatation, whereas the positions related to Li-O are temperature independent.

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