A new application for an old concept: Constant time (CT)-REDOR for an accurate determination of second moments in multiple spin systems with strong heteronuclear dipolar couplings

Echelmeyer, Thomas; Wüllen, Leo van; Wegner, Sebastian

doi:10.1016/j.ssnmr.2008.02.006

Cited by 16 publications

(16 citation statements)

References 13 publications

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“…Subsequently, results on novel hybrid electrolytes, in which a mixture of an ionic liquid and Li salt is confined within the pore system of a SiO 2 glass will be presented [96]. The section will conclude with a report on the analysis of the mechanism of Li transport in the crystalline electrolyte Li 5 La 3 Nb 2 O 12 [97,98]. Details of the syntheses and experimental procedures will not be given here, the reader is referred to the literature.…”

Section: Resultsmentioning

confidence: 99%

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Wüllen¹,

Echelmeyer

Voigt

et al. 2010

Zeitschrift Für Physikalische Chemie

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Ionic TransportResearch on solid ionic conductors for use as electrolytes in all solid state batteries still constitutes a rather vivid branch of today's materials science. Despite enormous efforts, neither the development of a solid electrolyte fulfilling the key requirements such as mechanical stability and high ionic conductivity at ambient temperature has been successful nor has an extended understanding of the local Li coordination motifs in the often amorphous systems been obtained. In this contribution, recent progress both in the development of novel solid state electrolytes with high ionic conductivity and mechanical stability and in the characterization of the local Li coordination motifs in these electrolytes from our laboratory is presented. The work was performed as a project within the framework of the Collaborative Research Centre SFB 458 "Ionic Motion in Materials with Disordered Structures -From Elementary Steps to Macroscopic Transport". Results will be given for polymer electrolytes based on polyethylene oxide (PEO), polyphosphazene (PPZ) and polyacrylonitrile (PAN) with various Li salts, nano-composites of these polymer electrolytes and Al 2 O 3 as a ceramic filler, novel inorganic/organic hybrid electrolytes, in which a mixture of an ionic liquid and Li salt is confined within the pore system of a SiO 2 glass, and a crystalline electrolyte, Li 5 La 3 Nb 2 O 12 . Employing a range of advanced solid state NMR methodologies including dipolar based NMR techniques and pulsed field gradient (PFG) NMR and impedance spectroscopy we were able to obtain a detailed knowledge about the local Li cation coordination motifs and the mechanism of Li transport in these electrolytes. Especially the hybrid electrolytes and the salt rich PAN based polymer electrolytes were identified as rather promising materials which combine a high ionic conductivity and mechanical stability.

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Section: Resultsmentioning

confidence: 99%

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Wüllen¹,

Echelmeyer

Voigt

et al. 2010

Zeitschrift Für Physikalische Chemie

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“…In the case of extremely large dipolar coupling constants (as to be expected for direct B‐F‐bonding), however, the REDOR curve very quickly reaches the plateau, leaving only but a few data points for analysis. For cases like these constant time REDOR was developed . Here, the dipolar evolution time is kept fixed at some low value (2 or 4 rotor cycles), then varying the pulse length of the dephasing pulses.…”

Section: Methodsmentioning

confidence: 99%

Sn[B₂O₃F₂]—The First Tin Fluorooxoborate as Possible NLO Material

Jantz

Dialer

Bayarjargal

et al. 2018

Advanced Optical Materials

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electrical control of the respective materials' SHG properties. Highly interesting as efficient large bandgap SHG materials are borates like KBBF, i.e., KBe 2 BO 3 F 2 , providing a layered structure. [10] According to these the coplanar configuration of the non-centrosymmetric building units promotes birefringence and SHG. Moreover, the weak ionic interactions mediated via K + -F − contacts between adjacent [Be 2 BO 3 F 2 ] layers strengthen its layer habit further. Recently, with Cs 3 Zn 6 B 9 O 21 (CZB) [11] within the same family of compounds another highly promising borate was presented, both of special interest because of their large bandgap allowing SHG also in the UV regime. A close relative to KBBF is Sr 2 Be 2 B 2 O 7 (SBBO), [12] comprising [Be 2 (BO 3 ) 2 O] layers. Both materials contain beryllium which is not favored in applications due to the high toxicity of Be 2+ ions.Fluorooxoborates should comprise sufficiently large bandgaps in the UV as well as preferential formation of non-centrosymmetric structures, thus making them ideal candidates for SHG materials in the UV. Beyond that, they normally combine the birefringence promoting triangular BO 3 or tetrahedral BO 3 F moieties providing terminal fluorine atoms with a proclivity for weak coordination. [13][14][15][16][17][18][19][20][21][22][23][24][25][26] Recent calculations [27] as well our own results [28] confirm these considerations and suggest a boost for NLO materials based on so-called fluorooxoborates.Apparently, nature normally strives for high symmetry, and therefore-from a solid state chemists point of viewnon-centrosymmetric structures are facilitated by the presence of suited basic building blocks like the mentioned triangular or tetrahedral ones. But frequently, also these are arranged centrosymmetrically in a crystal structure. Our approach therefore uses as second driving force the choice of such basic building Herein, the crystal structure as well as second-harmonic-generation (SHG), thermal and spectroscopic properties of Sn[B 2 O 3 F 2 ] (TFB = tin-fluorooxoborate) are presented. TFB adopts a novel non-centrosymmetric crystal structure, which is determined by single-crystal X-ray diffraction (XRD) (P31m, Z = 1, a = 4.5072(2) Å, c = 4.7624(3) Å) and comprises [B 2 O 3 F 2 ] 2− layers consisting solely of BO 3 F tetrahedra; the covalent BF bonds are unequivocally localized via solid-state NMR spectroscopy as well as density functional theory (DFT) calculations. TFB is insensitive to air and moisture, shows a stronger SHG intensity than K[H 2 PO 4 ] (KDP) and a bandgap of ≈5 eV. The thermal decomposition yields two new borate fluorides.

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“…38 Again, these studies were conducted with a compensation scheme. Figure 14 shows compensated CT-REDOR curves for 3 with three different evolution times probing characteristic parts of the REDOR curve.…”

Section: Journal Of the American Chemical Societymentioning

confidence: 99%

New Insights into Frustrated Lewis Pairs: Structural Investigations of Intramolecular Phosphane–Borane Adducts by Using Modern Solid-State NMR Techniques and DFT Calculations

et al. 2012

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Covalent bonding interactions between the Lewis acid and Lewis base functionalities have been probed in a series of "frustrated Lewis pairs" (FLPs) (mainly substituted vinylene linked intramolecular phosphane−borane adducts), using solid-state nuclear magnetic resonance techniques and accompanying DFT calculations. Both the 11 B NMR isotropic chemical shifts and nuclear electric quadrupolar coupling parameters turn out to be extremely sensitive experimental probes for such interactions, revealing linear correlations with boron−phosphorus internuclear distances. The principal component V zz of the 11

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A new application for an old concept: Constant time (CT)-REDOR for an accurate determination of second moments in multiple spin systems with strong heteronuclear dipolar couplings

Cited by 16 publications

References 13 publications

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Sn[B₂O₃F₂]—The First Tin Fluorooxoborate as Possible NLO Material

New Insights into Frustrated Lewis Pairs: Structural Investigations of Intramolecular Phosphane–Borane Adducts by Using Modern Solid-State NMR Techniques and DFT Calculations

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A new application for an old concept: Constant time (CT)-REDOR for an accurate determination of second moments in multiple spin systems with strong heteronuclear dipolar couplings

Cited by 16 publications

References 13 publications

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Sn[B2O3F2]—The First Tin Fluorooxoborate as Possible NLO Material

New Insights into Frustrated Lewis Pairs: Structural Investigations of Intramolecular Phosphane–Borane Adducts by Using Modern Solid-State NMR Techniques and DFT Calculations

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Sn[B₂O₃F₂]—The First Tin Fluorooxoborate as Possible NLO Material