Polarization-Transfer Methods in Solid-State Magic-Angle-Spinning NMR: Adiabatic CN Pulse Sequences

ChemPhysChem ◽  
2004 ◽  
Vol 5 (6) ◽  
pp. 851-862 ◽  
Author(s):  
René Verel ◽  
Beat H. Meier
Keyword(s):  
Solid State ◽  
Pulse Sequences ◽  
Magic Angle Spinning ◽  
Polarization Transfer ◽  
Magic Angle ◽  
Angle Spinning

Highly efficient19F heteronuclear decoupling in solid-state NMR spectroscopy using supercycled refocused-CW irradiation

2016 ◽  
Vol 18 (45) ◽  
pp. 30990-30997 ◽  
Author(s):  
Asif Equbal ◽  
Kristoffer Basse ◽  
Niels Chr. Nielsen
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Pulse Sequences ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Solid State Nmr Spectroscopy ◽  
Angle Spinning

We present heteronuclear19F refocused CW (rCW) decoupling pulse sequences for solid-state magic-angle-spinning NMR applications.

Characterization of Nanostructured Organic-Inorganic Hybrid Materials Using Advanced Solid-State NMR Spectroscopy

2009 ◽  
Vol 1184 ◽  
Author(s):  
Kanmi Mao ◽  
Jennifer L. Rapp ◽  
Jerzy W. Wiench ◽  
Marek Pruski
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Pulse Sequences ◽  
Magic Angle Spinning ◽  
Indirect Detection ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
Inorganic Hybrid ◽  
Angle Spinning ◽  
Fast Magic Angle Spinning

AbstractWe demonstrate the applications of several novel techniques in solid-state nuclear magnetic resonance spectroscopy (SSNMR) to the structural studies of mesoporous organic-inorganic hybrid catalytic materials. Most of these latest capabilities of solid-state NMR were made possible by combining fast magic angle spinning (at ≥ 40 kHz) with new multiple RF pulse sequences. Remarkable gains in sensitivity have been achieved in heteronuclear correlation (HETCOR) spectroscopy through the detection of high-λ (1H) rather than low-λ (e.g., 13C, 15N) nuclei. This so-called indirect detection technique can yield through-space 2D 13C-1H HETCOR spectra of surface species under natural abundance within minutes, a result that earlier has been out of reach. The 15N-1H correlation spectra of species bound to a surface can now be acquired, also without isotope enrichment. The first indirectly detected through-bond 2D 13C-1H spectra of solid samples are shown, as well. In the case of 1D and 2D 29Si NMR, the possibility of generating multiple Carr-Purcell-Meiboom-Gill (CPMG) echoes during data acquisition offered time savings by a factor of ten to one hundred. Examples of the studied materials involve mesoporous silica and mixed oxide nanoparticles functionalized with various types of organic groups, where solid-state NMR provides the definitive characterization.

scholarly journals Preparation of Li3PS4–Li3PO4 Solid Electrolytes by Liquid-Phase Shaking for All-Solid-State Batteries

2021 ◽  
Vol 2 (1) ◽  
pp. 39-48
Author(s):  
Nguyen H. H. Phuc ◽  
Takaki Maeda ◽  
Tokoharu Yamamoto ◽  
Hiroyuki Muto ◽  
Atsunori Matsuda
Keyword(s):  
Solid Solution ◽  
Solid State ◽  
Liquid Phase ◽  
Room Temperature ◽  
Reaction Medium ◽  
Magic Angle Spinning ◽  
Resonance Spectroscopy ◽  
Synthesis Methods ◽  
Magic Angle ◽  
Angle Spinning

A solid solution of a 100Li3PS4·xLi3PO4 solid electrolyte was easily prepared by liquid-phase synthesis. Instead of the conventional solid-state synthesis methods, ethyl propionate was used as the reaction medium. The initial stage of the reaction among Li2S, P2S5 and Li3PO4 was proved by ultraviolet-visible spectroscopy. The powder X-ray diffraction (XRD) results showed that the solid solution was formed up to x = 6. At x = 20, XRD peaks of Li3PO4 were detected in the prepared sample after heat treatment at 170 °C. However, the samples obtained at room temperature showed no evidence of Li3PO4 remaining for x = 20. Solid phosphorus-31 magic angle spinning nuclear magnetic resonance spectroscopy results proved the formation of a POS33− unit in the sample with x = 6. Improvements of ionic conductivity at room temperature and activation energy were obtained with the formation of the solid solution. The sample with x = 6 exhibited a better stability against Li metal than that with x = 0. The all-solid-state half-cell employing the sample with x = 6 at the positive electrode exhibited a better charge–discharge capacity than that employing the sample with x = 0.

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