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.

Analytical chemical applications of high-resolution nuclear magnetic resonance spectroscopy of solids

1982 ◽  
Vol 305 (1491) ◽  
pp. 591-607 ◽  
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Structural Data ◽  
Magic Angle Spinning ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
General Applicability ◽  
Phenolic Resins ◽  
X Ray ◽  
Angle Spinning

The basis of the combined cross-polarization-magic-angle spinning (c.p.-m.a.s.) experiment, which yields high-resolution n.m.r. spectra of solid materials, is described and the general applicability of the technique, including its quantitative reliability, discussed. Solid-state n.m.r. is in many ways complementary to X-ray diffraction, as shown by its application to amorphous systems in which diffraction methods cannot be used (for example resins, coals, glasses and surface-immobilized catalysts) and also by its application to crystalline materials where X-ray structural data are available but where, for various reasons, a fuller description of the structure may be obtained by n.m.r. Examples include zeolites and chemically exchanging solid systems. The technique also provides a bridge between the solid-state structures of conformationally mobile and charged species as determined by diffraction techniques and the structures of these species in solution. Quantitative reliability of the c.p.-m.a.s. technique has been evaluated for phenolic resins and coals.

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.

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