scholarly journals Application of Solid-State and In Situ NMR to Functional Materials

Author(s):  
Lauren E. Marbella
2017 ◽  
Vol 73 (3) ◽  
pp. 137-148 ◽  
Author(s):  
Kenneth D. M. Harris ◽  
Colan E. Hughes ◽  
P. Andrew Williams ◽  
Gregory R. Edwards-Gau

Solid-state NMR spectroscopy is a well-established and versatile technique for studying the structural and dynamic properties of solids, and there is considerable potential to exploit the power and versatility of solid-state NMR for in-situ studies of chemical processes. However, a number of technical challenges are associated with adapting this technique for in-situ studies, depending on the process of interest. Recently, an in-situ solid-state NMR strategy for monitoring the evolution of crystallization processes has been developed and has proven to be a promising approach for identifying the sequence of distinct solid forms present as a function of time during crystallization from solution, and for the discovery of new polymorphs. The latest development of this technique, called `CLASSIC' NMR, allows the simultaneous measurement of both liquid-state and solid-state NMR spectra as a function of time, thus yielding complementary information on the evolution of both the liquid phase and the solid phase during crystallization from solution. This article gives an overview of the range of NMR strategies that are currently available for in-situ studies of crystallization processes, with examples of applications that highlight the potential of these strategies to deepen our understanding of crystallization phenomena.


1988 ◽  
Vol 135 ◽  
Author(s):  
Y. Chabre

AbstractPreliminary results of in-situ NMR studies on lithium intercalated electrode materials in all solid state electro-chemical cells are presented. We discuss the interest for such measurements which, as far as we know, have never been reported before. The design of the cells is briefly presented and our results are compared with previous studies on compounds chemically intercalated with the n-butyllithium technique.


2019 ◽  
Author(s):  
Przemyslaw Rzepka ◽  
Zoltán Bacsik ◽  
Andrew J. Pell ◽  
Niklas Hedin ◽  
Aleksander Jaworski

Formation of CO<sub>3</sub><sup>2-</sup> and HCO<sub>3</sub><sup>-</sup> species without participation of the framework oxygen atoms upon chemisorption of CO<sub>2</sub> in zeolite |Na<sub>12</sub>|-A is revealed. The transfer of O and H atoms is very likely to have proceeded via the involvement of residual H<sub>2</sub>O or acid groups. A combined study by solid-state <sup>13</sup>C MAS NMR, quantum chemical calculations, and <i>in situ</i> IR spectroscopy showed that the chemisorption mainly occurred by the formation of HCO<sub>3</sub><sup>-</sup>. However, at a low surface coverage of physisorbed and acidic CO<sub>2</sub>, a significant fraction of the HCO<sub>3</sub><sup>-</sup> was deprotonated and transformed into CO<sub>3</sub><sup>2-</sup>. We expect that similar chemisorption of CO<sub>2</sub> would occur for low-silica zeolites and other basic silicates of interest for the capture of CO<sub>2</sub> from gas mixtures.


2021 ◽  
Vol 411 ◽  
pp. 128534
Author(s):  
Jianli Wang ◽  
Zhao Zhang ◽  
Hangjun Ying ◽  
Gaorong Han ◽  
Wei-Qiang Han

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