High-temperature in-situ magic angle spinning NMR studies of chemical reactions on catalysts

1992 ◽  
Vol 96 (20) ◽  
pp. 8106-8111 ◽  
Author(s):  
F. Gregory Oliver ◽  
Eric J. Munson ◽  
James F. Haw
2003 ◽  
Vol 775 ◽  
Author(s):  
Andrei Nossov ◽  
Flavien Guenneau ◽  
Marie-Anne Springuel-Huet ◽  
Valérie Montouillout ◽  
Jean-Pierre Cognec ◽  
...  

Summary:A Magic Angle Spinning (MAS) NMR probe has been designed allowing the in-situ measurements of NMR spectra of working catalyst. The probe was built following the original design of M. Hunger [Hunger, 1995 #2]. It allows the magic angle spinning of powder samples up to 3.5 kHz, under gas flowing conditions, and at temperatures up to 573K.


1994 ◽  
Vol 369 ◽  
Author(s):  
B. Ouyang ◽  
X. Cao ◽  
H.W. Lin ◽  
S. Slane ◽  
S. Kostov ◽  
...  

AbstractLithium-deficient cathode materials Li1-xCoO2 where x = 0.1, 0.4 and 0.6 were prepared electrochemically from the stoichiometric parent compound (x = 0.0).The materials were observed to be air-stable, and x-ray diffraction characterization yielded good agreement with the in situ studies of Dahn and co-workers, regarding changes in lattice parameters. In addition to both static and magic angle spinning (MAS) 7Li NMR, measurements, the samples were investigated by EPR and cobalt K-edge NEXAFS. The removal of Li is accompanied by compensating electrons from the Co d-orbitals, asevidenced by both shifts in the NEXAFS peak and the observation of EPR signals due to spins localized on the Co ions. These spins, in turn, result in dramatic 7Li chemical shifts (89 ppm for x = 0.6) and line broadening. Whereas MAS analysis of Li0.9CoO2 indicates two magnetically inequivalent Li sites, the spectra becometoo broad to resolve different sites for higher values of x. Finally NMR linewidth and spinlattice relaxation measurements as a function of temperature suggest a modest increase in Li+ ion mobility for Li-deficient samples as compared to the parent compound.


2018 ◽  
pp. 1073-1091 ◽  
Author(s):  
Nicholas R. Jaegers ◽  
Mary Y. Hu ◽  
David W. Hoyt ◽  
Yong Wang ◽  
Jian Zhi Hu

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