Endogenous Dynamic Nuclear Polarization for Natural Abundance 17O and Lithium NMR in the Bulk of Inorganic Solids

Wolf, Tamar; Kumar, Sandeep; Singh, Harishchandra; Chakrabarty, Tanmoy; Aussenac, Fabien; Frenkel, Anatoly I.; Major, Dan Thomas; Leskes, Michal

doi:10.1021/jacs.8b11015

Endogenous Dynamic Nuclear Polarization for Natural Abundance ¹⁷O and Lithium NMR in the Bulk of Inorganic Solids

Journal Article · Tue Dec 11 00:00:00 EST 2018 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.8b11015· OSTI ID:1493570

Wolf, Tamar ^[1]; Kumar, Sandeep ^[2]; Singh, Harishchandra ^[3]; Chakrabarty, Tanmoy ^[1]; Aussenac, Fabien ^[4]; ^[5]; ^[2]; ^[1]

Weizmann Institute of Science, Rehovot (Israel)
Bar-Ilan Univ., Ramat Gan (Israel)
Stony Brook Univ., Stony Brook, NY (United States)
Bruker BioSpin, Wissembourg Cedex (France)
Stony Brook Univ., Stony Brook, NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)

In recent years magic angle spinning-dynamic nuclear polarization (MAS-DNP) has developed as an excellent approach for boosting the sensitivity of solid-state NMR (ssNMR) spectroscopy, thereby enabling the characterization of challenging systems in biology and chemistry. Most commonly, MAS-DNP is based on the use of nitroxide biradicals as polarizing agents. In materials science, since the use of nitroxides often limits the signal enhancement to the materials’ surface and subsurface layers, there is need for hyperpolarization approaches which will provide sensitivity in the bulk of micron sized particles. Recently, an alternative in the form of paramagnetic metal ions has emerged. Here we demonstrate the remarkable efficacy of Mn(II) dopants, used as endogenous polarization agents for MAS-DNP, in enabling the detection of ¹⁷O at a natural abundance of only 0.038%. Distinct oxygen sites are identified in the bulk of micron-sized crystals, including battery anode materials Li₄Ti₅O₁₂ (LTO) and Li₂ZnTi₃O₈, as well as the phosphor materials NaCaPO4 and MgAl₂O₄, all doped with Mn(II) ions. Density functional theory calculations are used to assign the resonances to specific oxygen environments in these phases. Depending on the Mn(II) dopant concentration, we obtain significant signal enhancement factors, 142 and 24, for ⁶Li and ⁷Li nuclei in LTO, respectively. We furthermore follow the changes in the ^6,7Li LTO resonances and determine their enhancement factors as a function of Mn(II) concentration. Furthermore, the results presented show that MAS-DNP from paramagnetic metal ion dopants provides an efficient approach for probing informative nuclei such as ¹⁷O, despite their low gyromagnetic ratio and negligible abundance, without isotope enrichment.

View Accepted Manuscript (DOE)

Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: SC0012704

OSTI ID:: 1493570

Alternate ID(s):: OSTI ID: 1688483

Report Number(s):: BNL--211243-2019-JAAM

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 1 Vol. 141; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited By (4)

Selective NMR observation of the SEI–metal interface by dynamic nuclear polarisation from lithium metal Hope, Michael A.; Rinkel, Bernardine L. D.; Gunnarsdóttir, Anna B. Nature Communications, Vol. 11, Issue 1 https://doi.org/10.1038/s41467-020-16114-x	journal	May 2020
Blind spheres of paramagnetic dopants in solid state NMR Li, Wenyu; Zhang, Qianyun; Joos, Jonas J. Physical Chemistry Chemical Physics, Vol. 21, Issue 19 https://doi.org/10.1039/c9cp00953a	journal	January 2019
Selective NMR observation of the SEI-metal interface by dynamic nuclear polarisation from lithium metal. Hope, Michael A.; Rinkel, Bernardine; Gunnarsdóttir, Anna B. Apollo - University of Cambridge Repository https://doi.org/10.17863/cam.51487	text	January 2020
Selective NMR observation of the SEI–metal interface by dynamic nuclear polarisation from lithium metal Hope, Michael A.; Rinkel, Bernardine L. D.; Gunnarsdóttir, Anna B. Apollo - University of Cambridge Repository https://doi.org/10.17863/cam.69492	text	January 2020

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Related Subjects

17O NMR
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Density Functional Theory
Doping
Dynamic Nuclear Polarization
Magic Angle Spinning
Natural Abundance
Paramagnetic metal ions
Sensitivity Enhancement
Solid State NMR