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

Title: 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.

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

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

Grant/Contract Number:: SC0012704

OSTI ID:: 1493570

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

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

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 55 works

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

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

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