Formation of Stable Radicals by Mechanochemistry and Their Application for Magic Angle Spinning Dynamic Nuclear Polarization Solid-State NMR Spectroscopy

Carnahan, Scott L.; Riemersma, Kipper; Hlova, Ihor Z.; Dolotko, Oleksandr; Kmiec, Steven J.; Lamahewage, Sujeewa N. S.; Martin, Steve W.; Wishart, James F.; Dubroca, Thierry; Balema, Viktor P.; Rossini, Aaron J.

doi:10.1021/acs.jpca.4c00228

Title: Formation of Stable Radicals by Mechanochemistry and Their Application for Magic Angle Spinning Dynamic Nuclear Polarization Solid-State NMR Spectroscopy

Journal Article · 24 April 2024 · Journal of Physical Chemistry. A, Molecules, Spectroscopy, Kinetics, Environment, and General Theory

DOI: https://doi.org/10.1021/acs.jpca.4c00228 · OSTI ID:2340731

^[1]; Riemersma, Kipper ^[2];

^[3]; Dolotko, Oleksandr ^[3]; Kmiec, Steven J. ^[2]; Lamahewage, Sujeewa N. S. ^[4];

^[2];

^[5]; Dubroca, Thierry ^[6]; Balema, Viktor P. ^[7];

^[4]

Ames Lab., and Iowa State Univ., Ames, IA (United States); St. Mary's University of Minnesota, Winona, MN (United States)
Iowa State Univ., Ames, IA (United States)
Ames Laboratory (AMES), Ames, IA (United States)
Ames Lab., and Iowa State Univ., Ames, IA (United States)
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab)
Ames Laboratory (AMES), Ames, IA (United States); Clemson Univ., SC (United States)

High-field magic angle spinning (MAS) dynamic nuclear polarization (DNP) solid-state nuclear magnetic resonance (SSNMR) is becoming a common technique for improving the sensitivity in NMR by the hyperpolarization of nuclear spins. Recently, we have shown that gamma irradiation is capable of creating long-lived free radicals that are amenable to MAS DNP in quartz and a variety of organic solids. Here, we demonstrate that mechanochemical ball milling is able to generate millimolar concentrations of stable radical species in diverse materials, such as polystyrene, cellulose, borosilicate glass, and fused quartz. High-field electron paramagnetic resonance (EPR) was used to obtain further insight into the nature of the radicals formed in ball milled quartz and borosilicate glass. Finally, we further show that radicals generated in quartz by ball milling can be used for solid-effect DNP. We obtained ²⁹Si DNP enhancements of approximately 114 and 33 at 110 K and room temperature, respectively, from a sample of ball milled quartz.

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

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division (MSE); USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB); USDOE Office of Energy Efficiency and Renewable Energy (EERE), Office of Sustainable Transportation. Vehicle Technologies Office (VTO); National Science Foundation (NSF)

Grant/Contract Number:: SC0012704; AC02-07CH11358; EE0008852

OSTI ID:: 2340731

Alternate ID(s):: OSTI ID: 2341293

Report Number(s):: BNL--225519-2024-JAAM

Journal Information:: Journal of Physical Chemistry. A, Molecules, Spectroscopy, Kinetics, Environment, and General Theory, Journal Name: Journal of Physical Chemistry. A, Molecules, Spectroscopy, Kinetics, Environment, and General Theory Journal Issue: 18 Vol. 128; ISSN 1089-5639

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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36 MATERIALS SCIENCE
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Title: Formation of Stable Radicals by Mechanochemistry and Their Application for Magic Angle Spinning Dynamic Nuclear Polarization Solid-State NMR Spectroscopy

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