Probing surface hydrogen bonding and dynamics by natural abundance, multidimensional, 17O DNP-NMR spectroscopy

Perras, Frederic A.; Chaudhary, Umesh; Slowing, Igor I.; Pruski, Marek

doi:10.1021/acs.jpcc.6b02579

Title: Probing surface hydrogen bonding and dynamics by natural abundance, multidimensional, ¹⁷O DNP-NMR spectroscopy

Journal Article · Fri May 06 00:00:00 EDT 2016 · Journal of Physical Chemistry. C

DOI:https://doi.org/10.1021/acs.jpcc.6b02579· OSTI ID:1253766

Perras, Frederic A. ^[1]; Chaudhary, Umesh ^[2]; Slowing, Igor I. ^[2]; Pruski, Marek ^[2]

Ames Lab., Ames, IA (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States)

Dynamic nuclear polarization (DNP)-enhanced solid-state nuclear magnetic resonance (SSNMR) spectroscopy is increasingly being used as a tool for the atomic-level characterization of surface sites. DNP surface-enhanced SSNMR spectroscopy of materials has, however, been limited to studying relatively receptive nuclei, and the particularly rare ¹⁷O nuclide, which is of great interest for materials science, has not been utilized. We demonstrate that advanced ¹⁷O SSNMR experiments can be performed on surface species at natural isotopic abundance using DNP. We use ¹⁷O DNP surface-enhanced 2D SSNMR to measure ¹⁷O{¹H} HETCOR spectra as well as dipolar oscillations on a series of thermally treated mesoporous silica nanoparticle samples having different pore diameters. These experiments allow for a nonintrusive and unambiguous characterization of hydrogen bonding and dynamics at the surface of the material; no other single experiment can give such details about the interactions at the surface. Lastly, our data show that, upon drying, strongly hydrogen-bonded surface silanols, whose motions are greatly restricted by the interaction when compared to lone silanols, are selectively dehydroxylated.

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Research Organization:: Ames Lab., Ames, IA (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1253766

Report Number(s):: IS-J-8955

Journal Information:: Journal of Physical Chemistry. C, Journal Name: Journal of Physical Chemistry. C; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 47 works

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