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Licensed Unlicensed Requires Authentication Published by Oldenbourg Wissenschaftsverlag March 6, 2018

Surface Enhanced DNP Assisted Solid-State NMR of Functionalized SiO2 Coated Polycarbonate Membranes

Bharti Kumari, Daniel John, Paul Hoffmann, Anne Spende, Maria Eugenia Toimil-Molares, Christina Trautmann, Christian Hess, Philip Ruff, Marcus Schulze, Robert Stark, Gerd Buntkowsky, Annette Andrieu-Brunsen and Torsten Gutmann


Surface enhanced solid-state NMR by dynamic nuclear polarization (DNP SENS) enables the characterization of the inner-pore surface functionalization of porous etched ion-track membranes exhibiting low specific surface areas compared to typical SBA- or MCM-type mesoporous silica materials. The membranes were conformally coated with a 5 nm thin SiO2 layer by atomic layer deposition. This layer was subsequently modified by aminopropyl silane linkers that allow further functionalization via the terminal amine group. The results evidence that in principle DNP SENS is a capable tool to analyze more complex porous systems, e.g. bioinspired functional etched ion-track membranes down to the molecular level. These results are relevant also for single nanopore systems, for which a direct analysis of the channel surface functionalization is not feasible by classical characterization methods. The applicability of DNP SENS to complex porous systems requires the optimization of the sample preparation and measurement parameters.


This work has been supported by the DFG under contract Bu 911/20-1 (DNP spectrometer) and FOR1583 Grant Nos. Bu 911-18-2, HE 4515/4-2. The authors further thank the project iNAPO by the Hessen State Ministry of Higher Education, Research and the Arts for financial support.


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Received: 2017-09-08
Accepted: 2018-02-14
Published Online: 2018-03-06
Published in Print: 2018-07-26

©2018 Walter de Gruyter GmbH, Berlin/Boston