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

Bharti Kumari 1 , Daniel John 2 , Paul Hoffmann 3 , 4 , Anne Spende 3 , 4 , Maria Eugenia Toimil-Molares 4 , Christina Trautmann 3 , 4 , Christian Hess 1 , Philip Ruff 1 , Marcus Schulze 5 , Robert Stark 5 , Gerd Buntkowsky 1 , Annette Andrieu-Brunsen 2  and Torsten Gutmann 1
  • 1 Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
  • 2 Ernst-Berl Institute for Chemical Engineering and Macromolecular Science, Technische Universität Darmstadt, Alarich-Weiss-Str. 4, D-64287 Darmstadt, Germany
  • 3 GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstr. 1, D-64291 Darmstadt, Germany
  • 4 Materialwissenschaft, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt, Germany
  • 5 Physics of Surfaces, Institute of Materials Science and Center of Smart Interfaces, Technische Universität Darmstadt, Alarich-Weiss-Str. 16, D-64287 Darmstadt, Germany
Bharti Kumari
  • Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
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, Daniel John
  • Ernst-Berl Institute for Chemical Engineering and Macromolecular Science, Technische Universität Darmstadt, Alarich-Weiss-Str. 4, D-64287 Darmstadt, Germany
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, Paul Hoffmann
  • GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstr. 1, D-64291 Darmstadt, Germany
  • Materialwissenschaft, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt, Germany
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, Anne Spende
  • GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstr. 1, D-64291 Darmstadt, Germany
  • Materialwissenschaft, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt, Germany
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, Maria Eugenia Toimil-Molares
  • Materialwissenschaft, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt, Germany
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, Christina Trautmann
  • GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstr. 1, D-64291 Darmstadt, Germany
  • Materialwissenschaft, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt, Germany
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, Christian Hess
  • Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
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, Philip Ruff
  • Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
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, Marcus Schulze
  • Physics of Surfaces, Institute of Materials Science and Center of Smart Interfaces, Technische Universität Darmstadt, Alarich-Weiss-Str. 16, D-64287 Darmstadt, Germany
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, Robert Stark
  • Physics of Surfaces, Institute of Materials Science and Center of Smart Interfaces, Technische Universität Darmstadt, Alarich-Weiss-Str. 16, D-64287 Darmstadt, Germany
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, Gerd Buntkowsky
  • Corresponding author
  • Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
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, Annette Andrieu-Brunsen
  • Ernst-Berl Institute for Chemical Engineering and Macromolecular Science, Technische Universität Darmstadt, Alarich-Weiss-Str. 4, D-64287 Darmstadt, Germany
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and Torsten Gutmann
  • Corresponding author
  • Eduard-Zintl Institute for Inorganic and Physical Chemistry, Technische Universität Darmstadt, Alarich-Weiss-Str. 8, D-64287 Darmstadt, Germany
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Abstract

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.

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