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Plasma Polymerization of Allylamine onto Pan-Based Carbon Fibers

Published online by Cambridge University Press:  15 February 2011

R. J. Smiley  and
W. N. Delgass
R. J. Smiley
Affiliation:
Purdue University, Department of Chemical Engineering, West Lafayette, Indiana 47907.
W. N. Delgass
Affiliation:
Purdue University, Department of Chemical Engineering, West Lafayette, Indiana 47907.
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Abstract

The plasma polymerization of allylamine onto PAN-based carbon fibers has been investigated by XPS and SEM. Fiber surfaces were cleaned and oxidized by treating in an O2 plasma for 5 minutes. XPS characterization of pretreated samples showed surfaces functionalized with COH, C=O, and COOH species. Fibers were coated with poly(allylamine) by introducing a monomer-saturated stream of Ar gas into the plasma chamber and reacting for 2–30 minutes. Some samples were further treated in an O2 plasma to determine the stability of the polymer coating. N(1s) spectra from the fiber surfaces showed two nitrogen peaks at 399.9 eV and 400.7 eV, which may be assigned to amine and amide groups, respectively. C(1s) spectra showed a decrease with treatment in the amine carbon peak at 287.2 eV and a corresponding increase in the peak at 288.7 eV, assigned to carboxyl and/or amide carbon. The increase in higher binding energy carbon corresponded with an increase in the 400.7 eV N(1s) peak and gave evidence for the conversion of amines to amides. Total O(1s) intensity initially decreased following 2 minutes of allylamine treatment but increased with further treatment. In addition to the carbon fiber samples, a silica wafer was coated and analyzed by XPS. Quantitative XPS results revealed that all the nitrogen present on the surface was in the form of amine and not amide species. Oxygen in the form of carboxyl species was also present on coated silica surfaces. Most likely, oxygen dissolved in the allylamine monomer was carried into the plasma chamber by the Ar gas. Comparing the silica wafer with the fiber samples revealed treatments were strongly sample dependent. Even after only 2 minutes of treatment, fiber samples showed the presence of amide and substituted amide species. SEM revealed coatings filled in the fiber grooves and left clumps of material on the surface. Micrographs of fibers treated for longer times revealed surfaces covered with particles < 0.25 μm in diameter. Finally, the XPS N(1s)/C(1s) and O(1s)/C(1s) intensity ratios indicated that some polymer remained on the fiber surface even after 15 minute post O2 plasma treatment. These experiments illustrate that plasma polymerization can be effective for functionalizing carbon fiber surfaces, but that optimization of conditions is necessary to improve wetting and control amine/amide functionality.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 305: Symposium I – High-Performance Polymers and Polymer Matrix Composites , 1993 , 129
Copyright
Copyright © Materials Research Society 1993

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