Theoretical and Experimental X-Ray Photoelectron
Spectroscopy Investigation of Ion-Implanted Nafion
EUFROZINA A. HOFFMANN,
1,2
ZOLTAN A. FEKETE,
1,2
LJILJANA S. KORUGIC-KARASZ,
1
FRANK E. KARASZ,
1
EUGENE WILUSZ
3
1
Department of Polymer Science and Engineering, University of Massachusetts, Amherst, Massachusetts 01003
2
Department of Physical Chemistry, University of Szeged, Szeged, Hungary H-6701
3
U.S. Army Natick Soldier Center, Natick, Massachusetts 01760
Received 18 March 2003; accepted 13 June 2003
ABSTRACT: The membrane properties of a Nafion surface can be modified by ion
implantation with N
+
or F
+
. The results are presented of an X-ray photoelectron
spectroscopy (XPS) study of implanted surfaces. For the interpretation of the XPS
spectra, calculations using a semiempirical quantum chemical formalism (AM1) have
been applied, in conjunction with a charge–potential model, to predict the C
1s
core
electron binding energies. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42:
551–556, 2004
Keywords: semiempirical calculations; quantum chemistry; fluoropolymers; ESCA/
XPS; theory
INTRODUCTION
Nafion is a copolymer of tetrafluoroethylene and
perfluoro[2-(fluorosulfonylethoxy)-vinyl]ether,
1
and it is widely used in fuel cells as an electrolyte
membrane. This polymer has been a subject of
interest because of its membrane properties, such
as proton transport combined with chemical in-
ertness.
2–16
Ion implantation can further modify
the properties by developing barrier layers that
are selectively permeable to water vapor.
In the ion-implantation process, the target sur-
face is bombarded by a beam of ions. In this tech-
nique, the ion energy is typically 100 keV or more,
at normal incidence to the surface; this results in
penetration depths of hundreds of nanometers. In
contrast, in ion etching, a related technique, the
removal of one or more layers of atoms is achieved
by ion beams hitting the substrate at nonnormal
angles with energies in the range of 1–5 keV. This
leads to penetration depths of a few nanometers
and the transfer of collisional energy to target
atoms.
X-ray photoelectron spectroscopy (XPS) is a
widely used method for surface analysis that can
be applied to the analysis of polymer materi-
als.
17–19
Although X-ray exposure can damage
polymers, this problem becomes significant in
perfluorinated polymers only after exposures of
over 30 min.
20,21
Insulators pose a problem in this
technique because of charge buildup, and so peak
positions are usually assigned with respect to a
known peak in the spectrum. The assignment of
the peaks can be greatly aided by parallel theo-
retical considerations.
It has been recognized that partial atomic
charges play a decisive role in determining the
shifts of the binding energy (E
b
).
22
Calculated
charges have been used to correlate chemical
Journal of Polymer Science: Part A: Polymer Chemistry, Vol. 42, 551–556 (2004)
© 2003 Wiley Periodicals, Inc.
551