Infrared (IR) and x-ray photoemission spectroscopy (XPS) studies have been made on heterogeneously iodine-doped polyphenylacetylene (PPA) polymer films. Similarities and differences between the doping processes (heterogeneous and homogeneous) are presented. Results point to a surface doping process in the heterogeneously doped films vs. a bulk process in the homogeneously doped materials (doped in solution). The counter anion moiety in the films appears to be the polyiodide I<sub>5</sub><sup>−</sup> ion, as contrasted to the bulk powder (homogeneously doped) polymer in which the species of I<sub>2</sub>, I<sub>3</sub><sup>−</sup> in the presence of a predominance of I<sub>5</sub><sup>−</sup> ion coexist.

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