| Abstract: | A high‐yield, reliable, and reproducible method has been successfully developed to fabricate poly(oxyphenylene)‐coated carbon fiber ultramicroelectrodes (POCF UMEs) with tip radii r<2 μm. During the insulation process, the tip of the electrochemically etched electrode is protected by inserting it into an inert polymer while the remainder of the electrode is insulated by electrochemical deposition of a 1–3 μm thick poly(oxyphenylene) film. Optimum conditions for poly(oxyphenylene) deposition are developed and the resulting carbon fiber UMEs showed good cyclic voltammetric behavior even after storage for more than one year. These UMEs were tested for use as amperometric scanning electrochemical microscopy (SECM) tips and successfully imaged Au/Kel‐F and Al/SiCp metal matrix composites. |
