Fabrication, characterization, and potential application of carbon fiber cone nanometer-size electrodes

A novel method has been developed for the fabrication of carbon fiber cone nanometer-size ultramicroelectrodes (nanoelectrodes) with overall tip dimensions as small as 50 nm in diameter. In this method, carbon fibers were initially etched by an argon ion beam thinner. Afterward, a single etched carbon fiber was inserted into a glass capillary, which was then sealed by heating the glass/fiber interface in a vacuum; thus, no epoxy resin is involved. The success rate of our fabrication route for the electrodes with overall tip diameters of up to 500 nm was about 80%; for those with tip diameters of up to 100 nm, it was about 50%. The fabricated carbon fiber cone nanoelectrodes (CFCNEs) were inspected by optical and scanning electron microscopy. Their electrochemical behavior was examined by cyclic and linear sweep voltammetric measurements of ferricyanide and ferrocene ions in aqueous and nonaqueous media. The potential analytical applicability of the CFCNEs was tested by differential pulse voltammetric measurements of two well-known neurotransmitters, dopamine (DA) and 5-hydroxytryptamine (5-HT), and the results achieved were highly satisfactory. The calibration plots obtained were linear over the ranges from 5.0 × 10(-7) to 1.0 × 10(-4) and from 2.0 × 10(-6) to 1.0 × 10(-4) mol/L, with limits of detection of 1.0 × 10(-7) and 5.0 × 10(-7) mol/L for DA and 5-HT, respectively. Some advantages and improvements of the proposed CFCNE fabrication method, especially with respect to smoothness of the fiber (electrode) surface, strength, and control over the fiber tip dimensions, are also discussed.