TY - JOUR
T1 - Carbon Composite Microelectrodes: Charge Percolation and Electroanalytical Performance
AU - Forster, Robert J.
AU - Céspedes, Francisco
AU - Alegret, Salvador
AU - Ramírez-García, Sonia
PY - 2004/2/1
Y1 - 2004/2/1
N2 - Microelectrodes based on two different epoxy-graphite composites (Araldite-M/HY5162 and Araldite-PY302-2/HY943) that are compatible with organic solvents have been developed and characterized. The variation in the bulk conductivity with graphite particle loading is described by percolation theory and indicates that the particles interact strongly with one another. The percolation threshold is 52% v/v loading of graphite, and this composite exhibits a bulk conductivity of 15 S m-1. Microdisk electrodes of 25-μm diameter were produced by first etching a microcavity at the tip of a platinum microelectrode, which was then packed with a composite containing 60% v/v graphite so as to optimize both electrical conductivity and the electrode stability in acetonitrile and methanol solutions. Solution phase voltammetry of ferrocene is nearly ideal, and the responses are dominated by radial diffusion (slow scan rates) and semi-infinite linear diffusion (fast scan rates). The microelectrodes display high signal-to-noise ratios, good sensitivity, and low detection limits. The response times given by the product of the resistance, R, and capacitance, C, are 7.5 × 10-4 and 1.4 × 10 -1 s for the Araldite M and PY302-2 composites, respectively. Although these response times are significantly slower than those associated with microelectrodes based on carbon fibers or metal wires, they are sufficient for time-resolved electroanalytical applications. The long response times arise from the large composite resistances, 3.1 × 1011 and 8.3 × 1011 Ω CM-2 for Araldite M and PY302-2, respectively. Voltammetry of ferrocene in the absence of deliberately added supporting electrolyte is also reported. Significantly, indistinguishable slopes and intercepts for a calibration curve of peak current vs ferrocene concentration where 2 < [ferrocene] < 50 μM are obtained in the presence and absence of supporting electrolyte.
AB - Microelectrodes based on two different epoxy-graphite composites (Araldite-M/HY5162 and Araldite-PY302-2/HY943) that are compatible with organic solvents have been developed and characterized. The variation in the bulk conductivity with graphite particle loading is described by percolation theory and indicates that the particles interact strongly with one another. The percolation threshold is 52% v/v loading of graphite, and this composite exhibits a bulk conductivity of 15 S m-1. Microdisk electrodes of 25-μm diameter were produced by first etching a microcavity at the tip of a platinum microelectrode, which was then packed with a composite containing 60% v/v graphite so as to optimize both electrical conductivity and the electrode stability in acetonitrile and methanol solutions. Solution phase voltammetry of ferrocene is nearly ideal, and the responses are dominated by radial diffusion (slow scan rates) and semi-infinite linear diffusion (fast scan rates). The microelectrodes display high signal-to-noise ratios, good sensitivity, and low detection limits. The response times given by the product of the resistance, R, and capacitance, C, are 7.5 × 10-4 and 1.4 × 10 -1 s for the Araldite M and PY302-2 composites, respectively. Although these response times are significantly slower than those associated with microelectrodes based on carbon fibers or metal wires, they are sufficient for time-resolved electroanalytical applications. The long response times arise from the large composite resistances, 3.1 × 1011 and 8.3 × 1011 Ω CM-2 for Araldite M and PY302-2, respectively. Voltammetry of ferrocene in the absence of deliberately added supporting electrolyte is also reported. Significantly, indistinguishable slopes and intercepts for a calibration curve of peak current vs ferrocene concentration where 2 < [ferrocene] < 50 μM are obtained in the presence and absence of supporting electrolyte.
UR - https://dialnet.unirioja.es/servlet/articulo?codigo=817303
U2 - 10.1021/ac034536p
DO - 10.1021/ac034536p
M3 - Article
SN - 0003-2700
VL - 76
SP - 503
EP - 512
JO - Analytical Chemistry
JF - Analytical Chemistry
IS - 3
ER -