Sandison, Mairi Elizabeth
Micro- and nano-electrode arrays for electroanalytical sensing.
PhD thesis, University of Glasgow.
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A systematic investigation of the electrochemical behaviour of two sets of microelectrode arrays, fabricated by standard photolithographic and reactive-ion etching techniques, is presented. The first set of microelectrode arrays had a constant relative centre-centre spacing of 10r (where r is the electrode radius). As a value of r was decreased, the cyclic voltammograms recorded from the array became increasingly peak-shaped, due to merging of the diffusion fields of the individual electrodes. Furthermore, it was shown that the peak current densities obtained were largest for the arrays with the smallest individual electrodes, as were the signal-to-noise ratios (SNRs). Electroplating the individuals electrodes with platinum black was also shown to increase the peak currents and the SNRs, due to an increase in the effective surface area. Sigmoidal voltammograms, which are indicative of radial diffusion, were obtained for an individual electrode radius of 25 mm but not for arrays with smaller electrodes. To obtain radial diffusion for an array of 2.5 mm electrodes, it was shown (using a second set of microelectrode arrays) that a minimum relative centre-centre spacing of 40r is required.
Further enhancement of the peak current densities were obtained by decreasing the size of the individual electrodes. A series of nanoelectrode arrays were fabricated using electron-beam lithography (EBL). The voltammograms obtained from these arrays exhibited a continual increase in the recorded peak current as the individual electrodes radius was decreased to a value of 110 nm. Since EBL is a slow and costly technique, nanoimprint lithography (NIL) was investigated as an alternative method of fabricating nanoelectrode arrays and comparable results were obtained from arrays produced by EBL and NIL.
A dissolved oxygen and temperature sensor incorporating a working microelectrode array was also designed and fabricated. The sector comprised a densely packed array of 2.5 mm radius electrodes and a micro-reference electrode, both of which were covered with an agarose electrolyte gel enclosed in an SU8 chamber. A thermal resistor was included for temperature compensation of the dissolved oxygen measurements. The Ag|AgCl micro-reference electrode was found to be stable for approximately 80 hours in 0.1 M KCl, with 100 nA of current passing through it. Linear calibration curves were obtained from both temperature and dissolved oxygen measurements
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