This thesis describes the development of an electrochemical scanned probe microscope, SECCM, outlining the need for such a development, by highlighting previous techniques and their limitations. SECCM consists of a double barrel capillary pulled to small dimensions, filled with electrolyte solution and a redox mediator of choice, with a QRCE is inserted into each channel. A potential is applied between the QRCEs, whilst modulating the pipet normal to the surface. The probe is translated towards the surface and once contact is established, a modulation in the ion current arises due to the physical oscillation of the probe, which is then used as a feedback parameter for imaging. The potential at the working electrode substrate is also controlled. SECCM is introduced using a model test substrate, gold bands on glass, showing that the probe is able to track topographical features, making simultaneous electrochemical measurements. Ion conductance measurements between the two QRCEs, are shown to be sensitive to the nature of the substrate investigated. The fundamental electrochemical behaviour of CVD graphene and SWNT is investigated. A multimicroscopy approach is used for CVD graphene studies, correlating surface structure and activity, deducing heterogeneous electron transfer kinetics through simulation. The SWNT samples are studied in two different morphologies: as 3D forests; and, as a 2D network. In the forests, the probe is positioned at the ends and sidewalls, making spot measurements. The voltammetric behaviour shows very similar responses, whilst in the network, a nanosized probe is scanned across the surface, showing relatively uniform activity across an entire tube. These new insights indicate that SWNTs are highly active electrode materials. The fabrication and characterisation of SECM-SICM probes, in a straightforward manner is also presented. These types of probes were found to be ideal for the investigation of biological samples, being extremely easy and quick to fabricate.
| Identifer | oai:union.ndltd.org:bl.uk/oai:ethos.bl.uk:569005 |
| Date | January 2012 |
| Creators | Ebejer, Neil |
| Publisher | University of Warwick |
| Source Sets | Ethos UK |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
| Source | http://wrap.warwick.ac.uk/53742/ |
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