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Title: Nanoscale materials characterisation : nanoelectrode fabrication for topographic and electrochemical mapping
Author: Edmondson, James
ISNI:       0000 0004 9358 2838
Awarding Body: University of Warwick
Current Institution: University of Warwick
Date of Award: 2019
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Historical electrochemical methods of materials characterisation typically examine the macroscale response of a system of interest. This provides some information, but makes it difficult to elucidate the fundamental relationship between structure and functionality of a material. For this reason there has been a large push towards studying structure-activity relationships at the nanoscale or single entity level, with electrochemical imaging techniques coming to the fore. These techniques typically use a mobile electrode probe to investigate the system, and the probe that is used (a “nanoelectrode”) is key. A previous method of nanoelectrode fabrication involving the electrodeposition of platinum on pyrolysis formed carbon nanoelectrodes has been reported and investigated in terms of reproducibility and most effective methods of characterisation (Chapter 2). New methods for fabrication are still being pursued and a recent approach utilising chemical reduction at a nanopipette-solution interface is investigated for its application in electrochemical imaging techniques (Chapters 4 & 5). There is a myriad of analytical techniques for surface materials characterisation and several fall within the category of scanning electrochemical probe microscopy (SEPM). Within SEPM, hybrid techniques are popular, combining the advantages of individual techniques. The combination of scanning tunnelling microscopy (STM) with scanning electrochemical microscopy (SECM) has shown promise in previous studies, but has not been widely adopted due to the challenges associated with probe fabrication and instrument operation. These challenges have been addressed with the assessment of SEPM systems for conductance and/or tunnelling - SECM measurements using a novel scanning protocol (Chapter 3). If truly molecular topographical resolution is the goal, then STM has proven itself to be an extremely successful technique. To demonstrate, molecules of benzotriazole were deposited on a Cu(110) surface to elucidate fundamental structural information, this system is one where STM-SECM or conducting-SECM could potentially be applied in the future (Chapter 6).
Supervisor: Not available Sponsor: Engineering and Physical Sciences Research Council
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: QD Chemistry ; TP Chemical technology