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• W3048390983 abstract "The fabrication of high-quality ultramicroelectrodes (UME) was a prerequisite for a variety of scanning electrochemical microscopic (SECM) experiments carried out in this thesis. UMEs with diameters ranging from 1 to 25 µm with a thin soda lime glass insulation (RG 2-20) and desired electrochemical properties were routinely fabricated to accomplish these targets. Further, for the imaging of the reactive oxygen species (ROS) generated during electrochemical oxygen evolution reaction (OER), the formation of transient diffusion layers during electrochemical reactions at large substrates was one major limitation. To overcome this limitation the well-known advantages of convective mass transport in electrochemical systems were exploited. After the integration of a high-precision stirring device into the experimental setup, the well-defined stirring led to steady-state diffusion layer characteristics near large substrate electrodes operated as generator electrodes. The imaging of the electrochemical hydrogen evolution at a 2 mm Pt disk electrode in the substrate generation/tip collection (SG/TC) mode demonstrated that SECM with forced convection increases the amount of obtained information. The added complexity of hydrodynamic methods in the theoretical description and construction of devices with known and reproducible mass transport conditions were addressed with numerical simulations. The reliability of the simulation was verified numerically and experimentally. The simulation showed that the rotation of the cylindrical stirrer resulted in a laminar convection near the substrate electrode. The flow profile within the liquid depended on the rotational speed of the stirrer. This enabled the formation of steady-state diffusion layers with a defined layer thickness. The constructed numerical model paves the way for additional numerical studies involving other cell and substrate geometries. The combination with other simulation modules (e.g.: electrochemistry) could provide interesting and valuable information for future applications. Hydrodynamic SECM further enabled the detection and imaging of the production of ROS at Pt and boron-doped diamond (BDD) macroelectrodes during OER. The combination of the tip-substrate voltammetry with forced convection resulted in a measurement principle similar to the rotating ring disk electrode and enabled the detection of ROS at BDD and Pt. Imaging in hydrodynamic SG/TC mode revealed that both, H2O2 and another reducible ROS species, are produced simultaneously at different domains depending on the local boron content of the surface. These pioneering experiments established the advantage of hydrodynamic SECM for locally resolved studies of highly reactive species produced during electrochemical gas evolution reaction. The increased amount of accessible analytical information aids toward a better understanding of electrochemical processes. The application of SECM in combination with forced convection to other heterogeneous reactions could help to expand the knowledge in other scientific fields and opens the door for new applications. In addition, the high-resolution SECM was used to image individual gold nanowires (AuNWs) immobilized on glass and gold coated glass slides in negative and positive feedback modes, respectively. Later the enzymatic peroxidase activity of immobilized horseradish peroxidase on individual AuNWs was imaged. These images revealed a higher enzymatic activity located at the ends of the AuNWs. This work can be further extended for the characterization of other novel nanomaterials and to study their redox behavior alone or in combination with other redox enzymes. In another work, SECM was used to provide complementary information in combination with the atomic/chemical force microscopy to evaluate the surface characteristics of pretreated carbon fiber reinforced plastics (CFRP). SECM images revealed the exposure of carbon fiber strands and delivered additional information about the chemical and morphological structure of the pretreated CFRP." @default.
• W3048390983 created "2020-08-18" @default.
• W3048390983 creator A5016768752 @default.
• W3048390983 date "2020-08-03" @default.
• W3048390983 modified "2023-09-23" @default.
• W3048390983 title "Method development for scanning electrochemical microscopy and its application for material characterization" @default.
• W3048390983 hasPublicationYear "2020" @default.
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