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Investigation of localized electrochemical interfaces with advanced microscopic techniques : AFM-SECM and FIB/SEM tomography

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Erstveröffentlichung
2019-11-13
DOI
10.18725/OPARU-22165
Dissertation


Authors
Holzinger, Angelika
Referee
Kranz, Christine
Behm, Jürgen R.
Faculties
Fakultät für Naturwissenschaften
Institutions
Institut für Analytische und Bioanalytische Chemie
Institut für Oberflächenchemie und Katalyse
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https://oparu.uni-ulm.de/xmlui/license_opod_v1
Abstract
Combined scanning probe techniques (SPM) enable the investigation of localized surface properties. Amongst other hybrid methods, atomic force - scanning electrochemical microscopy (AFM-SECM) is highly attractive for studying processes at the solid/liquid interface, and also for investigations of liquid/liquid interfaces. In order to enhance the field of applications, AFM-SECM probes may be modified facilitating the requirements for biomedical applications and for usage with electroanalytical techniques. Whereas AFM-SECM provides predominantly information of surface processes, the combination of focused ion beam (FIB) and scanning electron microscopy (SEM) enables the detection and reconstruction of the inner structure of (nano)porous materials. Within the first part of this thesis, the focus of research is targeted towards modification of AFM-SECM probes facilitating biomedically relevant measurements, such as sensing hydrogen peroxide (H2O2) release or generation in close proximity to a sample surface (chapter 4), and localized pH sensing with associated surface changes (chapter 5). In chapter 6, detailed investigations of FIB-milled nanoporous arrays in silicon nitride (SiN) membranes are presented, which were used as solid-state support for electrochemistry at the interface between two immiscible electrolyte solutions (ITIES). The suitability of AFM-SECM in the investigation of micro- and nanoscale interfaces is shown by the performance of AFM-SECM with a conductive AFM tip, which was used to visualize the diffusion behavior at these nanoporous arrays. In addition, the localized electrochemical deposition of silica at the nanoITIES was used to visualize the location of the interface within the nanopores. FIB/SEM tomography was performed for the investigations of the location of this interface at such silica deposits.
Date created
2019
Subject Headings
Elektrochemie [GND]
Rasterkraftmikroskopie [GND]
Festkörperoberfläche [GND]
Nanopartikel [GND]
Electrochemistry [LCSH]
Nanostructured materials [LCSH]
Atomic force microscopy [LCSH]
Scanning electrochemical microscopy [LCSH]
Focused ion beams [LCSH]
Keywords
AFM-SECM; FIB/SEM tomography; Electrochemical micro- and nano-interfaces
Dewey Decimal Group
DDC 540 / Chemistry & allied sciences

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Holzinger, Angelika (2019): Investigation of localized electrochemical interfaces with advanced microscopic techniques : AFM-SECM and FIB/SEM tomography. Open Access Repositorium der Universität Ulm. Dissertation. http://dx.doi.org/10.18725/OPARU-22165

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