Development of novel EELS methods to unveil nanoparticle properties
[eng] The aim of this thesis has been two-fold. First, to develop new processing and analysis tools and strategies for extracting information from EELS data, and second, to apply the methods to different nanoparticle systems to shed light to relevant phenomena related to their synthesis and properti...
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| Tipo de recurso: | tesis doctoral |
| Estado: | Versión publicada |
| Fecha de publicación: | 2019 |
| País: | España |
| Institución: | Universidad de Barcelona |
| Repositorio: | Dipòsit Digital de la UB |
| OAI Identifier: | oai:diposit.ub.edu:2445/133158 |
| Acceso en línea: | https://hdl.handle.net/2445/133158 http://hdl.handle.net/10803/666906 |
| Access Level: | acceso abierto |
| Palabra clave: | Electrònica Nanopartícules Espectroscòpia de pèrdua d'energia d'electrons Electronics Nanoparticles Electron energy loss spectroscopy |
| Sumario: | [eng] The aim of this thesis has been two-fold. First, to develop new processing and analysis tools and strategies for extracting information from EELS data, and second, to apply the methods to different nanoparticle systems to shed light to relevant phenomena related to their synthesis and properties. In this regard, chapter 1 presented and overview of the EELS fundamentals and of the state of the art of the technique. Chapter 2 was focused on the advanced computational methods related to EELS data analysis. Moreover, the application of cluster analysis to EELS was introduced, showing its possibilities as an image segmenting and phase identification tool. The following chapters were devoted to the investigation of different material science problems related to NPs that take advantage of the capabilities of quantitative EELS. The results were grouped by increasing complexity of the performed analysis, with chapter 3 devoted to characterizations that were mainly carried out using EELS elemental mapping, chapter 4 being related to ELNES analysis and chapter 5 to EELS tomography. In chapter 2, the adaptation of data clustering algorithms to the analysis of EELS data, developed within the scope of the present thesis, has been undertaken. In chapter 3.1 the organic synthesis of FeOx@SiO2 NPs was assessed. Several findings were obtained through the HRTEM, STEM-HAADF and EELS characterization of the FeOx@SiO2 NPs at different stages of its synthesis. In chapter 3.2, concerning Au-Ag-Se and the Au-Ag-S system cation exchange reactions several findings were made. Chapter 4 was devoted to the characterization of different NPs with an emphasis on the direct observation the oxidation state of its constituents through EELS. In chapter 4.1, the synthesis of MnOx/Fe3O4 core/shell NPs was assessed. In chapter 4.2, the measurement of oxidation state at atomic resolution in spinel crystals was proposed as a method to assess cation inversion in the crystal. The necessary methods were developed and applied to iron oxide/manganese oxide core/shell NPs. Chapter 5 was devoted to the combination of EELS and tomography. In chapter 5.1 the synthesis of cobalt oxide/cobalt ferrite (CoO@CFO) core/shell NPs and cobalt oxide/manganese ferrite (CoO@MFO) NPs was investigated. Chapter 5.2 was focused on the achievement of an oxidation state-sensitive tomographic reconstruction. |
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