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Dang, Ning. "Développements de la microscopie électrochimique à balayage à sonde à gel". Electronic Thesis or Diss., Université de Lorraine, 2020. http://www.theses.fr/2020LORR0243.
Pełny tekst źródłaIn the past 30 years, scanning electrochemical probe microscopy (SEPM) techniques have been developed as powerful tools for studying electrochemistry at micro/nano scale. The most developed and commercialized techniques are Scanning Electrochemical Microscopy (SECM) and Scanning Ion Conductance Microscopy (SICM). However, the entire sample is immersed in the electrolyte solution during the measurements, which may yield uncontrolled change of the surface due to the long scanning time. Instead of localizing electrode, the electrolyte can also be localized, which is known as Scanning Droplet Cell (SDC) or Scanning Electrochemical Cell Microscopy (SECCM). The experiments are carried out under ambient conditions. However, the spreading of droplet over sample surface may be affected by the hydrophilicity and roughness of sample, which brings challenges in quantitative analysis. Recently, Scanning Gel Electrochemical Microscopy (SGECM) was reported by our group as a novel SEPM technique. It is mainly based on a gel probe that immobilizes the electrolyte on a micro-disk electrode. Thus, the analysis can be achieved in ambient environment with controllable electrolyte spreading. This thesis is devoted to the further developments of SGECM. Foremost, the background of developments of SGECM is introduced in Chapter I. Different SEPM techniques, gel polymer electrolytes, achievements of SGECM are systematically presented, respectively. In Chapter II, the lateral physical resolution of SGECM is thoroughly and quantitatively studied by both marking single pixels and scanning over periodic samples. In chapter III, the potentiometric mode of SGECM is developed based on a novel Ag/AgCl-gel micro-reference electrode. As the gel probe undergoes thousands of pressing-stretching cycles in a mapping measurement, it is highly important to improve its mechanical strength. Chapter IV describes the preliminary effort of chemically cross-linking chitosan gel by glutaraldehyde. Chapter V further pushes forward the development of integrated gel probes with both working and reference electrode
Dhahri, Samia. "Analyse topographique, mécanique et électrochimique à l'échelle sub-micrométrique de processus pilotes par les bactéries : Utilisation combinée de techniques de microscopie à sonde locale AFM - Microscopie à force atomique - et SECM - Microscopie électrochimique". Thesis, Montpellier 2, 2013. http://www.theses.fr/2013MON20146/document.
Pełny tekst źródłaThe presence of biological matter (biofilms) in deep geological sites for storage of, for instance, toxic elements or groundwater in aquifers was clearly proved. That biomass triggers physical and chemical processes which greatly modify the durability and the sustainability of the sites. These processes, mainly from oxidative/reductive reactions, are poorly understood. This is mainly due to the fact that former studies were done at the macroscopic level far away from the micrometric scale where relevant processes induced by bacteria take place. Investigations at microscopic level are needed. Thus, we developed an experimental set-up based on the combined use of optical microscopy (transmission), atomic force microscopy (AFM) and electrical and electro-chemical AFM microscopy (EC_AFM) in order to get simultaneous information on topographic and electro-chemical processes.The first highly sensitive step was to use AFM with biological samples in liquid environment: we present here a study about AFM imaging of living, moving or self-immobilized bacteria, in their genuine physiological liquid medium and in true in vivo conditions. No external immobilization protocol, neither chemical nor mechanical was needed. For the first time, the native gliding movements of Gram negative Nostoc cyanobacteria upon the surface were studied by AFM. AFM height and mechanical stiffness data were simultaneously acquired. From these, mechanical parameters, inner turgor pressure and Young modulus, were derived for different bacterial species (Anabaenopsis circularis, Rhodococcus wratislaviensis). Our study revealed that AFM imaging is thus possible on moving living species. These results open a large window on new studies of both dynamical phenomena of practical and fundamental interests such as the formation of biofilms and dynamic properties of bacteria in real physiological conditions.The second delicate step was to combine AFM and optical measurements with electrical ones. We mounted a new experimental set-up coupling real-time (i) monitoring of optical properties as the optical density (OD) evolution related to bulk bacterial growth in liquid or as the counting of number of bacteria adhering on the surface of the sample as well and (ii) electrical and electrochemical measurements. Furthermore, these results will shortly be applied to the optimized monitoring of the in-situ activity of bacteria consuming oil pollutants, following this way, in real-time, the bioremediation of an oil-contaminated soil (ANR ECOTECH_BIOPHY program)
Payan, Sandrine. "Comportement à la corrosion galvanique de matériaux composites à matrice d'alliage d'aluminium renforcée par des fibres de carbone haut-module". Phd thesis, Université Sciences et Technologies - Bordeaux I, 2001. http://tel.archives-ouvertes.fr/tel-00003521.
Pełny tekst źródłaVerchere, Lena. "Interactions microstructure - mécanique - électrochimie locale : application à l'alliage base nickel A600". Thesis, Bordeaux, 2019. http://www.theses.fr/2019BORD0239.
Pełny tekst źródłaStress corrosion cracking (SCC) is a local damaging phenomenon, which results from the synergy of microstructural, mechanical and environmental parameters. Understanding the interactions between those parameters allows manufacturers to continuously improve their reliability models for components and thus to improve facility safety. The present study focuses on Alloy 600, a nickel-based alloy which is used in pressurized water reactors and subject to SCC.Understanding and modelling interactions between the material, mechanics and environment requires decreasing the scale down to heterogeneities of the microstructure, mechanical fields and electrochemical properties, in order to avoid averaging effects. In this study, this scaling was achieved thanks to the use of experimental and numerical local techniques.A scanning electrochemical microscope (SECM) made it possible to measure currents at the grain scale. The effect of grain crystallographic orientation on the electrochemical properties of the passive film was quantified by means of a coupling of SECM with EBSD. The effect of the grain boundary type was also investigated. Thereafter, same measurements were conducted on a specimen under mechanical load thanks to the development of an experimental set-up composed of an in situ tensile machine coupled to SECM. The microstructure which was obtained by EBSD was then used to recreate a virtual microstructure on which local mechanical fields were determined through a crystal plasticity computation. The influence of cold-work and that of a tensile load on surface reactivity were then demonstrated at the microstructural scale, attesting that SCC models must integrate local heterogeneities
Rault, Vincent. "Analyse locale de la corrosion des renforts métalliques dans les pneumatiques exposés à des environnements représentatifs : vers un modèle prédictif". Thesis, Dijon, 2015. http://www.theses.fr/2015DIJOS022.
Pełny tekst źródłaThis work deals with analysis and corrosion prediction of steel cords exposed in representative environments. In this study, the system will become more and more complex starting from “délaitonné” metal reinforcement (perlitic) via the brass metal reinforcement (brass layer) to finish with the metal reinforcement sulfide (sulfide layer). This approach allows you to understand step by step corrosion phenomena and the interaction between different layers. Materials of the study are first characterized by microscopy techniques (SEM-EBSD, TEM) and surface analysis (XPS, Auger). These microstructural informations and chemical composition are essential for interpretation of corrosion tests. Electrochemical tests are worked out in 0,1M NaCl to observe and quantify corrosion behavior of the three kind of steel cords. Quantification is a significant element to establish predictive corrosion models. Two electrochemical techniques are used, measurements at global scale (voltammetry, electrochemical impedance, galvanic coupling ...) and locally measurements (microcell). Measurements at the local scale are directly linked to EBSD maps thanks to the microcell. A direct link microstructure-corrosion is established. From electrochemical tests, solutions analysis (AAS, ICP ...) and local pH measurements are performed to quantify species passing into solution. These results are input data to define a representative environment.New electrochemical tests are then performed in this representative solution to study the impact of this medium on the steel cords corrosion
Rode, Sabine. "Analyse spatio-temporelle des phénomènes hydrodynamiques et de transfert de matière au sein d'un réacteur à lit fixe opérant en écoulement monophasique de liquide ou en co-courant vers le bas de gaz et de liquide : mise en œuvre de la technique des microsondes électrochimiques". Vandoeuvre-les-Nancy, INPL, 1992. http://www.theses.fr/1992INPL093N.
Pełny tekst źródłaPortalis, Guillaume. "Compréhension des phénomènes de « cross-talking » au sein des accumulateurs Li-ion". Thesis, Sorbonne université, 2020. http://www.theses.fr/2020SORUS001.
Pełny tekst źródłaMany different degradation mechanisms can occur during the ageing of Li-ion batteries. Among them, a particular phenomenon takes place within the LiFePO4 (LFP)/graphite system during battery cycling operation, namely the “cross-talking”. The LFP material dissolves and the Fe2+ species migrate toward the graphite electrode and then reduce to form iron deposits in its protective layer (SEI). This poisoning entails a linear storage capacity fading during cycling and therefore reduces the life of the battery.The methodology used in this work bears on accelerated ageing tests carried on LFP/graphite coin cells and also relies on the characterization of the electrodes materials and the electrochemical processes thanks to a non-destructive technique, namely the electrochemical impedance spectroscopy (EIS). This approach is a preliminary step in the study of aging because it is necessary to understand the mechanisms at stake at each electrode.As a first step, several studies have been carried out in order to attribute the obtained EIS signals for each electrode material to their physico-chemical properties. In a second part, the performance and properties of accumulators during cycling were investigated. Thanks to the studies previously carried out by EIS, we were able to characterize the deterioration of the properties of the graphite electrode and its SEI due to the cross-talking from the early stage of the battery cycling. We have also shown that this phenomenon is thermally activated with greater degradation following high-temperature cycling
Jaouen, Kévin. "Backside absorbing layer microscopy : a new tool for the investigation of 2D materials". Thesis, Université Paris-Saclay (ComUE), 2019. http://www.theses.fr/2019SACLS296/document.
Pełny tekst źródłaOptical microscopy based on anti-reflective coatings is a simple yet powerful characterization tool which notably allowed the first observation of graphene in 2004. Since then, the field of two-dimensional (2D) materials has developed rapidly both at the fundamental and applied levels. These ultrathin materials present inhomogeneities (edges, grain boundaries, multilayers, etc.) which strongly impact their physical and chemical properties. Thus their local characterization is essential. This thesis focuses on a recent enhanced-contrast optical microscopy technique, named BALM, based on ultrathin (2-5 nm) and strongly light-absorbing (metallic) anti-reflective layers. The goal is notably to evaluate the benefits of this technique for the study of 2D materials and their chemical reactivity. The various levers to improve 2D materials observation were investigated and optimized for two model materials: graphene oxide and MoS₂ monolayers. The investigation of molecular layer deposition dynamic notably showed the extreme sensitivity of BALM for such measurements and the significant contribution of multilayers anti-reflective coatings to enhance contrast during the observation of 2D materials. One of the main assets of BALM comes from its combination to other techniques. We particularly considered the coupling between optical measurements and electrochemistry for which the anti-reflective layer serves as working electrode. We investigated optically the dynamic of electrochemical reduction of Graphene Oxide (GO), the electrografting of organic layers by diazonium salts reduction on GO and its reduced form (rGO), as well as the intercalation of metallic ions within GO sheets. By combining versatility and high-contrast, BALM is established as a promising tool for the study of 2D materials, especially for the local and in situ characterization of their chemical and electrochemical reactivity