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Pearmain, David. "Electron microscopy characterisation of size-selected Pd clusters and industrial Pd catalysts." Thesis, University of Birmingham, 2011. http://etheses.bham.ac.uk//id/eprint/1509/.
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This thesis presents an investigation into the morphology of palladium (Pd) size selected clusters and industrial Pd catalysts using high angle annular dark field scanning transmission electron microscopy (HAADF-STEM) technique. The driving force of this work is to establish reliable and efficient methods for the structural characterisation of nanostructures. The characterisation of nanostructures is essential to our fundamental understanding of cluster use within applications, such as catalysis. The complexity of the morphology of industrial catalysts presents a significant challenge to rapid screening techniques. This thesis presents an efficient method which uses size selected clusters as mass standards in STEM based mass spectrometry. Size selected clusters were created using a radio frequency magnetron sputtering cluster beam source in conjunction with a lateral time of ight mass selector, Pd clusters were soft-landed onto amorphous carbon grids between the size range of N = 454 to 10,000 (\(\pm\)4%), with a deposition energy of 500 eV. The quantitative image analysis allows one to gain insight into each catalytic Pd particle and, in combination with two-dimensional diameter measurements, evaluate the three dimensional morphology of the particles. The use of the cluster source has also allowed investigation into the formation mechanisms of nanostructures, finding specific size-dependant morphological features for Pd clusters. Elongation of Pd clusters has been observed for cluster sizes of \(\geq\) 2000 atoms, as well as the onset of voids within the cluster structure for sizes \(\geq\) 2622. HAADF-STEM analysis has proved to be an invaluable tool in the determination of cluster size, independent of morphology, as well as enabling specific structural features within clusters to be revealed. An investigation into the atomic structure of supported Pd\(_{887}\) clusters is also presented. Specific structural motifs are identified using aberration corrected STEM within the sample range via direct comparison with simulated HAADF-STEM images of structures simulated using global minimum techniques.
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Ellickson, Daniel Emick. "Assessment of microscopy methods for distinguishing engineered nanoparticles from incidental nanoparticles." Thesis, University of Iowa, 2011. https://ir.uiowa.edu/etd/960.
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The objective of this study was to assess the utility of electron microscopy for the purpose of distinguishing engineered nanoparticles from "incidental" nanoparticles. Methods included the use of transmission electron microscopy (TEM) with energy dispersive spectroscopy (EDS) to analyze samples of known ratios of titanium dioxide (TiO2) to Arizona road dust (ARD) or incense particles. TEM collection methods were analyzed for two different samplers: a Marple impactor and an electro-static precipitator (ESP). TEM grids were placed on the four lowest stages of the impactor. Results for impactor stages of a 10:1 ratio of TiO2/ARD mixture displayed the following percentages TiO2: 44%, 44%, 83%, and 90%. TiO2/incense samples had very high (79%-90%) TiO2 proportions, which was not expected since the ratio was 1:1. These combustion particles did not collect with the same efficiency as TiO2 or ARD. In conclusion, incense particles were entirely carbon based and were not identifiable using TEM/EDS. The TiO2/ARD mixture demonstrated that the impactor would remove most of the larger particles so that grids on the filter stage could be used to analyze and image TiO2 mostly alone. Sampling criteria for desired particle loading had to be established in order to obtain usable TEM grids. TiO2 was distinguishable from all other particles, but accurate particle identity and proportion in samples was not obtainable for combustion particles using these methods.
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Dobryden, Illia. "Surface characterization and force measurements applied to industrial materials with atomic force microscopy." Licentiate thesis, Luleå tekniska universitet, Materialvetenskap, 2012. http://urn.kb.se/resolve?urn=urn:nbn:se:ltu:diva-17820.
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The thesis focuses on the application of force measurements with atomic force microscopy (AFM) on materials with a few surface contacts/asperities and chemically modified surfaces. The technique allows measurements of ultra-small intermolecular and surface forces, down to the piconewton level. The force measurements between surfaces of well-defined geometry are often used to measure and model the interaction between different systems of charged and neutral surfaces in various environments. However, detailed knowledge of the contacting surface profile geometry and surface properties is required to model the fundamental forces involved in the interaction. The preparation of such well-defined and idealized surfaces is often time consuming and the surfaces may not possess the behavior and properties of a source material in real processes, such as in industry. Moreover, external factors such as magnetic fields, ionic strengths and pH-values in a solution, may further complicate the evaluation. Hence, it is desirable to explore and develop techniques for trustable measurements of forces between “real” surfaces. These are often a complex composition of various force interactions and multiple surface contacts.The AFM probe technique was explored to measure force interactions between “real” particle surfaces. The work shows the applicability of the AFM technique to study the interaction forces despite the forecasted difficulties with the roughness of the particles.A technique to measure the adhesion and work of adhesion from AFM force curves was implemented and used. The thermal tune method was implemented in our commercial NT-MDT microscope to determine cantilever spring constants. The force interactions between natural microsize (m-s) magnetite particles and synthetic nanosize (n-s) magnetite particles were studied in calcium solution with concentrations of 1, 10, 100 mM and at pH values 4, 6 and 10. The changes in force interactions, due to variations in calcium concentration and pH were investigated. The adhesion force change with the concentration and pH was similar for m-s/m-s and m-s/n-s systems, and the adhesion force increased with the concentration at pH 6, except for the highest calcium concentration of 100 mM at pH 10. It was found that the magnetite surface modification could appear at the highest calcium concentration at pH 10. Moreover, the thesis contains preliminary results of the force interaction study between natural and synthetic bentonite-magnetite particles in calcium solution with concentrations of 1, 10 and 100 mM at pH 6.The influence of roughness on the calculation of contact mechanics parameters were studied with AFM and Vertical Scanning Interferometry (VSI). This is important for future development of a model to describe and characterize the force interaction between samples with multiple surface contacts. It was found that the optical artifacts, induced by VSI, have a large influence on all the roughness parameters calculated on the calibration grids, which represent extreme surface topographies.Godkänd; 2012; 20120502 (illdob); LICENTIATSEMINARIUM Ämnesområde: Fysik/Physics Examinator: Docent Nils Almqvist, Institutionen för teknikvetenskap och matematik, Luleå tekniska universitet Diskutant: Docent Aji P Mathew, Institutionen för teknikvetenskap och matematik, Luleå tekniska universitet Tid: Fredag den 1 juni 2012 kl 10.00 Plats: E632, Luleå tekniska universitet
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Lai, Pooi-fun. "TEM and structural investigations of synthesized and modified carbon materials /." Connect to thesis, 1999. http://eprints.unimelb.edu.au/archive/00000770.
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Coleman, Kristen. "Detection of silica particles in lung tissue of non-occupationally exposed individuals by computer controlled scanning electron microscopy." Thesis, University of Iowa, 2013. https://ir.uiowa.edu/etd/1572.
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For years crystalline silica has been recognized as an occupational hazard of the dusty trades with exposures resulting in silicosis. As recently as 1997, IARC categorized the respirable portion of crystalline silica as a Grade 1 human carcinogen indicating that silica may be implicated in the development of lung cancer. Evidence in the literature indicates that silica may be not only an occupational hazard, but an environmental hazard as well, with patients with no known exposure showing measurable quantities of silica within cancerous tissue samples.
This study aims to establish a methodology using computer-controlled scanning electron microscopy to examine silica content in lung cancer tissue. Furthermore, demonstrating that silica is not evenly distributed within the tissue will establish the need to use automated full scanning techniques, such as CCSEM, in order to guarantee that the analysis is not subject to random sampling error or researcher driven error, which may be rendering the traditional random sampling of zones for analysis under-representative of silica concentration in the tissue.
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Krishna, Sujata. "Atomic and electronic structure of grain boundaries in gallium arsenide." Thesis, University of Oxford, 1994. http://ora.ox.ac.uk/objects/uuid:0f7d1156-12e4-4a8d-b3a7-71ff7a8b65f1.
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HREM imaging was performed using the Jeol 4000ex microscope on specimens prepared from an as-grown ingot of semi-insulating Gallium Arsenide. Various low angle grain boundaries were imaged in the [110] orientation, misorientations varying between 4°-13°. Detailed study of a grain boundary of 11.5° misorientation about the [110] rotation axis has been carried out. Burgers vector analysis showed the presence of perfect 60° and [001] dislocations. Modelling of the [001] dislocation has been carried out using the Tersoff potential, Bond Order Potential and a tight binding Hamiltonian for GaAs, using Chadi (1984) parameters. The dislocation core was associated with an 8-membered and two 5-membered rings. Assum- ing there is a minimum of wrong bonds, we predict that the core has two wrong bonds, one being Ga-Ga, and the other As-As, both in equivalent positions where the two 5-membered rings were appended to the 8-membered ring. The Ga-Ga bond is considerably shorter and hence stronger than the As-As bond. Band structure calculations performed using a Vogl (1983) sp3s* Hamiltonian revealed deep states in the gap, which are associated with atoms in the core only. Using Stadelmann's (1987) EMS program, successful image matching of calculated images of the [001] dislocation has been achieved with the experimental image, using the atomic structure generated by tight binding relaxation. Ga and As being only two atomic numbers apart have similar scattering factors and cannot be easily distinguished in the experimental image. The equivalence of the position of the two wrong bonds greatly eases image matching as it is no longer necessary to know which is the Ga-Ga , and which is the As-As bond. This is the first suggested model of the [001] dislocation in GaAs, to the best of my knowledge. It is found to be similar to the atomic structure of the 90° partial dislocation in silicon (Bigger et al., 1992). No account of segregation of impurities to the grain boundary, or the [001] dislocation core is taken here, though it is very likely that an impurity atom would sit itself in this large space. The relaxed atomic structure for the 60° dislocation showed a doubling of periodicity along the dislocation line, similar to that found in the 30° partial in Si. The core consists of a 7-membered and a 5-membered ring with a minimum of two wrong bonds. In addition to this, quantitative comparisons of the [001] HREM image and simulated structures have been made and an iterative structure refinement carried out in order to achieve the best image matching. The resultant 'experimental-best-fit' structure was not found to be physically or chemically plausible.
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Barrales, Francisco Manuel 1986. "Extração de óleo de semente de maracujá (Passiflora edulis sp.) usando CO2 supercrítico assistido por ultrassom." [s.n.], 2015. http://repositorio.unicamp.br/jspui/handle/REPOSIP/254630.
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Orientador: Julian MartínezDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: O presente trabalho teve como principal objetivo avaliar a influência da aplicação de ultrassom na extração de óleo de semente de maracujá com CO2 supercrítico, focando no rendimento da extração, na cinética do processo, conteúdo de tocoferóis e tocotrienóis, perfil de ácidos graxos, e atividade sequestrante do radical DPPH do óleo, usando como matéria-prima sementes de maracujá misturadas com polpa provenientes da indústria de processamento da fruta. Com esse intuito, a metodologia de superfície de resposta foi empregada, partindo como base de um planejamento experimental de tipo composto central para três fatores. Os fatores avaliados foram temperatura (38; 40; 45; 50 e 52°C), pressão (13; 16; 21; 26 e 29 MPa) e potência de ultrassom (0; 160; 400; 640 e 800 W). Os extratos obtidos apresentaram alto porcentagem de ácidos graxos poli-insaturados (aproximadamente 67%) e teor de tocoferóis e tocotrienóis (entre 60 e 90 mg/100g óleo), atividade sequestrante do radical DPPH (entre 1,8 e 2,6 mg TE/g óleo) que demonstrou correlação com o conteúdo total de tocoferóis e tocotrienóis (r = +0,872). A análise de polifenóis totais não conseguiu detectar a presença de polifenóis nos extratos. A aplicação de ultrassom na menor potência (160 W) resultou vantajosa, gerando incrementos de até 29% no rendimento de SFE. Este efeito foi registrado na temperatura de 40 °C e pressão de 16 MPa. O modelo de Sovová (1994) mostrou-se adequado para descrever o comportamento da cinética de extração, permitindo avaliar os parâmetros ajustados. Quando foi evidenciado grande incremento no rendimento da SFE, decorrente da aplicação do ultrassom, os parâmetros cinéticos foram modificados, sendo o tempo da etapa CER maior, junto com o coeficiente de transferência de massa da fase fluida, houve diminuição da proporção de extrato de difícil acesso. As imagens obtidas por microscopia eletrônica de varredura com fonte de emissão de campo (FESEM) demonstraram efeitos de atrito e menor tamanho de partículas quando o ultrassom foi aplicado
Abstract: The present work had as main objective the evaluation of the effect of the application of ultrasound in the extraction of passion fruit seed oil using supercritical CO2, on the global extraction yield, the process kinetics, the tocopherol and tocotrienol content and DPPH radical scavenging activity, using as raw material passion fruit seeds mixed with pulp, a byproduct of the pulp processing industry. To accomplish that, the response surface methodology was used. The evaluated factors were: temperature (38; 40; 45; 50 and 52 °C), pressure (13; 16; 21; 26 and 29 MPa) and ultrasound power (0; 160; 640 and 800 W). Fatty acids composition, total polyphenolic content, identification and quantification of tocopherols and tocotrienols and the antioxidant activity were evaluated on the extracts, which resulted rich in polyunsaturated fatty acids (about 67%) and tocopherols and tocotrienols (between 60 and 90 mg/100g oil), of high antioxidant activity (between 1,8 to 2,6 mgTE/g oil) that shown correlation with the tocopherol and tocotrienol total content (r = +0,872). The total polyphenol analysis was not able to detect the presence of polyphenols in the extracts. The application of low power ultrasound (160 W) resulted advantageous; the SFE global yield improvement achieved 29%. This effect was registered at a temperature of 40 °C and pressure of 16 MPa. The model of Sovová (1994) was adequate to describe the extraction kinetics behavior, and it was possible to evaluate the adjusted parameters. When a great increase of SFE yield was achieved due to the ultrasound application, the kinetic parameters were modified, being the CER time and the fluid phase mass transfer coefficient increased, also showing reduction of solute ratio inside the cells. . The images obtained by field emission scanning electron microscopy (FESEM) demonstrated mechanical damage effects and smaller particle size when ultrasound was applied
Mestrado
Engenharia de Alimentos
Mestre em Engenharia de Alimentos
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Marty, Adam J. "Generation and Characterization of Nanoaerosols Using a Portable Scanning Mobility Particle Sizer and Electron Microscopy." Scholar Commons, 2014. https://scholarcommons.usf.edu/etd/5536.
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The purpose of this research is to demonstrate the ability to generate and characterize a nanometer sized aerosol using solutions, suspensions, and a bulk nanopowder, and to research the viability of using an acoustic dry aerosol generator/elutriator (ADAGE) to aerosolize a bulk nanopowder into a nanometer sized aerosol. The research compares the results from a portable scanning mobility particle sizer (SMPS) to the more traditional method of counting and sizing particles on a filter sample using scanning electron microscopy (SEM). Sodium chloride aerosol was used for the comparisons. The sputter coating thickness, a conductive coating necessary for SEM, was measured on different sizes of polystyrene latex spheres (PSLS). Aluminum oxide powder was aerosolized using an ADAGE and several different support membranes and sound frequency combinations were explored.
A portable SMPS was used to determine the size distributions of the generated aerosols. Polycarbonate membrane (PCM) filter samples were collected for subsequent SEM analysis. The particle size distributions were determined from photographs of the membrane filters. SMPS data and membrane samples were collected simultaneously. The sputter coating thicknesses on four different sizes of PSLS, range 57 nanometers (nm) to 220 nm, were measured using transmission electron microscopy and the results from the SEM and SMPS were compared after accounting for the sputter coating thickness. Aluminum oxide nanopowder (20 nm) was aerosolized using a modified ADAGE technique. Four different support membranes and four different sound frequencies were tested with the ADAGE. The aerosol was collected onto PCM filters and the samples were examined using SEM.
The results indicate that the SMPS and SEM distributions were log-normally distributed with a median diameter of approximately 42 nm and 55 nm, respectively, and geometric standard deviations (GSD) of approximately 1.6 and 1.7, respectively. The two methods yielded similar distributional trends with a difference in median diameters of approximately 11 - 15 nm. The sputter coating thickness on the different sizes of PSLSs ranged from 15.4 - 17.4 nm. The aerosols generated, using the modified ADAGE, were low in concentration. The particles remained as agglomerates and varied widely in size. An aluminum foil support membrane coupled with a high sound frequency generated the smallest agglomerates.
A well characterized sodium chloride aerosol was generated and was reproducible. The distributions determined using SEM were slightly larger than those obtained from SMPS, however, the distributions had relatively the same shape as reflected in their GSDs. This suggests that a portable SMPS is a suitable method for characterizing a nanoaerosol. The sizing techniques could be compared after correcting for the effects of the sputter coating necessary for SEM examination. It was determined that the sputter coating thickness on nano-sized particles and particles up to approximately 220 nm can be expected to be the same and that the sputter coating can add considerably to the size of a nanoparticle. This has important implications for worker health where nanoaerosol exposure is a concern. The sputter coating must be considered when SEM is used to describe a nanoaerosol exposure. The performance of the modified ADAGE was less than expected. The low aerosol output from the ADAGE prevented a more detailed analysis and was limited to only a qualitative comparison. Some combinations of support membranes and sound frequencies performed better than others, particularly conductive support membranes and high sound frequencies. In conclusion, a portable SMPS yielded results similar to those obtained by SEM. The sputter coating was the same thickness on the PSLSs studied. The sputter coating thickness must be considered when characterizing nanoparticles using SEM. Finally, a conductive support membrane and higher frequencies appeared to generate the smallest agglomerates using the ADAGE technique.
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Havlíček, Petr. "Design elektronového mikroskopu." Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2011. http://www.nusl.cz/ntk/nusl-229634.
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The aim of my Master's thesis is the design of a scanning electron microscope. The designed concept presents an innovative approach to the problems and respects all technical, ergonomic and aesthetical demands made on it. The main creative part of design process starting from the concept development and ending up with the final solution is preceded by a background research study including a historical, technical and design analysis of the electron microscope. The conclusion of my Master's thesis analyses the final design, its character and its contribution in broader context.
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Švajdová, Anna. "Design elektronového mikroskopu." Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2017. http://www.nusl.cz/ntk/nusl-319480.
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The theme of this diploma thesis is the design of a scanning electron microscope with a focused ion beam. Specifically, the thesis is focused on the design of the microscope covers and the adjacent workplace of the operator for Tescan Orsay Holding a.s.. Design is solved as the first proposal aimed at future innovation of the design of the entire product line.
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Schiavone, Marion. "Combination of biochemical, molecular and biophysical approaches to investigate the impact of strain background and production process on the yeast cell wall composition and molecular architecture." Thesis, Toulouse, INSA, 2014. http://www.theses.fr/2014ISAT0043.
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L’intérêt pour la paroi de la levure s’est accru récemment par l’explosion des activités de bioraffineries augmentant la production de biomasse, et par le besoin de valoriser cette biomasse dans d’autres débouchés comme en nutrition animale et en œnologie pour leurs propriétés probiotiques et de sorption. Le but de cette thèse était de combiner des approches biochimiques, biophysiques et les puces à ADN afin d'étudier les relations entre ces paramètres ainsi que de mettre en évidence l'impact des souches, des conditions de croissance et des procédés sur la composition et les propriétés biophysiques de la paroi cellulaire. Une méthode acido-enzymatique a été développée pour quantifier spécifiquement chacun des quatre composants de la paroi cellulaire de la levure, à savoir les mannanes, la chitine, les β-1,3-glucanes et les β-1,6-glucanes. Cette méthode a été validée sur des souches mutantes et a permis d’évaluer les effets de divers stress. Ultérieurement, l'utilisation de la microscopie à force atomique (AFM) a permis l'étude des mêmes souches et de quatre souches utilisées dans la fermentation industrielle. Ils ont démontré des propriétés nanomécaniques et adhésives distinctes, en raison de différences dans la composition et la structure de la paroi cellulaire. Dans la dernière partie, les effets du procédé d’autolyse et du séchage à lit fluidisé sont présentés. Ce procédé industriel ne modifie pas la composition de la paroi cellulaire, mais induit une modification de la topographie et des propriétés de surface de la cellule. En outre, en utilisant l'AFM nous avons imagés sur S. cerevisiae des patchs hautement adhésifs formant des nanodomaines à la surface de la celluleDue to increasing yeast biomass production resulting from the expansion of the Biorefinery as an alternative to petrol-based energy, the yeast cell wall is receiving an increasing interest as an added value product targeting agro-nutrition markets, such as in animal nutrition and in wine for its probiotic and sorption properties. The purpose of this thesis was therefore to combine DNA microarrays, biochemical and biophysical approaches in order to investigate the relationships between these parameters as well as to highlight the impact of strains, growth conditions and processes on the cell wall composition and biophysical properties. To achieve this objective, an acido-enzymatic method was developed to specifically quantify each of the four components of the yeast cell wall, namely mannan, chitin, β-1,3-glucan and β-1,6-glucan. This method was validated on mutant strains and allowed highlighten various stresses effects. Then, the use of atomic force microscopy (AFM) has allowed investigating the same strains and four strains used in industrial fermentation. They demonstrated distinct nanomechanical and adhesive properties, due to differences in their cell wall structure and composition. In the last part, the effects of the autolysis and fluid-bed drying processes are presented. This industrial process does not change the composition of the cell wall but induces a modification in topography and surface properties of the cell. Moreover, using AFM we imaged on S. cerevisiae cell surface highly adhesive patches forming nanodomains
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TAKAHASHI, ELISA A. N. "Utilização da escória de alumínio na fabricação de argila expandida." reponame:Repositório Institucional do IPEN, 2006. http://repositorio.ipen.br:8080/xmlui/handle/123456789/11461.
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Dissertacao (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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FERNANDES, ALBERTO de A. "Síntese de zeolitas e wolastonita a partir da cinza da casca do arroz." reponame:Repositório Institucional do IPEN, 2006. http://repositorio.ipen.br:8080/xmlui/handle/123456789/11429.
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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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ARAUJO, MARIANA S. de. "Utilização de resíduos de catalisador (ECAT) e cinzas da casca de arroz (CCA) na elaboração de vidros silicatos soda-cal destinados a embalagem." reponame:Repositório Institucional do IPEN, 2016. http://repositorio.ipen.br:8080/xmlui/handle/123456789/26381.
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Dissertação (Mestrado em Tecnologia Nuclear)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
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Leroy, Joël. "Caractérisation et qualification de cokes industriels : relations entre texture poreuse, microtexture, sites actifs et carboxyréactivité." Vandoeuvre-les-Nancy, INPL, 1991. http://docnum.univ-lorraine.fr/public/INPL_T_1991_LEROY_J.pdf.
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Ce travail a pour but de relier carboxyréactivité et caractéristiques de 5 cokes. On étudie en fonction de la gazéification: texture poreuse, microtexture et sites actifs. La confrontation des résultats conduit à des conclusions concordantes et complémentaires. Plus un coke est microporeux, plus il est réactif. Cependant la mésoporosité ouvre l'accès aux réactifs. Une forte réactivité résulte de la présence simultanée de micro- et de mésoporosité ce qui est en accord avec le fait que les cokes les plus réactifs présentent une grande diversité dans les dimensions des domaines d'O. M. Les variations de la réactivité au cours de la gazéification, dont le régime est essentiellement diffusionnel dans le domaine exploré, sont liées à l'évolution de la porosité. Il est possible de calculer les gazéifications interne et externe. La microtexture renseigne sur l'existence d'une microporosité et de sites actifs, pour la plupart inaccessibles, donc sur la réactivité potentielle. Cependant la réactivité effective dépend de la surface accessible. Les sites actifs ont été étudiés par T. D. P des oxydes de surface. L'Aire de la Surface Active (A. S. A. ) ainsi mesurée sur les cokes bruts est en très bonne corrélation avec leur carboxyréactivité à 900°C ce qui s'interprète comme suit: les oxydes thermodésorbés des cokes bruts proviennent des complexes formes au cours de l'extinction humide sur les sites accessibles, la carboxyréactivité considérée est liée aux sites accessibles au CO2 à 900°C. Ces deux types de sites ne sont vraisemblablement pas très différents. On teste donc ainsi directement sur un coke brut une grandeur caractéristique de sa carboxyréactivité à 900°CThis work was intended to connect the carboxyreactivity of 5 cokes samples with their physico-chemical properties. Porous textures, microtextures and active sites were studied with respect to the gasification extent. Analysis of the results leads to concordant and complementary conclusions. The more microporous a sample the more reactive. However mesoporosity gives access to the reactants. The simultaneous presence of micro-and of mesoporosity results in a high reactivity. This agrees with the fact that the most reactive cokes exhibit a wide distribution of the sizes of M. O. Dormains. Variations of reactivity during gasification, whose mode is mainly diffusional, are linked to the alterations of the porosity. It was possible to compute the extent of internal and of external gasification. Microtexture gives informations about the presence of a microporosity and of active sites, mainly non accessible, therefore about “potential reactivity”. However “effective reactivity” depends on surface accessibility. Active sites were studied by TPD of surface oxides. The Active Surface Area (A. S. A. ) determined on raw cokes correlates well with their carboxyreactivity at 900° C. This is interpreted as follows : desorbed oxides from raw cokes originate in complexes formed on accessible sites during quenching, the carboxyreactivity studied at 900°C is related to accessible sites ; these two types of sites are likely to be not too different. So it seems possible to determine on a raw coke a feature relevant of its carboxyreactivity at 900°C
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Pechard-Presson, Béatrice. "Méthodologie pour l'étude par analyse d'images de la microstructure de matériaux composites biphasés." Vandoeuvre-les-Nancy, INPL, 1997. http://docnum.univ-lorraine.fr/public/INPL_T_1997_PECHARD_PRESSON_B.pdf.
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Les matériaux composites jouent un rôle très important dans l'économie, en particulier dans les domaines de haute technicité, tel que l'aéronautique. Leurs propriétés dépendent naturellement de celles de leurs constituants, mais également des interactions entre ceux-ci. Le génie des matériaux s'intéresse à leur conception, ainsi qu'aux relations qui existent entre leur structure et leurs caractéristiques générales. L’analyse d'images permet de qualifier les microstructures visibles par microscopie optique ou électronique. Elle constitue donc un outil très intéressant pour la science des matériaux. Dans cette étude, la structure de matériaux biphasiques, utilisés pour leurs propriétés électromagnétiques en aviation militaire, a été quantifiée par analyse d'images. Des images de synthèse ont été également étudiées, ainsi que des matériaux frittés et des sols, dans le but de préciser les paramètres calculés, et d'étendre la méthodologie mise en place à d'autres types de structures. L’orientation et la dispersion des charges dans la matrice ont été étudiées, ainsi que leur distribution de taille. Leur forme, leur connexité (à partir de la théorie de la percolation) et leur fractalité ont été caractérisées. Une méthodologie adaptée à l'étude en routine de la microstructure de matériaux biphasés (i. E. à propos desquels on ne s'intéresse qu’à une phase parmi d'autres, confondues) a ainsi été mise en place.
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Levi, Sala Irene. "A study of microscopic polish on flint implements /." [Oxford] : Tempus reparatum, 1996. http://catalogue.bnf.fr/ark:/12148/cb358401027.
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Guilbaud, Sarah. "Etude du vieillissement des aérosols inorganiques industriels en milieu urbain." Thesis, Littoral, 2018. http://www.theses.fr/2018DUNK0524/document.
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Lors de leur séjour dans l’atmosphère, les aérosols sont soumis, entre autres, à des processus d’agrégation, ainsi que de condensation sur leurs surfaces. Ces processus, dit de vieillissement, dépendent du temps de résidence des particules dans l’atmosphère, des conditions météorologiques et de l’environnement chimique rencontré. Cette étude vise à caractériser l’aérosol inorganique et étudier son évolution physico-chimique sur quelques dizaines de milliers de mètres, dans les panaches industriels et urbains où les concentrations atmosphériques en particules fines (PM₁₀) sont relativement élevées. Il s’agit notamment de rendre compte de l’évolution des particules d’aérosol primaire lors d’épisodes de formation d’aérosols secondaires inorganiques.Dans ce cadre, dans un premier temps, une nouvelle méthodologie d’analyse des aérosols inorganiques, à basse température, par cryo-microscopie électronique (cryo-TSEM-EDX) a été mise au point. L’enjeu était notamment de rendre compte de l’état de mélange des composés atmosphériques d’origine secondaire (composés semi-volatils), avec l’aérosol primaire. Ces développements analytiques ont tout d’abord été réalisés à l’aide de composés modèles, avant d’être validés sur particules environnementales. Dans un second temps, l’étude des processus physico-chimiques mis en jeu lors du vieillissement des aérosols, à l’échelle locale (quelques kilomètres), a été réalisée au cours d’une campagne intensive de terrain sur le dunkerquois, visant à étudier plus particulièrement l’évolution des émissions industrielles en milieu urbain. Des prélèvements ont ainsi été réalisés en bordure de zone industrielle et sur de sites "récepteurs" sous l’influence potentielle des émissions industrielles. Les analyses réalisées sur ces particules par cryo-SEM-EDX ont notamment montré qu’en zone péri-urbaine, à quelques kilomètres de la zone industrielle, des particules émises par la sidérurgie, comme les oxydes de fer, évoluaient rapidement, pour se retrouver, en mélange interne, associés à de la matière organique particulaire. En parallèle, nous avons pu caractériser, sur ces sites récepteurs, la présence d’aérosols inorganiques secondaires absents de la zone source et donc formés au sein de l’air ambiant, lors du survol de l’agglomération dunkerquoiseDuring their transport in the atmosphere, aerosols are subject, for example, to aggregation and condensation processes on their surfaces. These processes, so-called aging, depend on particle residence time in the atmosphere, meteorological conditions and chemical environment. This study aims to characterize inorganic aerosols and to highlight their physico-chemical evolution on a few tens of thousands meters, from an industrial area to the urban environment of Dunkirk (Northern France), in which PM₁₀ concentrations are quite important. It notably includes reporting on the evolution of primary particles during the formation of secondary inorganic aerosols. First, a new analytical methodology of inorganic aerosols, at low temperature, with cryo-electronic microscopy (cryo-TSEM-EDX) has been developed. Our goal was to characterize the mixing state of secondary atmospheric components (semi-volatile components) with primary aerosols. These analytical developments have been realized with model particles, before validation on real atmospheric particles. In a second time, the study of physico-chemical processes involved in the aging of industrial inorganic aerosols has been undertaken through an intensive field campaign. The objective is to describe the particles evolution between the industrial zone and receptor sites located in the suburb of Dunkirk. Our main results show that Fe-rich particles (Fe oxides), released in the atmosphere by steelworks, incorporate particulate organic matter in a few kilometers, between the source and receptor sites. In addition, the formation of secondary inorganic aerosols (SIA), not present at the source, has been evidenced. Clearly, these SIA have been formed during the transport of air masses over the urban area
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Pedgley, Owain F. "Industrial designers' attention to materials and manufacturing processes : analyses at macroscopic and microscopic levels." Thesis, Loughborough University, 1999. https://dspace.lboro.ac.uk/2134/7155.
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Silva, Karla 1971. "Sorvetes com diferentes produtos de soro de leite bovino : avaliações sensoriais, fisico-quimicas e ultra-estruturais." [s.n.], 2004. http://repositorio.unicamp.br/jspui/handle/REPOSIP/254264.
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Orientador: Helena Maria Andre Bolini CardelloDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: O soro de leite bovino é um subproduto da manufatura de queijo ou caseína caracterizado por sua funcionalidade e valor biológico. O soro ácido, obtido da coagulação ácida do leite, apesar do seu valor funcional ainda é considerado um rejeito industrial. Neste contexto, foi proposta a adição de produto do soro ácido de leite (SAP), em cinco diferentes níveis de substituição do leite em pó, na formulação de sorvete. A avaliação do efeito provocado, pela introdução do SAP no sorvete, foi feita por teste sensorial. Considerando ainda os fabricantes de sorvete que, reconhecendo a importância funcional e nutricional dos produtos de soro de leite, gostariam de aumentar os níveis de substituição por estes produtos em suas formulações, efetuou-se aplicação de leite em pó desnatado e diferentes substituintes deste (SAP, soro desmineralizado e concentrado protéico de soro 35%), comparando-se os resultados. A primeira etapa do trabalho identificou uma boa aceitação dos provadores para o produto contendo 30% de SAP, sendo este nível selecionado para continuidade do trabalho. Na segunda etapa as misturas foram caracterizadas (proteína, gordura, minerais, açúcar, sólidos totais, pH, acidez titulável, viscosidade, temperatura de congelamento e frações protéicas) e os produtos aerados e congelados submetidos a avaliações físicas (potencial de aeração, firmeza e resistência ao derretimento), aspectos ultra-estruturais e testes sensoriais. Os resultados demonstraram que a introdução do SAP aumentou a viscosidade da mistura, manteve o potencial de aeração, estabilizou a firmeza e melhorou a estrutura microscópica do sorvete comparativamente com a formulação padrão (sem substituição do leite). Houve boa aceitação dos provadores para as formulações com substituição do leite desnatado por 30% de SAP, 100% de desmineralizado e 100% de concentrado protéico de soro
Abstract: Whey protein is a by product of cheese or casein production, which is characterized by a high functionality and biological value. Acid whey protein is obtained by acid coagulation of milk, has been viewed as dairy wastes so represent a critical environmental pollution. In this context, we proposed the acid whey addition in ice cream formulations, as a dry skim milk total or parcial substitute, ascertaining by sensory evaluation the panelists acceptance for five different substitutions levels. Ice cream manufacturers interesting in increasing the percentual of this product in ice cream formulations showed the importance of the comparative application of dry skim milk and others different replacers (acid whey product, demineralized whey and whey protein concentrate) in ice cream formulations. At the first stage of this work a good panellists acceptance for 30% acid whey product content product was obtained then this level was selected to the followed experiments. In the second level mixtures were characterized (protein, fat, minerals, sugar, total solids, pH, titratable acidity, viscosity, freezing temperature and proteins fractions) and whippened and freezing products were submitted to physical evaluations (whipping potential, firmness and melting resistance), structural electron microscopy aspects and sensory evaluations. Results showed that acid whey addition in ice cream formulations increased the viscosity of mix, maintained the whipping ability, stabilized the firmness and improved the microscopic structure, as the standard product comparison (formulation without milk substitutions). There was good sensory panel acceptance for all milk substituted formulations (30% acid whey product, 100% demineralized whey and 100% whey protein concentrate)
Mestrado
Mestre em Alimentos e Nutrição
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FONSECA, ANA C. M. "Processos de obtenção e caracterização físico-química de quitinas e quitosanas extraídas dos rejeitos da indústria pesqueira da região de Cananéia – SP." reponame:Repositório Institucional do IPEN, 2016. http://repositorio.ipen.br:8080/xmlui/handle/123456789/26794.
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A quitina é o principal produto obtido do processamento das cascas de crustáceos. Esse biopolímero e o seu derivado, quitosana, têm despertado grande interesse comercial em virtude das possibilidades de aplicações que possuem. O gerenciamento desses resíduos e dos subprodutos gerados nas etapas no processo de obtenção pode ser considerado um modelo de biorrefinaria. A implementação de plantas para extração de quitina e quitosana é um desafio, uma vez que a demanda produtiva deve ser atendida sem causar danos ao meio ambiente. Uma grande variedade de quitosanas com diferentes propriedades físicoquímicas podem ser obtidas variando-se as condições de reação. Essas propriedades dependem da origem da matéria-prima, do seu grau médio de desacetilação, distribuição média dos grupos acetil ao longo da cadeia principal e da sua massa molecular média. Os fornecedores de quitosana comercial geralmente não mencionam a procedência da matéria-prima e pouca ou nenhuma informação é fornecida acerca do seu processamento. Sendo assim, as características e a reatividade do produto final podem variar gerando resultados não reprodutíveis. No presente estudo, foi utilizada a biomassa oriunda de rejeitos da indústria pesqueira de camarão da região de Cananéia SP. As amostras de - quitina foram obtidas por dois procedimentos diferentes: no primeiro, P1, as cascas de camarão após passar pelo pré-tratamento (lavagem, secagem e moagem) foram desproteinizadas para retirada das proteínas em hidróxido de sódio (NaOH) diluído nas concentrações 2%, 5% e 10% e desmineralizadas em ácido clorídrico (HCl) a 20% (v/v) para retirada dos carbonatos; no segundo procedimento, P2, essas etapas foram invertidas. A biomassa resultante foi desacetilada com hidróxido de sódio concentrado a 30%, 40% e 50% em tempos que variaram de 2 a 6 horas. As principais propriedades físico-químicas das amostras de quitosanas obtidas foram determinadas utilizando a espectroscopia na região do infravermelho com transformada de Fourier (FT-IR) para a determinação do grau médio de acetilação, GA, e a técnica de titulação ácido-base mensurada por condutimetria foi utilizada para comparar os resultados; a viscosimetria capilar para a determinação da massa molar média viscosimétrica, Mv , e a difração de raios X (DRX) para avaliar o grau médio de cristalinidade, X. Além disso, foram empregadas as técnicas de microscopia eletrônica de varredura (MEV) para análises morfológicas dos materiais obtidos e a espectrometria de fluorescência de raios X por dispersão de comprimento de onda (WDXRF) para análise química das quitosanas. O GA e o X das amostras diminuíram à medida em que o tratamento se tornou mais vigoroso, enquanto a Mv aumentou. O procedimento 2 foi o mais viável por eliminar a etapa de despigmentação, pois originou amostras com tonalidade mais clara e fáceis de pulverizar.
Dissertação (Mestrado em Tecnologia Nuclear)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
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Benissad, Farida. "Elaboration de fibres de carbone à partir du mélange méthane-hydrogène." Grenoble INPG, 1986. http://www.theses.fr/1986INPG0121.
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On etudie l'elaboration de fibres de carbone par pyrolyse d'un melange h::(2)-ch::(4) a 950-1150**(o)c en presence de particules de fer deposees sur un support en carbone. Les observations se font par microscopies electroniques a balayage et transmission et par microscopie optique. On determine les conditions operatoires optimales (composition et debit du melange gazeux) et on etudie les mecanismes des etapes sucessives: germination, croissance catalytique et croissance pyrolytique
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Barrios, Silmar Balsamo. "Aplicação de polimerização em miniemulsão em tintas industriais." reponame:Biblioteca Digital de Teses e Dissertações da UFRGS, 2014. http://hdl.handle.net/10183/117657.
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Esta tese de doutorado apresenta a obtenção de resinas acrílicas base-água para uso em tintas anticorrosivas obtidas através de polimerização em miniemulsão de metacrilato de metila (MAM), acrilato de butila (AB) e ácido acrílico (AA) utilizando uma resina hidrocarbônica (RHC) como agente osmótico. A técnica de polimerização em miniemulsão difere da polimerização em emulsão convencional em vários aspectos, principalmente no que se refere ao local de onde ocorre a polimerização. Na polimerização em miniemulsão não há transferência de monômero pelo meio contínuo ao longo da polimerização. As gotas de monômeros (inicialmente formadas) são suficientemente pequenas e estáveis de forma que a nucleação e crescimento da cadeia polimérica ocorrem nas próprias gotas, que agem como “nano-contêineres”. O sistema é obtido por alto cisalhamento e a alta estabilidade das gotas é garantida pela combinação do componente anfifílico (surfactante) e o agente osmótico, que é solúvel e homogeneamente distribuído na fase descontínua. O agente osmótico tem baixíssima solubilidade na fase contínua e, portanto, cria uma pressão osmótica dentro das gotas, anulando a pressão de Laplace e prevenindo o efeito de Ostwald ripening, que é a difusão de massa das gotas menores para as maiores em razão da diferença de pressão. Nesta tese, uma resina hidrocarbônica (RHC) foi utilizada como agente osmótico. RHC é um polímero de baixo custo largamente utilizado em tintas e adesivos base-solvente. A sua utilização em látex pode aumentar a hidrofobicidade do filme e age como agente osmótico na polimerização em miniemulsão, levando a látices com distribuições, tamanhos de partícula e estabilidade similares quando usado n-hexadecano (HD) como agente osmótico. Entretanto, quando RHC é utilizado, menor conversão de monômeros e menor massa molar indicam a ocorrência de reação de transferência de cadeia. Análise de microscopia de força atômica (AFM) do filme do látex com RHC demonstrou uma morfologia lisa, porém com separação de fases. Testes em uma formulação de tinta anticorrosiva mostraram maior desenvolvimento de dureza quando utilizado RHC quando comparado com HD. Comparando com uma resina padrão de mercado tanto RHC quanto HD tiveram aderências similares sobre painel de aço, porém durezas mais altas. Entretanto, brilho mais baixo foi obtido quando usado RHC. A xix visualização do filme através de AFM mostrou separação de fases quando RHC é utilizada, o que pode explicar o menor brilho alcançado. As tintas anticorrosivas preparadas foram submetidas a ensaio de espectroscopia de impedância eletroquímica (EIS). Resultados similares foram obtidos comparando a resina de mercado com os látices com RHC e HD em concentrações padrão de surfactante. Quando utilizado um látex com RHC com menor concentração de surfactante melhores resultados foram obtidos.Waterborne acrylic resins suitable for anticorrosive coatings were obtained by miniemulsion polymerization of methyl methacrylate (MAM), butyl acrylate (AB) and acrylic acid (AA) using a hydrocarbon resin (RHC) as osmotic agent. Miniemulsion polymerization is powerful technique that allows the incorporation of preformed solventborne polymers in a waterbased matrix. It consists of small, stable, and narrowly distributed droplets in a continuous phase, which acts as “nanocontainers” were the polymerization takes place. The system is obtained by high shear and the high stability of the droplets is ensured by the combination of the amphiphilic component, the surfactant, and the osmotic agent, which is soluble and homogeneously distributed in the droplet phase. The osmotic agent has a lower solubility in the continuous phase and therefore builds up an osmotic pressure in the droplets counteracting the Laplace pressure, preventing the so called Ostwald ripening. RHC is a cheap polymer widely used for solventborne coatings and pressure sensitive adhesives. Using the as osmotic agent in the miniemulsion polymerization can lead to a higher hydrophobicity for the acrylic latex film, leading to latexes with particle sizes, size distributions and stability comparable to those obtained using n-hexadecane (HD) as osmotic agent. However, when using RHC, the monomer conversion and molecular weight were lower indicating the occurrence of a chain transfer reaction. Atomic force microscopy (AFM) analysis demonstrated that a smooth film surface with phase separated morphology was formed when using RHC. Tests in an anticorrosive paint formulation showed fast hardness development for RHC comparing to HD. Comparing with a market resin reference both RHC and HD had equivalent adhesion results on steel panels but higher final hardness. However lower gloss were found when using RHC which supports the AFM phase separation observations. The anticorrosive paints formulations were submitted to electrochemical impedance spectroscopy (EIS) analysis. Similar results were achieved for the market resin compared to RHC and HD with standard surfactant levels. When using RHC latex with less surfactant concentration better results in anticorrosive performance were achieved.
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Santander, Morales Carolina Beatriz. "Estudio Experimental de Corrosión en Metales de Uso Industrial por Desulfovibrio desulfuricans." Tesis, Universidad de Chile, 2008. http://repositorio.uchile.cl/handle/2250/103133.
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El desarrollo alcanzado por la humanidad desde la Revolución Industrial hasta hoy exige
a la industria mundial, procesos que sean eficientes en el uso de materias primas y metales que
sean confiables de acuerdo a los requerimientos de cada aplicación industrial. Es aquí, entonces,
en donde el conocimiento sobre la corrosión y particularmente la corrosión mediada por
microorganismos juega un papel fundamental para poder generar alternativas de mitigación y
prevención de la corrosión, que permitan aminorar las millonarias pérdidas económicas que año a
año aquejan a las industrias.
En el presente trabajo se realiza un estudio experimental de corrosión en diversos tipos de
acero, los cuales son incubados a tres tiempos distintos en un reactor anaeróbico con un cultivo
de bacterias sulfato reductoras autotróficas Desulfovibrio desulfuricans, siendo el objetivo del
trabajo poder simular una corrosión mediada por microorganismos, junto con cuantificarla
indirectamente a través del área cubierta por bacterias en la superficie de las muestras. Posterior a
la incubación, las placas metálicas son analizadas mediante Microscopía Electrónica de Barrido,
para poder visualizar las bacterias y el daño sobre la superficie. El área cubierta por bacterias en
cada una de las muestras fue calculada con un programa para contar pixeles, el cual discrimina a
partir de las diferencias de color de las áreas seleccionadas entregando un porcentaje de área
cubierta con respecto al área total.
Los principales resultados de este trabajo fueron los siguientes: se pudo simular con éxito
una corrosión mediada por bacterias ya que fue posible observar daño en la superficie de los
metales a partir del menor tiempo de incubación. Por otra parte, se observó una heterogeneidad
de bacterias sobre la superficie, luego, el cultivo empleado no corresponde solamente a
Desulfovibrio desulfuricans. Los aceros inoxidables AISI 316L, AISI 420 y el fierro fundido
ASTM A536, fueron las muestras con menor superficie cubierta por bacterias, mientras que el
acero al carbón AISI 1020 y el acero estructural AISI A36 fueron las muestras con mayor
cantidad de bacterias depositadas en su superficie.
Se ajustaron cinéticas de poblamiento de superficie por bacterias para cada una de las
muestras, excepto para el acero inoxidable AISI 316L por tener un extraño comportamiento de
cubrimiento en el tiempo. Se obtuvieron cinéticas de primer orden para los siguientes metales:
Fierro fundido (vel. inicial de poblamiento de superficie observada, -0,039 [d-1]), SAE 4340 (vel.inicial de poblamiento de superficie observada, -0,043 [d-1]); y cinéticas de segundo orden para
los siguientes metales: AISI 420 (vel. inicial de poblamiento de superficie observada, -3×10-6
[mm-2d-1]), AISI 1020 (vel. inicial de poblamiento de superficie observada, -8×10-6 [mm-2d-1]) y
A36 (vel. inicial de poblamiento de superficie observada, -8×10-6[mm-2d-1]).
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Graça, Leonardo Martins. "Implicações das propriedades mineralógicas e microestruturais do minério de ferro no processo industrial de pelotização." reponame:Repositório Institucional da UFOP, 2015. http://www.repositorio.ufop.br/handle/123456789/5248.
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Programa de Pós-Graduação em Evolução Crustal e Recursos Naturais. Departamento de Geologia. Escola de Minas, Universidade Federal de Ouro Preto.Submitted by Oliveira Flávia (flavia@sisbin.ufop.br) on 2015-04-30T17:32:20Z No. of bitstreams: 2 license_rdf: 22190 bytes, checksum: 19e8a2b57ef43c09f4d7071d2153c97d (MD5) TESE_ImplicaçõesPropriedadesMineralógicas.pdf: 11857797 bytes, checksum: a797d14c98ee60a6f203b9234090cfe1 (MD5)
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O presente trabalho compreende os resultados de estudos específicos desenvolvidos sobre as implicações mineralógicas e microestruturais de minério de ferro nos processos unitários de cominuição, filtragem e queima em forno, como fatores de avaliação e controle da qualidade final do produto de pelotização, tendo em vista a otimização da sua produção industrial. Foram caracterizadas amostras das minas de Itabira, Brucutu, Alegria e Fábrica Nova, todas localizadas no Quadrilátero Ferrífero, as quais, são utilizadas no complexo pelotizador de Tubarão localizado em Vitória, no Espírito Santo. As amostras referem-se a diferentes produtos de flotação, de separação magnética e de peneiramento a seco. Características físicas como distribuição granulométrica, densidade, área de superfície específica, além de características mineralógicas como fases minerais, morfologia tridimensional de grão e microestruturas foram determinadas. As características físicas foram determinadas conforme procedimentos utilizados no complexo pelotizador de Tubarão e as características mineralógicas foram determinadas a partir de estereoscópio, microscópio óptico e microscópio eletrônico com o módulo electron backscater difraction. As relações entre as características mineralógicas e os resultados dos testes de moagem permitiram definir os tipos de produto e propor uma relação entre o índice de moabilidade e os tipos morfológicos caracterizados. Posteriormente, foi planejada e implementada uma matriz de experimento a partir de misturas dos produtos para testes nos processos estudados. Também foi caracterizada a mistura desses concentrados que alimentam a pelotização. Em ambos os processos unitários estudados, os testes aconteceram em escala de bancada e piloto. Nos testes de moagem e filtragem as variações mineralógicas causaram impacto, respectivamente, no índice de moabilidade e na umidade da torta retida. Os resultados dos testes de filtragem indicam uma relação entre os valores de umidade e produtividade com os valores de hematita martítica. Já para o teste de compressão das pelotas queimadas, a estatística dos resultados indicaram diferença de compressão entre misturas com diferentes quantidades de goethita. _________________________________________________________________________
ABSTRACT: This work includes the results of specific studies on the mineralogical and microstructural implications of iron ore in the processes of comminution, filtering and induration process oven as evaluation factors, and control the quality of the final pellet product, with a view to optimizing industrial process. Iron ore samples of the mine Itabira, Brucutu, Alegria e Fábrica Nova were characterized. The samples are different products of flotation, magnetic separation and screening. Grain size distribution, density, specific surface area, mineral phase, morphology and microstructure were determined. The physical characteristics were determined according to industrial procedures of the Tubarão pelletinzing plant in Vitória, Espírito Santo. The mineralogical characteristics were determined with stereoscope, optical microscope and electron backscatter diffraction. The relationship between mineralogy and grinding test were then established after the iron ore characterization. Afterwards, we carried out an experiment using blends of the iron ore plant products to test in the pelletizing process. The blends that feed the pelletinzing plants were also tested with the same purpose. Both tests were accomplished in bench as well as in pilot scale. It was also characterized blends these concentrates that feed pelletinzing. The grinding and filtration tests showed that the mineralogical types exert a strong influence on the grinding index and moisture of the filter cake. A direct relationship arouse from the grinding process in which the morphological types are closely related to the grinding index. Likewise the results of the filtration tests pointed up that the martitic types affect considerably the moisture and therefore the performance of the filtration process. Finally, the compress tests of the fired pellets demonstrate that the proportion of goethite phases in the iron ores affects the cold compression strength results of the pellets.
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López, Córdova Pastor. "Química e industria de la curcumina." Bachelor's thesis, Universidad Nacional Mayor de San Marcos, 2017. https://hdl.handle.net/20.500.12672/7516.
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Resume 30 años de experiencia en la industria de los colorantes naturales en la especialidad de aislamiento, purificación y concentración de los principios activos siempre considerando el margen de utilidad para las empresas. Se describe una detallada explicación sobre la industrialización de la Cúrcuma longa (Palillo), los pasos a seguir para la obtención de los cristales de curcumina, oleorresina desodorizada y preparaciones solubles, dispersiones en agua y aceite para ser utilizados como aditivos alimentarios e insumos cosméticos y farmacéuticos, con el objetivo de potenciar el color amarillo de los preparados en estos campos. Incluye los resultados de pruebas piloto para la obtención de los curcuminoides totales, sin llegar a cristalizar la curcumina, para lograr un mejor costo y mayor recuperación del color. Asimismo, debido a la gran investigación que ha suscitado la curcumina por sus propiedades bioquímicas y benéficas para la salud, como ser anti radical libre y en muchos casos como una alternativa natural al colorante artificial tartrazina o amarillo N°5, se considera pertinente mencionar las referencias bibliográficas que sustentan la importancia de la Cúrcuma longa en el ámbito medicinal.Trabajo de suficiencia profesional
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Khadhraoui, Boutheina. "éco-extraction assistée par ultrasons des plantes médicinales : mécanisme(s), intensification et industrialisation ULTRASOUND TECHNOLOGY FOR FOOD PROCESSING, PRESERVATION AND EXTRACTION Histo-cytochemistry and scanning electron microscopy for studying spatial and temporal extraction of metabolites induced by ultrasound. Towards chain detexturation mechanism Microscopic imaging as a tool to target spatial and temporal extraction of bioactive compounds through ultrasound intensificationUltrason. Review of Alternative Solvents for Green Extraction of Food and Natural Green solvents for analytical chemistry." Thesis, Avignon, 2019. http://www.theses.fr/2019AVIG0715.
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Le retour à la naturalité a favorisé le développement des compléments alimentaires à base de ressources végétales qui apparaissent comme un réservoir quasi-infini de nutriments et de substances naturelles bioactives. Ceci fait de l’extraction solide/liquide une étape incontournable au sein des industries intéressées par ce type de molécules. Avec les préoccupations environnementale set sociétales, il est devenu nécessaire d’inventer et développer de nouveaux procédés qui répondent aux six principes de l’éco-extraction. Cette démarche a totalement inspiré cette thèse qui a pour principal objectif le développement d’une technique d’éco-extraction assistée par ultrasons en substitution de la technique conventionnelle. Ce travail a permis de montrer qu’il était possible d’intensifier l’extraction de composés d’intérêt en utilisant les ultrasons avec une meilleure sélectivité et de meilleurs rendements d’extraction. Une attention particulière a été accordée à la compréhension des mécanismes d’action des ultrasons via une étude macroscopique et microscopique approfondie des structures végétales. Cette investigation a prouvé que les ultrasons agissent différemment en fonction des structures végétales et de leurs propriétés morphologiques et chimiques qui leur confèrent un degré de résistance plus ou moins important face à l’action des ultrasons. Partant de ces résultats, l’étude macroscopique et microscopique a été définie comme un outil de décision pour une extraction ciblée. Cette variabilité a été aussi constatée à l’échelle industrielle prouvant davantage l’importance de l’analyse microscopique. Enfin, le procédé d’extraction par ultrasons a été adopté à l’échelle industrielle pour ses performances d’extraction et pour son empreinte environnementale significativement réduite par rapport au procédé CV. Ce travail a également conduit à des travaux complémentaires sur l’étude du potentiel de solubilisation des produits naturels en vue d’une utilisation pour l’extraction de composés végétaux difficiles à solubiliser dans l’eau. Des résultats prometteurs ont été obtenus en termes de pouvoirs de solubilisation et d’extraction notamment à partir de la matière végétale broyée. Les résultats de cette dernière partie soulèvent cependant des questions qui pourraient faire l’objet de futures recherches et de perspectives pour ce travail qui sont principalement liés à l’étude des problèmes liés au changement du solvant et au prétraitement de la matière première et de la faisabilité industrielle de ce nouveau procédéWith recent trends in the increasing interest to environmental, economic and safety considerations,extraction techniques have largely focused on finding solutions with sustainable and green values toimplement in food processing, cosmetic and pharmaceutical industries. In this context, new “green”extraction techniques were developed such as Ultrasound-Assisted Extraction (UAE). The mainobjective of this thesis is industrial implementation of this new process in substitution to theconventional (CV) process. It has been shown in this work that the extraction of compounds ofinterest from rosemary and other plant matrices could be intensified using ultrasound, and thatdifferent performance gain could be achieved according to the plant matrix structural properties.Indeed, macroscopic and microscopic investigation of untreated and treated raw materials provedthat US act through different mechanisms and its resulting impacts can be extremely limited by plantstructural morphological and chemical properties, especially those of the specialized structures.Significant variability in performance gain was also observed at the industrial scale. Overall, USappears as a promising technique with a significant performance gain in terms of extraction yield andselectivity. Moreover, this process presents low environmental footprint compared to the CV one.Finally, it has been shown that natural products, such as honey and fruit juices, can be used toimprove solubilization and extraction of molecules that are poorly soluble in water. Encouragingresults were obtained in terms of solubilization and extraction abilities, especially from ground rawmaterials. However, these results raise questions related to the feasibility of industrialimplementation of this new process
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Nhanga, José Nascimento. "Sensores de oxigénio para aplicação industrial." Master's thesis, Universidade de Aveiro, 2017. http://hdl.handle.net/10773/21876.
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Mestrado em Engenharia de MateriaisO trabalho apresentado nesta dissertação consiste no estudo de uma família de eletrólitos sólidos cerâmicos à base de óxido de zircónio dopado com óxido de magnésio, normalmente identificados como Mg-PSZ (zircónia parcialmente estabilizada com magnésia), usados nomeadamente no fabrico de sensores de oxigénio para metais fundidos. Preparou-se um conjunto de eletrólitos por processamento mecânico (moagem) e térmico (sinterização), variando a composição em magnésia e a velocidade de arrefecimento desde a temperatura de sinterização. Estes dois parâmetros são essenciais em termos de composição em fases e microestrutura das Mg-PSZ, determinando o comportamento destes materiais. A caracterização estrutural e microestrutural foi feita por meio da difração de raios-X (amostras densas e pós) e microscopia eletrónica de varrimento, tendo em vista a determinação das percentagens relativas das fases cúbica, tetragonal e monoclínica, bem como da sua localização em termos microestruturais. O comportamento térmico foi estudado por dilatometria. As propriedades elétricas foram analisadas por espetroscopia de impedância em ar até cerca de 800 °C. De uma forma geral os resultados obtidos a partir de diversas concentrações de dopante (6-8 mol% MgO), diferentes velocidades de arrefecimento (1, 2 e 4 ºC.min-1) e igual condição de patamar de sinterização (1700 °C, 3 horas), mostraram um aumento da condutividade para as amostras com predomínio das fases estáveis de alta temperatura (tetragonal e cúbica). De todas as composições estudadas a 8 Mg-PSZ com elevada velocidade de arrefecimento é a que apresenta maior condutividade iónica. Do mesmo modo, o melhor comportamento térmico parece ser conseguido em amostras com a fase monoclínica finamente dispersa no seio da fase cúbica, envolvendo mais baixas concentrações de dopante e/ou menor velocidade de arrefecimento. Atendendo à importância destes dois aspetos, a solução ideal deve corresponder a um compromisso entre estas duas situações. Os resultados obtidos abrem caminho para estudos mais profundos visando aplicações em sensores para metal fundido.
The work presented in this dissertation is a study of a family of solid ceramic electrolytes based on zirconium oxide doped with magnesium oxide, usually identified as Mg-PSZ (zirconia partially stabilized with magnesia), used in the manufacture of oxygen sensors for molten metals. A set of electrolytes was prepared by mechanical (milling) and thermal (sintering) processing, varying the composition in magnesia and the cooling rate from the sintering temperature. These two parameters are essential in terms of phase composition and microstructure of Mg-PSZ, determining the behaviour of these materials. The structural and microstructural characterization was done by means of X-ray diffraction (dense samples and powders) and scanning electron microscopy, in order to determine the relative percentages of the cubic, tetragonal and monoclinic phases, as well as their location in terms microstructures. The thermal behaviour was studied by dilatometry. The electrical properties were analysed by impedance spectroscopy in air up to about 800 ° C. In general, the results obtained from various concentrations of dopant (6-8 mol% MgO), different cooling rates (1, 2 and 4 °Cmin-1) and the same sintering step condition (1700 °C, 3 hours) showed an increased conductivity for samples with predominance of high temperature stable phases (tetragonal and cubic). 8 Mg-PSZ with high cooling rate is the one with the highest ionic conductivity amongst all the compositions studied. Likewise, the best thermal behaviour appears to be achieved in samples with the monoclinic phase finely dispersed within the cubic phase, involving lower dopant concentrations and/or lower cooling rates. Given the importance of these two aspects, the ideal solution must correspond to a compromise between these two situations. The obtained results open the way for deeper studies aiming at applications in sensors for molten metals.
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Guo, Shuo. "Evaluation of deformed MnS in different industrial steels by using electrolytic extraction." Thesis, KTH, Materialvetenskap, 2017. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-217880.
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The inclusions have a different chemical composition and give the steel different mechanical properties. These inclusions affect several properties of steel. In order to understand how the inclusions will affect the steel properties, the electrolytic extraction of 3D investigate method is applied on the steel grade of 42CrMo4. Then follow with Scanning Electron Microscope (SEM) observation. Steel samples from both ingot and rolling with and without heat treatment are observed and compared with different ratios. The result shown that, heat treatment can be applied for removing carbides successfully. And most inclusions are belonging to Type RS which is rod like MnS. The percentage of broken particles can be up to 80%, which means that the reason for the inclusions broken should be find. And heat treatment can affect the characteristics of elongated MnS.
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Rouland, Solene. "Etude expérimentale des cinétiques de diffusion et de la ségrégation induite sous irradiation d'alliages modèles et industriel austénitiques." Thesis, Normandie, 2020. http://www.theses.fr/2020NORMR050.
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L’implication de la ségrégation induite par l’irradiation (SIR) dans la majorité des mécanismes de dégradation des composants du cœur des réacteurs nucléaires en aciers inoxydables austénitiques est avérée. Aux températures de fonctionnement des réacteurs actuels et possibles prototypes du futur, les éléments chimiques des pièces métalliques des structures internes se redistribuent de manière hétérogène en ségrégeant sur les défauts préexistants et nouvellement créés par l’irradiation. L’intensité des enrichissements ou des appauvrissements locaux dépendent, entre autres, de la nature de l'élément et du défaut concerné. Si les différents mécanismes de ségrégation sont aujourd’hui bien identifiés, leur cinétique et leur degré d’implication respectifs sont encore peu renseignés. En effet, les modèles théoriques actuels de la SIR souffrent d'un manque de données expérimentales. Ces deux aspects sont le moteur de cette étude. Dans un premier temps, les cinétiques d'interdiffusion après vieillissement thermique et sous irradiation ont été déterminées dans des alliages modèles du système Fe-Ni-Cr. L'effet de l'irradiation sur la diffusion a été étudié à 440°C. A cette température les coefficients de diffusion sont faibles et les méthodes classiques d'étude de la diffusion ne permettent pas d'y accéder dans un délai raisonnable. La mise en œuvre expérimentale de la méthode des multicouches à période nanométrique dans des alliages binaires et ternaires a montré, dans ce cas, des résultats encourageants. Toutefois, des divergences entre les résultats expérimentaux et les prévisions théoriques ont révélé la nécessité d'optimiser ces deux approches. Dans le cadre de cette étude, des recommandations ont été formulées pour tenir compte de l’impact de la microstructure et du choix des conditions de vieillissement sur les cinétiques effectives mesurées. Les expériences réalisées sur des alliages modèles offrent l’intérêt de pouvoir être directement confrontées à la simulation. Néanmoins, les aciers de l’industrie nucléaire contiennent une grande variété d'éléments d'alliage minoritaires et d'impuretés qui jouent un rôle clé sur le comportement des éléments impliqués dans la SIR. Ainsi, dans un second temps, une étude de la SIR sur différents défauts intragranulaires d'un acier inoxydable austénitique optimisé, un 316L(N) a été réalisée. Pour cela, des techniques couplées et corrélées à l'échelle nanométrique (Sonde Atomique Tomgraphique et Miscroscopie Electronique en Transmission) ont été mises en place. La complémentarité des techniques a rendu possible l'association des enrichissements locaux observés à la cristallographie des défauts concernés. Des tendances singulières de SIR ont été observées selon l'élément et la nature du défaut impliqués. Une teneur plus élevée en azote et en niobium dans la composition nominale de l'acier a entrainé la précipitation de phase Z primaire. La stabilité de cette phase sous irradiation dans les aciers inoxydables austénitiques a pour la première fois pu être étudiéeRadiation induced segregation (RIS) is a process identified to be involved in most of the degradation mechanisms of austenitic stainless steels core components of nuclear reactors. During irradiation within the operating temperature range of present and possible prototypes of future reactors, chemical elements of reactor internal metallic components redistribute heterogeneously and segregate on the pre-existent and newly created defects. Local enrichments or depletions levels depend, inter alia, on the element and nature of the defect affected. While mechanisms involved in RIS have already been identified, their kinetics and mutual weigh are still poorly known. Indeed, current theorical models of RIS suffer from a lack of experimental data. These two aspects motivated this study. First, by the determination of interdiffusion kinetics after thermal ageing and under irradiation on model alloys in the Fe-Ni-Cr system. Irradiation effect on diffusion have been studied at 440°C. At this temperature, conventional methods to study diffusion fail to give access to such slow kinetics under reasonable time. Experimental implementation of the nanolayers method on binary and ternary alloys gave, in this case, encouraging results. However, discrepancies between experiments and predictions revealed the need of optimizations on both sides. In the framework of this study, recommendations have been established to account for the effect of the microstructure and the selected ageing conditions on measured effective kinetics. Experiments on model alloys have the great interest to be directly confronted to simulation. Nevertheless, nuclear steels contain a large variety of minor alloying elements and impurities which have shown to play a key role on RIS behaviour. Thus, in a second part, RIS study on various bulk defects of an optimized nuclear austenitic stainless steel, a 316L(N) has been performed. Consequently, nanoscale coupled and correlated techniques (Atom Probe Tomography and Transmission Eelectron Microscopy) have been implemented. Techniques complementarity offered the possibility to associate enrichments to defect crystallography and revealed singular tendencies of RIS depending on the element and the defect involved. Furthermore, a higher nitrogen and niobium content in the steel nominal composition formed primary Z-phase, its stability under irradiation had also been for the first time studied in austenitic stainless steels
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Le, Bris Didier. "Élaboration d'un module de focalisation automatique pour l'intégration d'un capteur de vision en microscopie epifluorescente dans un contexte industriel." Nancy 1, 1991. http://www.theses.fr/1991NAN10018.
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L'émergence en biologie de disciplines technologiques telles que la visionique s'accompagne couramment d'un développement important des techniques d'analyse d'image au détriment de l'aspect réalisationnel. Ces travaux ont pour objectif de contribuer à l'élaboration du concept d'automate vers lequel devrait tendre tout système de routine d'analyse d'image en biologie par la réalisation d'une carte de focalisation automatique sur ibm pc et de la motorisation d'un microscope. Cette réalisation est également le point de départ d'une approche plus méthodologique sur ce genre de systèmes
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Bonnail, Nicolas. "Analyse des données, modélisation et commande pour la microscopie en champ proche utilisant des actionneurs piézoélectriques." Aix-Marseille 2, 2001. http://www.theses.fr/2001AIX22059.
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Meyendorf, N., M. Oppermann, P. Krueger, M. Roellig, and K. J. Wolter. "NDE applications in microelectronic industries." SPIE, 2016. https://tud.qucosa.de/id/qucosa%3A35100.
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New concepts in assembly technology boost our daily life in an unknown way. High end semiconductor industry today deals with functional structures down to a few nanometers. ITRS roadmap predicts an ongoing decrease of the “DRAM half pitch” over the next decade. Packaging of course is not intended to realize pitches at the nanometer scale, but has to face the challenges of integrating such semiconductor devices with smallest pitch and high pin counts into systems. Advanced techniques of nondestructive evaluation (NDE) with resolutions in volume better than 1 micrometer vixen size are urgently needed for the safety and reliability of electronic systems, especially those that are used in long living applications. The development speed of integrated circuits is still very high and is not expected to decrease in the next future. The integration density of microelectronic devices is increasing, the dimensions become smaller and the number of I/O's is getting higher. The development of new types of packages must be done with respect to reliability issues. Potential damage sources must be identified and finally avoided in the new packages.
In power electronics production the condition monitoring receives a lot of interest to avoid electrical shortcuts, dead solder joints and interface crac king. It is also desired to detect and characterize very small defects like transportation phenomenon or Kirkendall voids. For this purpose, imaging technologies with resolutions in the sub-micron range are required.
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FERREIRA, MATHEUS C. "Obtenção de fritas vitroceramicas a partir de resíduos sólidos industriais." reponame:Repositório Institucional do IPEN, 2006. http://repositorio.ipen.br:8080/xmlui/handle/123456789/11469.
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Dissertacao (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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Blythe, Kevin S. "A methodology of aggregating discrete microscopic traffic data for macroscopic model calibration and nonequilibrium visual detection purposes." Ohio : Ohio University, 1991. http://www.ohiolink.edu/etd/view.cgi?ohiou1183653868.
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Ferreira, Matheus Chianca. "Obtenção de fritas vitrocerâmicas a partir de resíduos sólidos industriais." Universidade de São Paulo, 2006. http://www.teses.usp.br/teses/disponiveis/85/85134/tde-14052012-111305/.
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O resíduo estudado neste trabalho é originado do processo de obtenção de alumínio metálico, de grande interesse no Brasil pelo fato do país ser detentor de algumas das maiores reservas do mineral bauxita no mundo, utilizado como fonte de alumínio. Tendo como estratégia a geração de resíduo zero, colaborando para as tecnologias ambientalmente amigáveis, este trabalho estuda a incorporação de um resíduo resultante da recuperação de alumínio presente na escória gerada durante o processo de produção primária do alumínio metálico, por plasma térmico. Utilizando-se o diagrama de equilíbrio de fases do sistema Al2O3-CaO-SiO2, fez-se a adequação das composições visando a incorporação de resíduo no produto cerâmico sem alterar as características de processamento do material. A obtenção de vidros e de fritas vitrocerâmicas com o resíduo borra branca foi realizada fazendo-se a fusão das composições calculadas e, para os vitrocerâmicos, tratamento térmico posterior de devitrificação. Os produtos obtidos foram caracterizados utilizando-se técnicas de análise tais como difração de raios X (DRX), microscopia eletrônica de varredura (MEV) e espectroscopia do infravermelho (FTIR). Foi possível obter material vitrocerâmico com até 30% de resíduo de alumínio, após a fusão a 1300°C e devitrificação a 900°C. Em adição, o resíduo demonstrou ser um promissor material auxiliar na formação de fases cristalinas em baixos tempos de tratamento térmico.This work studies the residue obtained from the process of aluminum metal extraction activities, a great interest process, because of Brazil own some of the biggest bauxite mineral reserves in all the world. As a useful choice for no residue generation, and a support for environmentally friendly technologies, this work studies the white dross residue (WDR), from the process of aluminum metal reduction by thermal plasma. The phase equilibrium diagram of Al2O3-Ca O-SiO2 system was used to calculate the compositions. The WDR were incorporated in a ceramic product without modifying its principal characteristics. The fusion and devitrification treatments were studied. XRD (X-ray diffractometry), SEM (scanning electron microscopy) and FTIR (transformed Fourier infrared) were used to investigate the glass and glassceramic samples. These techniques showed that is possible to get glassceramic with up to 30 mass% of WDR after molten at 1300 deg C and annealed at 900 deg C. In addition, the WDR showed to be a promising material in attainment of crystalline phases in less times of heat treatment for annealing.
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González, Martínez Juan Francisco. "Explorando los límites de la microscopía de fuerzas : ruido térmico y ruido e la interacción punta-muestra." Doctoral thesis, Universidad de Murcia, 2015. http://hdl.handle.net/10803/334415.
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En esta tesis se analizan y discuten los aspectos que determinan los límites de la microscopía de fuerzas (SFM). Para tal fin, se han expuesto un conjunto de modelos de diversa complejidad (oscilador armónico, modelo continuo). Además, se ha descrito con detalle el origen y significado físico de las señales electrónicas en las que convertimos el desplazamiento físico (amplitud, fase, frecuencia y fuerza normal) y el sistema electrónico encargado de su adquisición y procesado (Capítulos 1 y 2). El comportamiento dinámico del fleje no puede limitarse a un oscilador armónico ya que constituye un sistema más complejo: es necesario considerar el fleje como un conjunto de osciladores, excitados en mayor o menor medida, donde cada uno de ellos, se ve afectado por disipaciones (internas, despreciables en este contexto) y externas (de tipo hidrodinámico) que, a su vez, tienen una dependencia en función de la distancia punta-muestra. Desde el punto de vista hidrodinámico, se analiza dicha disipación a través del factor de calidad del oscilador (Capítulo 6). Dicho análisis parte de la descomposición del sistema físico (el fleje) en sus diversas partes (el fleje, propiamente dicho, la punta y el vértice de la punta) y permite la optimización de la geometría del sistema fleje-punta para conseguir la máxima sensibilidad posible. El ruido térmico es uno de los límites fundamentales en las aplicaciones desarrolladas en esta tesis y es pues, el eje central que ha permitido su confección. Las fluctuaciones térmicas afectan a la posición del fleje y limitan la determinación de la frecuencia de resonancia del sistema. Se desarrolla una relación precisa (Capítulo 3) para el ruido térmico en frecuencia en función del ancho de banda y de la amplitud de oscilación del fleje, que rectifica la relación clásica empleada en la literatura. La diferente composición química de los compuestos presentes en una superficie se refleja en la existencia de una contribución adicional al ruido térmico, y, por tanto, a los límites de las medidas en microscopía de fuerzas. Se han realizado experimentos que evidencian la presencia de este ruido y explican cómo es posible extraer información del mismo (Capítulo 5). Además, justificamos su existencia a raíz de las diferentes interacciones hidrófobica e hidrofílica presentes en la superficie. La variación de la amplitud de oscilación está relacionada con la disipación del sistema punta-muestra. Además, sólo para pequeñas amplitudes el sistema dinámico puede considerarse armónico. Es necesario desarrollar un método de calibración de la amplitud de oscilación que permita conocer con precisión cuánto varía la posición del fleje. Esto es posible mediante una calibración correcta de la señal de la amplitud de oscilación y para tal fin, se proponen dos métodos (Capítulo 4): uno de ellos está basado en el cálculo de la desviación cuadrática media de la señal de salida de la electrónica; el segundo método se basa en el análisis del espectro de la señal correspondiente y en el cálculo del factor de calidad, la frecuencia de resonancia y la intensidad de la señal. Ambos métodos son también aplicables a la calibración de la fuerza normal. En este caso la importancia radica en que es posible calibrar la sensibilidad en fuerza normal sin que la punta del fleje sufra daños. Finalmente, en los experimentos expuestos se ha hecho uso de un sistema de reposicionamiento preciso (Capítulo 7). Este sistema, permite la manipulación ex-situ de las muestras y el reposicionamiento preciso en el microscopio de fuerzas sin ayuda de un microscopio óptico o marcas de posición.This thesis analyses and describes the fundamental and experimental limits of Scanning Force Microscopy. To this end, a set of models for the dynamical behaviour of the system are proposed. In addition, the origin and physical meaning of the electronic signals generated by the motion of the cantilever (amplitude, phase, frequency and normal force) and the electronics involved in its acquisition and processing have been described in detail (Chapters 1 and 2). The dynamic behaviour of the cantilever cannot be described correctly by the harmonic oscillator. It is necessary to consider the cantilever as a set of oscillators, excited in different modes, each of them being affected by dissipations (internal, negligible in this context) and external (hydrodynamic) that, in turn, depends on the tip-sample distance. From the hydrodynamic point of view, this dissipation is analysed through the quality factor of the oscillator (Chapter 6). This analysis is based on the decomposition of the system (the cantilever) in its components (the lever, the tip and the apex of the tip) and allows the optimization of the geometry of the system (cantilever) in order to obtain the maximum sensitivity possible. The thermal noise is one of the fundamental limits of Scanning Force Microscopy. Temperature fluctuations affect the position of the cantilever and limit the resolution of the frequency measurements. A precise relationship (Chapter 3) for thermal frequency noise as a function of the bandwidth and amplitude of oscillation of the cantilever has been developed. This result rectifies the classic relationship from the scientific literature. We have found that the chemical composition of a surface induces an additional contribution to noise, and therefore to the limits in SFM. To show and analyse in more detail the presence of this noise and the information it contains, various experiments have been developed (Chapter 5). Furthermore, we justify the nature of this noise from the different hydrophobic and hydrophilic interactions on the surface. The fluctuations in the amplitude of oscillation is related to the dissipation of the tip-sample system. Only for small amplitudes, the dynamic system can be considered harmonic. It is important to develop a calibration method for the oscillation amplitude. For this purpose, two methods (Chapter 4) are proposed: one based on the mean square deviation calculus of the output signal of the electronics; the second method, based on spectral analysis and the calculation of the quality factor, resonant frequency and signal strength. Both methods are also applicable to the calibration of the normal force. In this case, the importance lies in the calibration of the sensitivity of normal force without tip damage. Finally, for some of the experiments reported along this thesis, a precise repositioning system (Chapter 7) has been developed. This system allows the ex-situ sample handling and the precise repositioning of the sample in the SFM without the aid of an optical microscope or position marks.
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Amboni, Renata Dias de Mello Castanho. "Utilização de metodos avançados de microscopia e analise sensorial para detecção de fraudes em cafe torrado e moido." reponame:Repositório Institucional da UFSC, 1997. http://repositorio.ufsc.br/xmlui/handle/123456789/77313.
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Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro de Ciencias AgrariasMade available in DSpace on 2012-10-17T02:55:08Z (GMT). No. of bitstreams: 0
Atualmente a detecção de fraudes em café em pó é realizada por microscopia ótica. Assim, foram propostos métodos mais rápidos e eficientes de microscopia e análise sensorial. Para as análises microscópicas, comparou-se café puro com café fraudado com 2,5, 5 e 10% de centeio, cevada, milho e trigo. Para análise sensorial, comparou-se o café puro com café fraudado com 20,30 e 40% dos mesmos cereais. O painel sensorial formado por seis julgadores foi selecionado após intensivo treinamento. Em todas as análises de microscopia de fluorescência e eletrônica de varredura (SEM) de café fraudado, detectou-se, imediatamente, a presença de amido, o que não ocorreu na microscopia ótica. Entretanto, a detecção de fraudes por SEM não é tão óbvia e rápida quanto pela microscopia de fluorescência. Através das avaliações organoléticas das bebidas de café e dos cereais, observou-se que a amostra mais semelhante ao café é a cevada. A análise estatística dos testes sensoriais mostrou que o centeio e o milho apresentaram maiores diferenças significativas em relação ao café puro. Todos os adulterantes foram percebidos em concentrações superiores a 20%, porém, o único efetivamente reconhecido foi a cevada. Todos os métodos propostos para detecção de fraudes em café parecem ser mais eficazes do que o utilizado atualmente.
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Masquelier, Isaure. "Influence de la formulation sur les propriétés en fatigue d'élastomères industriels." Thesis, Brest, 2014. http://www.theses.fr/2014BRES0110/document.
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Cette étude concerne l’influence de la formulation sur les propriétés en fatigue des élastomères. Pour cela, douze matériaux ont été préalablement choisis de façon à ce que leur formulation soit simplifiée mais représentative de celles de matériaux industriels. La première partie de l’étude vise la description des mécanismes et des scénarios d’endommagement par fatigue, pour différents matériaux, niveaux de sollicitation et pourcentages de durée de vie. Une vaste campagne d’essais de fatigue interrompus a été menée permettant une analyse statistique de la population de défauts. Ces données ont permis d’une part de proposer des scénarios de ruine pour les différents matériaux étudiés, et d’autre part d’identifier deux types de mécanismes d’amorçage autour d’inclusions de différentes natures. La deuxième partie de l’étude vise à comprendre les mécanismes d’amorçage de fissure de fatigue. Un protocole expérimental permettant d’obtenir les champs d’énergie dissipée directement à partir des champs de température mesurés a été mis en place. Ce protocole a d’abord été développé à une échelle macroscopique et validé grâce à des simulations par éléments finis. Il a ensuite été appliqué avec succès à l’échelle des inclusions pour des cas 2D. Enfin, la troisième partie de cette étude propose un critère énergétique basé sur un protocole d’auto-échauffement permettant une détermination rapide des propriétés en fatigue. L’approche proposée utilise un critère à deux paramètres et permet de prédire la courbe de Wöhler déterministe avec une seule éprouvette, en une demi-journée d’essai et uniquement à partir de mesures thermiques. Ce critère a été validé sur une large gamme d’élastomères, et s’avère capable de rendre compte de l’influence de la gomme, du taux et du type de chargesThis study deals with the influence of the formulation on the fatigue properties of elastomeric materials. Twelve materials have been chosen so that their formulations are simplified but representative of these used in the industry. The first part of the study aims to describe the fatigue damage mechanisms and scenarios, for different materials, strain levels and fatigue life durations. A large experimental campaign of interrupted fatigue tests has been performed enabling a statistical analysis of the defects population. On one hand, these data led to propose damage scenarios for the studied materials, and on the other hand, to identify two classes of initiation mechanisms around different nature of inclusions. The second part of this study aims to better understand the fatigue crack initiation mechanisms. An experimental protocol enabling to obtain directly the dissipated energy fields from the measurement of the temperature fields has been set up. This protocol has been first developed at the macroscopic scale and validated thanks to numerical simulations. Then, it has been applied successfully at the scale of inclusions for 2D cases. Finally, the third part of this study suggests an energetic criterion based on a heat build-up protocol leading a fast determination of the fatigue properties. This approach uses a criterion with two parameters and is able to predict the deterministic Wöhler curve with one sample, in half a day and thanks to thermal measurements only. This criterion has been validated on a wide range of elastomeric materials and is able to reflect the influence of the gum, the type and the amount of carbon black
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Guerra, Carvallo Claver Hugo. "Estudio de la corrosión atmosférica sobre dos tipos de acero de bajo carbono en instalaciones industriales petroleras cercanas al mar en el nor oeste del Perú." Master's thesis, Universidad Nacional Mayor de San Marcos, 2014. https://hdl.handle.net/20.500.12672/3689.
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Este estudio de tesis, relacionado con la corrosión atmosférica sobre aceros de bajo carbono en instalaciones industriales petroleras, fue realizado en el área del Lote X operado por PETROBRAS ENERGIA PERU S.A. en el noroeste de Perú.
El objetivo consistió en determinar la velocidad de corrosión atmosférica sobre dos aceros de bajo carbono, en diferentes ubicaciones del Lote X, categorizarla de acuerdo a la norma ISO 9223 y mapearla. Se han utilizado probetas de acero, AISI/SAE 1020 y ASTM A 36 ya que estos materiales son usados en la construcción de facilidades de producción, transporte y recolección de petróleo, siendo de mayor uso el acero ASTM A36.
Las probetas fueron instaladas en 10 estaciones y expuestas al ambiente atmosférico en el periodo de septiembre del 2010 a noviembre del 2012. La ubicación de las estaciones fue seleccionada en función de la distancia al mar, altitud, topografía del terreno e impactos industriales, entre otros aspectos.
La velocidad de corrosión y el grado de corrosividad atmosférica fueron determinadas por la pérdida de peso de probetas construidas en acero AISI/SAE 1020, durante un año de exposición. Se han caracterizado los productos de corrosión por difracción de rayos X, fluorescencia de rayos X y microscopia electrónica. También se estudió el impacto de las siguientes variables ambientales: humedad, cloruros, SO2, NO2, H2S y velocidad del viento.
Como resultado de este estudio de tesis, podemos afirmar que en el Lote X la corrosión atmosférica es causada por la acción del oxígeno atmosférico e influenciado por la humedad, salinidad ambiental, por la capacidad del viento para transportar la brisa del mar al continente y polución sólida. Los productos de corrosión encontrados son: oxihidróxidos de hierro, akaganeita, lepidocrocita y goethita. La corrosión es influenciada por los cloruros de una manera polinómicas para los dos tipos de metal evaluados. Asimismo, se concluye que los gases contaminantes como SO2, H2S, NO2, no influyen en los fenómenos de corrosión. Las áreas próximas al mar y de libre circulación del viento favorecen la corrosión atmosférica y son categorizadas como ambientes de corrosión alta, categoría C4, para acero AISI/SAE 1020 y corrosión media, categoría C3, para acero ASTM A36. Para el resto de áreas la corrosión de ambos materiales es baja, categoría C2.
También podemos concluir que en ambiente marino, el acero ASTM A36 es de mayor resistencia a la corrosión atmosférica del Lote X que el acero especificado bajo norma AISI/SAE 1020.
Gracias a la información obtenida de velocidad de corrosión de este estudio, hemos podido elaborar mapas de corrosión para los dos tipos de acero estudiados, AISI /SAE 1020 y ASTM A 36. Esto es muy importante porque disponer de un mapa, permite una rápida visualización de las áreas de corrosividad crítica y no crítica, especialmente cuando se seleccionan materiales para construcción, selección de sistemas de pintura, selección de procedimientos de preparación de superficie para pintado, estimación de la vida de operación de instalaciones metálicas nuevas y antiguas. En el Lote X, la velocidad de corrosión es mayor en áreas cercanas al mar y de libre exposición a la brisa marina.
El presente trabajo de tesis ha permitido formular una ecuación que estima la corrosión atmosférica sobre probetas de acero al carbono AISI/SAE 1020, para las estaciones lejanas al mar y ubicadas en ambientes secos:
C = 164,99 t – 0,4045
Donde C es la velocidad de corrosión en m/año y t es el tiempo de exposición en días.
Palabras Clave: corrosión atmosférica, probetas, velocidad de corrosión, categorización de la corrosión, mapas de corrosividad, microscopia electrónica, fluorescencia y difracción de rayos X.Tesis
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Lizárraga, Olivares Wendy Carito. "Caracterización fenotípica y análisis genómico de dos cepas de Shewanella sp. nativas con capacidad de degradar colorantes azoicos." Bachelor's thesis, Universidad Nacional Mayor de San Marcos, 2019. https://hdl.handle.net/20.500.12672/11522.
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La industria textil utiliza principalmente colorantes de tipo azo dentro de sus procesos de tinción debido a su alto rendimiento y bajo costo, sin embargo, los colorantes azoicos son el grupo de colorantes más difíciles de degradar cuando son desechados al ambiente. Por ello la investigación realizada tiene como objetivo la caracterización fenotípica y el análisis genómico de dos cepas nativas del género Shewanella con capacidad de degradar colorantes azoico. Las cepas usadas fueron Shewanella sp. LC6 y Shewanella sp. 2NE11, caracterizadas a nivel fisiológico, bioquímico y genómico. Se realizaron cinéticas de crecimiento y de decoloración con los colorantes azul directo 71, anaranjado de metilo, amarillo proción HEXL y azul brillante remazol. Los ensayos relacionados a su fisiología incluyeron la evaluación de crecimiento bajo distintos parámetros como temperatura, pH y NaCl (%); entre las pruebas bioquímicas se evaluaron la producción de catalasa, oxidasa, movilidad, indol, H2S, lisina descarboxilasa, consumo de citrato, reducción de nitratos, licuefacción de gelatina, hemólisis y consumo de carbohidratos. El análisis genómico estuvo dirigido hacia la búsqueda de genes relacionados a decoloración, resistencia a metales y consumo de carbohidratos. Los resultados obtenidos muestran que las características fisiológicas y bioquímicas relacionan a la cepa Shewanella sp. LC6 dentro de la especie Shewanella xiamenensis y a Shewanella sp. 2NE11 dentro de Shewanella algae. Se identificaron proteínas como azorreductasas, peroxidasas, oxidorreductasas y ACP fosfodiesterasas relacionadas al proceso de decoloración y una gran cantidad de genes de resistencia a metales como el mercurio, zinc, cadmio, cobre y plata. Asimismo se encontraron proteínas relacionadas al consumo de carbohidratos como N-acetylglucosamina, maltosa, L-arabinosa, DL-lactato, D-fructosa y sucrosa. La presente investigación muestra el amplio potencial que tienen estas cepas para ser utilizadas en biorremediación de colorantes textiles y metales pesados.Tesis
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Derelli, Davide. "Self-assembly of colloidal particles - a combination of experimental and simulation approaches." Master's thesis, Alma Mater Studiorum - Università di Bologna, 2019. http://amslaurea.unibo.it/18076/.
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In this project, self-assembly behaviour of colloidal particles was investigated by a combination of both computer simulations and experimental approach. In particular, a Brownian Dynamics algorithm was used to simulate either steep-repulsive spheres or spherocylinders in a shrinking spherical confinement. In accordance with literature, in the former case packed spheres were shown to crystallize into a distinctive icosahedral structure. In the latter study, spherocylinders clearly revealed a local tendency to form smectic layers. After the synthesis of micro-sized fluorescent-labelled silica spheres and rods, particle self-assembly in a spherical confinement was experimentally explored. While our selected method widely produced well-defined spherical supraparticles, it generally failed in inducing crystalline or liquid-crystalline ordering. This outcome was supposed to emerge due to fast compression of particles inside the confinement.
In the last part of the project, Brownian Dynamics simulations of mixtures of rods and spheres in a spherical confinement were performed. Our preliminary investigation unveiled a modest tendency for rod-rich mixtures to form a binary smectic configuration. However, same-shape phase separation prominently occurred for increasing fractions of spheres. Notably, a quantitative analysis on the simulated configurations was accomplished by introduction of a novel binary smectic local order parameter.
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Baptistella, Marco Antonio. "Caracterização microestrutural de um aço aar m-201 grau e, em engate ferroviário fixo tipo "F", após magnetização por PRODS no ensaio com partículas magnéticas /." Guaratinguetá, 2016. http://hdl.handle.net/11449/143427.
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Orientador: Marcelo dos Santos PereiraCoorientadora: Cristina de Carvalho Ares Elisei
Banca: José Vitor de Cândido Souza
Banca: José Wilson de Jesus Silva
Resumo: Atualmente, as cargas aplicadas nos eixos de vagões ferroviários têm sofrido aumento de esforços devido ao choque e tração no engate ferroviário. Neste trabalho o estudo foi realizado no engate tipo "F", que tem maior utilização e interesse por parte da ferrovia, por se tratar de um engate rotativo e utilizado para descarregamento de vagões com os mais diversos tipos de carga. Este trabalho tem como objetivo, verificar se existem transformações da microestrutura no material do engate, e possíveis gerações de trincas, através do estudo do aço AAR M-201 Grau E, após o ensaio de partículas magnéticas, com corrente alternada através da aplicação de Prods. A faixa de amperagem variou-se de 100 a 1000 ampères e como meio de resfriamento, utilizou-se a água a temperatura ambiente e o ar forçado. A preparação foi feita partindo de um engate Tipo "F" completo, fornecido por um operador logístico, a cauda foi magnetizada por inteiro e depois separados os corpos de prova por corte de serra, refrigerado para não haver aquecimento. Para a caracterização microestrutural, utilizou-se uma preparação metalográfica de laboratório de bancada e ataque com Nital 2%, e fez-se uso de microscopia ótica convencional e microscopia eletrônica de varredura (MEV). Através da utilização da microscopia ótica e da microscopia eletrônica de varredura (MEV), pode-se verificar a microestrutura nas áreas que sofreram alterações microestruturais. Concluiu-se que o aço do engate, AAR M-201 grau E, após a magnetiz... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: Currently, the applied loads on the axles of railway cars has been increasing efforts due to shock and traction in railway coupling. In this work, the study was performed on the coupling type "F", which has increased use and interest on the part of the railway, because it is a rotary coupling and used for unloading of wagons with the most diverse types of cargo. This work aims, check for microstructural changes on the coupling material, and possible generation of cracks through the study of steel AAR M-201 grade and after the test of magnetic particles with alternating current by applying Prods. As amperage range, was varied from 100 to 1000 amps and as cooling medium water was used at room temperature and forced air. The preparation was made starting from a coupling type "F" full, provided by a logistics operator, the tail was magnetized in full and then separate the specimens by cutting saw, cooled to no heating. For microstructural characterization, we used a metallographic preparation of benchtop laboratory and attack Nital 2%, and was made use of conventional optical microscopy and scanning electron microscopy (SEM). By using light microscopy and scanning electron microscopy (SEM), you can check the microstructure in areas that suffered microstructural changes. It was concluded that the coupling of steel, AAR M-201 grade And after magnetization by Prods 300-1000 amps, presented change microstructural where there was a martensite acicular structure not tempered and genera... (Complete abstract click electronic access below)
Mestre
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Escale, Nicolas. "Étude par microscopie électronique en transmission des microstructures et des micromécanismes de déformation d'alliages de titane béta-métastables." Toulouse 3, 2012. http://thesesups.ups-tlse.fr/2509/.
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L'allègement des structures qui est une des taches prioritaires dans le développement de nouveaux avions peut être obtenu par l'introduction de matériaux ayant de très hautes performances mécaniques spécifiques. Les alliages de titane, par leurs hautes propriétés mécaniques, leur faible densité, leur haute tolérance au dommage et leur résistance à la corrosion sont particulièrement intéressant pour atteindre cet objectif. Ce travail a pour but de caractériser et de comprendre les micro-mécanismes fondamentaux de déformation dans deux alliages de titane de nouvelle génération, dits -métastables, que sont le Ti 5553 (Ti-5Al-5Mo-5V-3Cr) et le Ti 17 (Ti-5Al-2Sn-2Zr-4Mo-4Cr). Ces deux alliages apparaissent comme de très bons candidats pour remplacer l'alliage de référence dans l'aéronautique qu'est le TA6V (Ti-6Al-4V). Pour mener à bien cette étude nous avons dans un premier temps caractérisé par Microscopie Electronique en Transmission la microstructure très complexe de ces deux alliages : celle-ci est constituée de différentes phases hexagonales compactes ayant précipité dans une matrice cubique centrée. Une étude par déformation MET in situ couplée à des observations conventionnelles et en haute résolution ont permis d'identifier et quantifier les micro-mécanismes de déformation jouant un rôle dans la plasticité de ces matériaux. Nous avons ainsi déterminé que la résistance de ces alliages est due à différentes contributions telles qu'un durcissement structural, la présence d'un ordre local ou encore la structure de cœur des dislocations visThe lightening of structure is one of the most important issue in the aircraft industry. The weight saving for future planes could be obtained by the use of materials with very high specific mechanical performances. Titanium alloys have high mechanical properties, a relatively low density, an high damage tolerance and corrosion resistance are particularly interesting to reach this purpose. The aim of this present work is to characterize and understand the fundamental micro-mechanisms of deformation in two titanium alloys: Ti 5553 (Ti-5Al-5Mo-5V-3Cr) and Ti 17 (Ti-5Al-2Sn-2Zr-4Mo-4Cr). These two alloys seem to be good candidates to substitute the Ti64 alloy, which is the aeronautical industry reference. To carry out this study we have characterized by Transmission Electron Microscopy the microstructure, which consists in hexagonal phases embedded in a cubic centered matrix. In situ straining TEM experiments combined with conventional and High Resolution observations allow us to identified and quantified the micro-mechanisms of deformation that influence the plasticity in these materials. So we have determined that the strength is due to several contributions like: a structural hardening, the presence of a local order or the core structure of screw dislocations
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Rakotomavo, Tiana. "Etude de la génération du piégeage interne dans le silicium par tomographie laser à balayage." Montpellier 2, 1991. http://www.theses.fr/1991MON20125.
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Dans le cadre d'une etude sur le mecanisme de condensation de l'oxygene dans le silicium, une technique de caracterisation nouvelle, la tomographie laser a balayage a ete utilisee. Elle s'est revelee tres bien adaptee pour suivre l'evolution du processus de formation des precipites d'oxyde, etape importante dans la technique du piegeage interne. Sa non destructivite, sa capacite d'observation tridimensionnelle, sa sensibilite et sa rapidite conferent un large avantage sur les autres methdoes d'analyse
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Guedj, Cyril. "Elaboration, caracterisation et modelisation d'heterostructures silicium germanium carbone sur silicium. Applications industrielles des composes a base de si, ge, ou c (filiere iv-iv)." Paris 11, 1997. http://www.theses.fr/1997PA112397.
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Ce travail exploratoire porte sur l'elaboration, la caracterisation, la modelisation theorique et le potentiel industriel des composes a base de silicium, germanium, carbone. Les methodes possibles d'elaboration sont presentees. Les echantillons etudies ont ete realises par rtcvd, uhvcvd, plie, spem et mbe et caracterises par de nombreuses techniques complementaires. Un potentiel interatomique est adapte aux resultats experimentaux, afin de correler l'ordre nanoscopique aux proprietes liees a la microstructure. Cet outil, qui permet de calculer les parametres thermodynamiques a partir d'une repartition atomique, est notamment applique a l'interpretation conjointe des mesures raman, ftir, hrtem et de diffraction x. La microstructure depend de la methode d'elaboration, et un phenomene d'autoorganisation de c par rtcvd est demontre, par un faisceau convergent de caracterisations etayees par des simulations a l'echelle atomique. Les particularites liees a l'epitaxie laser (plie) sont detaillees. Une nouvelle methode de depot (spem) permet d'obtenir pour la premiere fois une couche contrainte contenant 70% de ge et 1. 6 % de c. Au niveau des proprietes thermiques, la mesure de dilatation de couches minces si#1#-#x#-#yge#xc#y constitue une nouvelle methode de dosage de ge et c. Une determination originale du pouvoir thermoelectrique par microscopie photothermique est suggeree. Pour des recuits a plus haute temperature, le carbone precipite sous forme de carbure de silicium incoherent, et l'hypothese d'un milieu devenu lacunaire s'accorde le mieux avec les resultats experimentaux. L'interdiffusion thermique de ge est etudiee quantitativement par diffraction x dans le cas de multipuits quantiques. L'etude controversee de la structure de bande des composes si#1#-#x#-#yge#xc#y est presentee. Les mesures ellipsometriques indiquent que le carbone induit un decalage de +65 mev/%c de e#1, alors que e#2 reste quasiment constant. Ce resultat est analyse dans le cadre de la theorie des potentiels de deformation. Cette etude physique eclaire l'analyse des applications industrielles de la filiere iv-iv, sous l'angle des brevets et des dispositifs, notamment en micro et opto-electronique. La comparaison avec la filiere iii-v paracheve ce memoire.
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Oger, Loïc. "Corrosion sous contrainte et fragilisation par l'hydrogène d'alliages d'aluminium de la série 7xxx (Al-Zn-Mg) : identification des paramètres microstructuraux critiques pilotant l'endommagement à l'échelle locale." Phd thesis, Toulouse, INPT, 2017. http://oatao.univ-toulouse.fr/19559/19/OGER_Loic_1_sur_2.pdf.
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Dans un contexte normatif toujours plus sévère concernant les rejets automobiles polluants, la substitution des aciers par des alliages d’aluminium dans les structures des véhicules est en plein essor. Ce projet de thèse, qui s’inscrit dans un programme de développement de la société Constellium, cible plus précisément les alliages d’aluminium de la série 7xxx (Al-Zn-Mg) qui, malgré leurs propriétés mécaniques élevées, peuvent présenter une sensibilité à la corrosion sous contrainte (CSC) liée au phénomène de fragilisation par l’hydrogène (FPH). La compréhension des mécanismes mis en jeu dans ce type d’endommagement constitue donc une première étape vers une optimisation métallurgique en vue d’une industrialisation future de ces alliages dans le secteur automobile. La première partie de ces travaux est consacrée à l’étude de l’influence de l’état métallurgique de l’alliage 7046 sur son comportement en CSC et à l’identification des mécanismes de dégradation. Un lien direct a pu être mis en évidence entre l’abattement des propriétés mécaniques et les modes de rupture actifs et la quantité d’hydrogène dans l’alliage. Les deux modes d’endommagement observés, intergranulaire-fragile et transgranulaire-fragile, ont respectivement été attribués à un enrichissement en hydrogène aux joints de grains et au piégeage de l’hydrogène au niveau des précipités intragranulaires. Les interactions entre l’hydrogène et les précipités fins d’une part et les dislocations d’autre part, identifiés comme deux hétérogénéités microstructurales critiques vis-à-vis de la FPH, ont été étudiées à une échelle plus locale dans la seconde partie du travail de thèse. Les essais ont été réalisés sur des échantillons modèles, chargés en hydrogène en milieu H2SO4 sous polarisation cathodique et la profondeur de pénétration de l’hydrogène a été évaluée par SKPFM (Scanning Kelvin Probe Force Microscopy). L’ensemble des résultats obtenus met en évidence : 1/ un effet « barrière » des précipités fins et des dislocations sur la diffusion de l’hydrogène en relation avec un abattement des propriétés mécaniques moins important, 2/ un transport possible de l’hydrogène par les dislocations et 3/ l’efficacité du SKPFM pour déterminer précisément des coefficients de diffusion apparents de l’hydrogène. Ces résultats ouvrent ainsi de nouvelles pistes vers la compréhension des mécanismes de CSC dans les alliages Al-Zn-Mg.
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Armanni, Thibaut. "Étude de nouveaux alliages de titane pour applications aéronautiques hautes températures." Electronic Thesis or Diss., Université de Lorraine, 2023. http://www.theses.fr/2023LORR0342.
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L'amélioration de la tenue en température des alliages de titane représente un défi de taille pour l'industrie aéronautique. En effet, dépasser la limite actuelle de 550°C dans les turbomoteurs requiert de trouver le meilleur compromis entre une bonne tenue à l'oxydation et de bonnes propriétés mécaniques en température. Les alliages dits quasi-alpha, constitués majoritairement de phase hexagonale compacte, sont ceux qui offrent les meilleures performances. Ils sont malheureusement sensibles à la fatigue/fluage à froid dit effet Dwell. Dans ce contexte, l'objectif de notre travail est double. D'une part, il s'agit de contribuer à la conception de nouveaux alliages quasi-alpha par apprentissage automatique grâce à une campagne extensive de caractérisation des propriétés mécaniques, à l'ambiante et à chaud. D'autre part, il s'agit de mieux comprendre l'impact de la composition chimique, notamment la teneur en silicium, sur la microstructure et le comportement mécanique. Pour cela, notre démarche a reposé sur la caractérisation de la microstructure de plusieurs alliages sélectionnés judicieusement, en croisant différentes techniques de microscopie. Nous avons ainsi examiné l'influence d'une variation de la teneur en silicium à différentes échelles, en combinant la microscopie électronique à balayage (MEB) et la microscopie électronique en transmission (MET). Nous avons mis en évidence la précipitation de siliciures au-delà d'une certaine teneur en Si, et entrepris de les caractériser de manière approfondie. En particulier, nous avons démontré les limitations d'une analyse en deux dimensions, et nous avons utilisé une technique alternative, combinant le découpage par faisceau d'ions (FIB) et l'observation par MEB pour reconstruire la microstructure en trois dimensions. Cette approche nous a permis d'observer en détail les formes, les tailles et les répartitions spatiales des siliciures. Enfin, nous avons mené des essais de traction à différentes vitesses de déformation ainsi que des essais de fluage dans diverses conditions, pour mieux comprendre le rôle bénéfique du silicium sur le comportement à froid et à chaud des alliages quasi-alphaImproving the high-temperature resistance of titanium alloys is a major challenge for the aerospace industry. Exceeding the current limit of 550°C in aircraft engines requires finding the best compromise between good oxidation resistance and good mechanical properties. Near-alpha alloys consisting mainly of a compact hexagonal phase are the best candidates. Unfortunately, they are sensitive to cold creep-fatigue, known as the dwell effect. In this context, our work aims to achieve two main objectives. Firstly, to contribute to the design of new near-alpha alloys based on machine learning, supported by extensive mechanical testing, at both ambient and high temperatures. Secondly, to gain a better understanding of the effect of chemical composition, particularly silicon content, on the microstructure and mechanical behaviour. Our approach was based on multi-scale microstructure study of selected alloys using a combination of different microscopy techniques. We examined the influence of a variation in silicon content using a combination of scanning electron microscopy (SEM) and transmission electron microscopy (TEM). We showed that silicide precipitation occurs above a certain silicon content. We demonstrated the limitations of two-dimensional analysis, and used an alternative technique combining ion beam cutting (FIB) with SEM observation to reconstruct the 3D microstructure. This approach enabled us to analyze and quantify the shapes, sizes and spatial distributions of the silicides. Finally, we carried out tensile tests at different strain rates as well as creep tests under various conditions to better understand how silicon addition improves the behaviour of near-alpha alloys
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Anxionnaz, Françoise. "Microstructure et composition chimique de composites sic/si : :(3)n::(4)." Paris 6, 1987. http://www.theses.fr/1987PA066141.
Full textAbstract:
On etudie par microscopie (meb, met, eels, edx) et par analyse par sonde ionique (sims) les composites prepares par impregnation de fibres de sic par depot chimique en phase vapeur de si::(3)n::(4) ou sic. On etudie l'influence du substrat sur la microstructure des depots, puis on caracterise la microstructure et la composition chimique de fibres elementaires de sic revetues par cvd de c et de sic. L'analyse des fibres revetues et tout particulierement de l'interface fibre/matrice montre la complementarite des methodes eels et sims pour caracteriser les composites a fibres longues
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Ramos, Aline. "Nucleation et croissance cristallines dans un verre sio::(2)-al::(2)o::(3)-li::(2)o : etude par microscopie electronique a haute resolution et absorption des rayons x." Paris 6, 1988. http://www.theses.fr/1988PA066504.
Full textAbstract:
Etude des premieres etapes de la cristallisation dans un verre du systeme sio::(2)-al::(2)o::(3)-li::(2)o(mgo) dans lequel de faibles quantites de titane et de zirconium sont introduites comme elements nucleants