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3D Printing of Specialty Devices for Geochemical Investigations: Real-Time Studies of Goethite and Schwertmannite FormationKletetschka, Karel 29 June 2018 (has links)
New types of laboratory reactors that are highly customizable, low-cost and easy to produce are needed to investigate low-temperature geochemical processes. We recently showed that desktop 3D printing stereolithography (SLA) can be used to efficiently fabricate a mixed flow reactor (MFR) with high dimensional accuracy comparable to traditional machining methods (Michel et al., 2018). We also showed that the SLA method allowed for the addition of complex features that are often beyond the capabilities of traditional methods. However, the stability of 3D printed parts at low-temperature geochemical conditions has not been fully evaluated. The objectives of this work were twofold: 1) to provide a framework for assessing the stability and compatibility of SLA printed materials at geochemically relevant conditions, and 2) to show how 3D printed specialty devices can enable new laboratory geochemical experiments. Part 1 of this Master's thesis presents findings for enhancing mechanical and solvent resistance properties of a commercial 3D printing material (Formlabs Clear) by UV post-curing procedures and also provide data showing its stability in aqueous solutions at pH 0, 5.7, and 12 for periods of up to 18 days. Thermal degradation patterns, mechanical analysis, and leachable fraction data are provided. Part 2 shows experiments coupling 3D printed reactors and flow devices for in situ small-angle x-ray scattering (SAXS). Schwertmannite (pH 2.7) and goethite (6.2) are precipitated from solution using various setups and observed differences in growth rates are discussed. The data show the potential of 3D printing for enabling novel laboratory geochemical experiments. / MS / New types of laboratory devices are needed to investigate environmental processes such as how minerals form, transform, and interact with their surroundings. These devices should be highly customizable, low-cost, and easy to produce. We have recently showed how 3D printing, specifically a technique called stereolithography (SLA), can be used to fabricate reactors with complex features that are often difficult to produce using traditional machining methods. However, in order to ensure that these materials don’t interfere with reactions of interest, we must assess the stability and compatibility of these materials in the relevant environmental conditions. As 3D printing techniques are still an emerging and rapidly developing technology, the methods we present will be useful for evaluating how new printer types and materials (i.e. resins) impact the suitability of 3D printed devices for future experimental studies. In part 1 of this thesis, the properties of a commercial 3D printing material were investigated by thermal and mechanical analyses; the propensity for leaching out material from the solid was also investigated. We show how exposing SLA printed materials to ultraviolet (UV) light post-printing can enhance material properties and minimize leaching. We then provide data showing the stability of the material after exposure to an array of acidic, neutral and basic conditions for a period of up to 18 days. In part 2, we describe experiments showing how novel 3D printed devices can be used to enhance laboratory investigations. Syntheses of two common iron oxide minerals using various custom reactor setups are presented. The setups were coupled with an analytical technique allowing for nanoscale observation of crystal growth in real-time. The data show how 3D printed specialty devices can be used to solve important questions in the geosciences such as the mechanisms of complex crystal formation.
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Nanomanipulação e caracterização de nano-objetos individuais por experimentos in situ de microscopia eletrônica / Nanomanipulation and characterization of individual nano-objects for in situ experiments of electron microscopyNakabayashi, Denise Basso 23 March 2007 (has links)
Orientador: Daniel Mario Ugarte / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-08T03:21:06Z (GMT). No. of bitstreams: 1
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Previous issue date: 2007 / Resumo: Há grandes expectativas de que, no futuro, componentes de alta tecnologia sejam baseados em novas e inesperadas propriedades físicas e químicas de objetos nanométricos. Muitas aplicações exigem que nano-objetos sejam posicionados precisamente em áreas bem definidas de um componente. Entretanto, os métodos estabelecidos de manipulação física usados na escala macroscópica não são aplicáveis na escala nanométrica. Muitas questões continuam em aberto e os avan»cos no estudo de nanossistemas são lentos. Muitos experimentos tem explorado a manipulação física usando microscopias de força atômica (AFM) e de tunelamento (STM), mas, nestes métodos, manipulação e observação não podem ser realizadas simultaneamente. Os microscópios eletrônicos de varredura (SEM) e de transmissão (TEM) são equipamentos essenciais no estudo de nano-objetos devido µa sua alta resolução e µa possibilidade de observar os movimentos realizados in situ em tempo real. Unindo esta técnica ao uso de nanomanipuladores, obtemos uma ferramenta poderosa para manipular e caracterizar nano-objetos. Existem diversos nanomanipuladores comerciais que operam em SEMs. Entretanto, o custo destes instrumentos é elevado, e os mesmos ficam restritos a grandes centros de pesquisa.
Nesta tese, descrevemos o desenho, construção e aplicação de nanomanipuladores com uma ou duas pontas de prova, cujos sistemas são baseados em mecânica simples e materiais de baixo custo. Estes sistemas operam dentro de um SEM equipado com um canhão por emissão de campo (FEG-SEM, JSM-6330F, resolução nominal 1.5 nm a 25 kV). Os movimentos grosseiros são baseados em um sistema elásticos (um eixo de movimento) e em uma modificação inovadora deste sistema. Em tal modificação, dois sistemas elásticos são acoplados, o que gera movimentos em dois eixos. Quanto aos movimentos finos, um conjunto de elementos piezoelétricos é responsável pelo deslocamento preciso em três eixos independentes de cada ponta de prova. O porta-amostra possui um grande deslocamento (15 mm), o que nos permite trabalhar com várias amostras em um mesmo experimento. Os instrumentos desenvolvidos permitem uma grande variedade de experimentos de nanomanipulação e nanocaracterização, incluindo a medicão de correntes e a aplicação de voltagens.
Os sistemas foram usados em diversos experimentos, tais como: a) fabricação de pontas de AFM de alta razão de aspecto baseadas em nanotubos de carbono multi-camadas; b) coletar, mover e posicionar nanofios semicondutores (100 - 300 nm de diâmetro, microns de comprimento) em contatos elétricos pré-definidos ou em áreas específicas de uma amostra; c) fabricação e caracterização elétrica de dispositivo eletrônico baseado em nanofios semi-condutores; d) caracterização das propriedades mecânicas de nano-objetos unidimensionais, como nanotubos de carbono e nanofios; etc. Finalmente, nossos resultados de manipulação demonstram que existem muitas oportunidades para a aplicação de manipulação física no método "bottom-up"em nanotecnologia / Abstract: It is expected that, in the future, high-technology devices should be based on new and unexpected physical and chemical properties of nanometric objects. Many applications require nano-objects to be selectively positioned at well-defined positions of a device. However, the well-established methods of physical manipulation used in the macroscopic scale are not applicable in nanoscale. Here, there are lots of open questions and the progress is still rather slow. Several experiments have exploited physical manipulation using atomic force microscopy (AFM) and scanning tunnelling microscopy (STM), but, in these techniques, manipulation and observation can not be performed simultaneously. The scanning (SEM) and transmission (TEM) electron microscopes are essential equipments for studying nano-objects due to their high resolution and to the possibility of observing performed movements in real time. Those techniques, together with the use of nanomanipulators, are powerful tools to manipulate and characterize nano-objects. There are several commercial nanomanipulators for SEMs. However, the price of these instruments is reasonably high, and they become restricted to a few research groups.
In this work, we report the development and applications of home-made nanomanipulators (with one or two probe tips) whose systems are based on simple mechanics and on low-cost materials. They operate inside a FEG-SEM (JSM-6330F, 1.5 nm nominal resolution at 25 kV). The coarse movements rely on parallel guiding spring based mechanics (one axis of movement) and on two overlapped parallel guiding spring based mechanics (two axes of movement). The precise movements are due to an ensemble of piezoelectric elements that has three independent axes of movement for each probe tip. The sample support has a large range (15 mm) on one axis, which allows working with several samples during the same experiment. The instruments are suitable for a wide spectrum of nanomanipulation and nanocharacterization experiments, including measuring currents and applying voltages.
The systems have been used for a variety of applications, such as: a) fabricating high aspect-ratio AFM tips based on multi-walled carbon nanotubes; b) collecting, moving, and positioning semiconductor nanowires (100 - 300 nm in diameter, microns in length) on predefined electrical contacts or special sample sites; c) fabrication and electrical characterization of an electronic device based on semiconductor nanowires; d) characterization of mechanical properties of one-dimensional nano-objects, as carbon nanotubes and nanowires; etc. Brie°y, our manipulation results demonstrate that there are plenty of opportunities for applications of physical manipulation in the bottom-up approach to nanotechnology / Doutorado / Física da Matéria Condensada / Doutor em Ciências
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Exploring metallic materials behavior through in situ crystallographic studies by synchrotron radiation = Explorando o comportamento de materiais metálicos através de estudos cristalográficos in situ via radiação síncrotron / Explorando o comportamento de materiais metálicos através de estudos cristalográficos in situ via radiação síncrotronFaria, Guilherme Abreu, 1987- 26 August 2018 (has links)
Orientador: Antonio Jose Ramirez Londono / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-26T15:15:59Z (GMT). No. of bitstreams: 1
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Previous issue date: 2014 / Resumo: O objetivo deste trabalho foi desenvolver a metodologia de medição e análise de dados para a instalação experimental XTMS. Esta instalação foi projetada para possibilitar a medição simultânea de difração de raios X e informações térmicas e mecânicas de materiais enquanto estes são submetidas a condições termomecânicas controladas. Esta é uma área de grande interesse para cientistas de materiais uma vez que uma vasta gama de propriedades termomecânicas têm suas origens em propriedades microscópicas que são acessíveis através de dados de difração. Durante o trabalho, foram estudadas estratégias de medição, desenhos de amostras, métodos de processamento e análise de dados, assim como foi feita a caracterização da instalação como equipamento de medida de dados de difração. Como parte do trabalho, a instalação foi aplicada no estudo de casos científicos de interesse, que envolvem tanto diferentes metodologias de ensaios quanto dados de difração que exigem diferentes metodologias de análise. Os estudos consistiram em um ensaio de deformação em uma liga com memória de forma, ensaios de decomposição isotérmica em um aço inoxidável Superduplex UNS-S32750, e um ensaio de dilatometria acompanhado por difração do aço supermartensítico SuperCr13 / Abstract: The aim of this work was to develop measurement and data analysis methodologies for the XTMS experimental installation. This facility was engineered to simultaneously collect X-ray diffraction and thermo-mechanical information of materials as they are subjected to controlled thermo-mechanical conditions. This is an area of great interest for material scientists given the wide range of thermo-mechanical properties correlated with microscopic properties which are accessible through X-ray diffraction. Developments performed during this work include the development and/or study of measurement strategies, sample designs, and data processing and analysis, as well as the characterization of the XTMS installation as an X-ray diffraction station. As part of the work, the installation was used to study several cases of scientific interest, involving different testing and data analysis methodologies. The studies performed were the deformation of a shape memory alloy, the isothermal ferrite decomposition on a Superduplex stainless steel UNS-S32750, and phase transformations on a SuperCr13 supermartensitic steel through dilatometry coupled with time resolved X-ray diffraction / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica
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Influência da adição de nitrato de cálcio e de PhoslockTM no abatimento dos fluxos de nutrientes e metais na interface sedimento-coluna de água em um sistema lacustre eutrofizadoOliveira, Aline Fernandes de 16 February 2012 (has links)
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Previous issue date: 2012-02-16 / Financiadora de Estudos e Projetos / This research project evaluated the changes in the fluxes of nutrients
and metals at the sediment-water interface as a result of sediment treatment by the
additions of PhoslockTM and calcium nitrate solution. The experiments were executed
in situ using mesocosms that were assembled in the Ibirité Reservoir (MG). The
calcium nitrate addition experiments showed nutrients flux abatement for Porthophosphate,
ammoniacal-N and nitrate-N that were ≥ 90% whilst for the metals
Fe and Mn the percentages reached 48 and 69%, respectively, as a result of
sediment oxidation promoted by the intensification of denitrification rates. For the
PhoslockTM addition the percentages of reduction in the fluxes across sediment-water
interface was over 90% for P-orthophosphate and ammoniacal-N, 78% for nitrate-N
and for the metals, Fe and Mn, 47 and 50%, respectively, as a result of the increased
adsorption capacity of sediments due an excess of adsorbent material left on
sediment surface. / Este projeto avaliou a capacidade de abatimento dos fluxos de metais e
nutrientes na interface sedimento-coluna de água da represa de Ibirité (MG),
comparando-se duas diferentes tecnologias de remediação de sistemas lacustres, a
adição de PhoslockTM e de nitrato de cálcio. Os experimentos foram realizados in
situ, com montagem de mesocosmos na citada represa. Os resultados referentes ao
tratamento com injeção de nitrato de cálcio mostraram, em função da oxidação dos
sedimentos promovida por esta tecnologia, um abatimento dos fluxos de nutrientes
(P-ortofosfato, N-amoniacal, N-nitrato) iguais ou superiores a 90%, enquanto que
para os metais Fe e Mn, as porcentagens de abatimento de fluxo alcançaram 48 e
69%, respectivamente. Para o tratamento dos sedimentos com a adição de
PhoslockTM, devido ao aumento da capacidade de adsorção dos sedimentos
promovida pelo excesso de material adsorvente depositado na superfície dos
mesmos, as porcentagens de redução dos fluxos sedimento-água foram superiores
a 90% para o P-ortofosfato e N-amoniacal, 78% para o N-nitrato, e para os metais
(Fe e Mn), 47 e 50%, respectivamente.
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Characterization methodology to assess the mechanical properties of delignified birch/PMMA transparent wood biocomposites / Karakteriseringsmetodik för att bedöma de mekaniska egenskaperna hos transparenta trä biokompositer av delignifierad björk/PMMAArcieri, Nicolò January 2022 (has links)
Transparent trä biokompositer (TW) är en ny attraktiv klass av biokomposit. De är uppbyggda av delignifierat trä som impregnerats med en polymer med matchande brytningsindexet. TW kan skräddarsys för inom ett brett spektrum av funktionella, optiska och mekaniska egenskaper. Eftersom de är biobaserade ses de dessutom som ett möjligt material som kan ersätta andra, mer miljöpåverkande material, inom olika sektorer, däribland byggnadsindustrin. Till skillnad från de funktionella egenskaperna har det mekaniska beteendet hos dessa biokompositer dock inte undersökts särskilt ingående. Syftet med denna avhandling är därför att utöka den nuvarande kunskapen om det mekaniska beteendet av dessa material genom att använda två olika mekanisk karakterisering metoder av TW och vanligt trä som referensmaterial. TW framställdes genom impregnering av delignifierade björkfaner med PMMA. Den mekaniska karakteriseringen utfördes med hjälp av olika metoder. Elastiska modulen och böjhållfastheten i tvärriktningen studerades med hjälp av fyrpunktsböjningprov. Resultaten visade en förbättring för båda egenskaperna jämfört med vanligt björkträ. Brottet vinkelrätt mot fibern (TR-systemet) undersöktes genom att utföra in situ fyrpunktsböjningstester på prover med en kant-spricka i ett svepelektronmikroskop för att observera hur sprickorna fortplantar sig i den komplexa mikrostrukturen. En anmärkningsvärd förbättring (cirka 175 procent) av brottsstyrkan konstaterades jämfört med vanligt trä. Dessutom användes DIC-teknik (digital image correlation) på fyrpunktsböjningstesterna, med kant-spricka, för att studera spänningsfältet under spricktillväxten, särskilt bildandet av brottprocesszonen (FPZ) runt sprickspetsen. Därefter föreslogs en ekvation som beskriver kohesionslagen för båda materialen baserat på experimentella observationer som i slutändan kan användas för sprickmekaniska simuleringar. Slutligen visades kort hur man kan använda de uppmätta mekaniska egenskaperna hos den nya TW för materialval för tekniska tillämpningar. / Transparent wood (TW) biocomposites are a new attractive class of materials. They are based on a delignified wood template impregnated by a refractive index-matching polymer. TWs can be tailored in order to show a wide range of functional, optical, and mechanical properties. Moreover, being biobased, they are seen as a possible key material to replace more environmentally impactful materials in various sectors including the construction industry. However, unlike the functional properties, the mechanical behaviour of this class of materials has been poorly investigated. Therefore, in this thesis, the aim was to extend the current knowledge about the mechanical response of these materials by using a two-step mechanical characterization on TW and native wood as reference material. The analysed TW biocomposite was prepared by impregnation of delignified birch veneers by PMMA. The mechanical characterization was carried out using different techniques. The Young’s modulus and the flexural strength along the transverse direction were studied by four-point bending tests. The results showed an improvement for both properties compared to native birch wood. The fracture perpendicular to the grain (TR system) was investigated by performing in situ single-edge-notched four-point bending tests onto a scanning electron microscope to observe how the cracks propagate in this complex microstructure. A remarkable improvement (about 175 percent) in fracture toughness was found compared to the native wood. Furthermore, the in situ single-edge-notched four-point bending test was also applied, together with the digital image correlation (DIC) technique, to study the strain field during the crack growth, specifically the formation of the fracture process zone (FPZ) around the crack tip. Then, an equation describing the cohesive law was proposed for both materials based on experimental observations that can be ultimately used for fracture mechanics simulations. Finally, it was briefly shown how to make use of the measured mechanical properties of the novel TW for material selection for engineering applications.
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Thermo-Mechanische Charakterisierung von Grenzflächen zwischen Einwandigen Kohlenstoffnanoröhren und Metallen mittels Auszugsversuchen / Thermo-Mechanical Characterization of Interfaces between Single-Walled Carbon Nanotubes and Metals by Pull-Out TestingHartmann, Steffen 22 April 2016 (has links) (PDF)
Vor dem Hintergrund zukünftiger Sensoren, basierend auf dem piezoresistiven Effekt von einwandigen Kohlenstoffnanoröhren (SWCNT), werden in dieser Arbeit umfangreiche Ergebnisse zum mechanischen Verhalten von Grenzflächen zwischen SWCNTs und edlen Metallen am Beispiel von Pd und Au präsentiert. Im Fokus steht dabei die Synergie von rechnerischen und experimentellen Methoden Molekulardynamik (MD), nanoskalige Tests und Analytik , um (1) mit guter Genauigkeit maximale Kräfte von gezogenen SWCNTs, welche in Metall eingebettet sind, vorauszuberechnen und (2) einen wertvollen Beitrag zum Verständnis der zu Grunde liegenden Fehlermechanismen zu liefern.
Es wurde ein MDModell eines in eine einkristalline Matrix eingebetteten SWCNTs mit Randbedingen eines Auszugsversuchs entwickelt. Mit diesem Modell können Kraft-Weg-Beziehungen und Energieverläufe für einen quasistatischen verschiebungsgesteuerten Auszugsversuch errechnet werden. Das Modell liefert kritische Kräfte bei Versagen des Systems. Des Weiteren können mit diesem Modell der Einfluss des SWCNT-Typus, der Einbettungslänge, der Temperatur, von intrinsischen Defekten und Oberflächengruppen (SFGs) auf das Grenzflächenverhalten untersucht werden.
Zum Vergleich wurden kritische Kräfte experimentell durch in situ Auszugsversuche in einem Rasterelektronenmikroskop bestimmt. Es wurde eine sehr gute Übereinstimmung von rechnerischen und experimentellen Daten festgestellt. Der vorherrschende Fehler im Experiment ist der SWCNT-Bruch, jedoch wurden auch einige SWCNT-Auszüge beobachtet.
Mit Hilfe der MD-Simulationen wurde gefunden, dass die SFGs als kleine Anker in der umgebenden metallischen Matrix wirken und somit die maximalen Kräfte signifikant erhöhen. Diese Grenzflächenverstärkung kann Zugspannungen verursachen, die genügend hoch sind, so dass SWCNT-Bruch initiert wird. Im Gegensatz dazu zeigten Simulationen von Auszugstests mit idealen SWCNTs nur kleine Auszugskräfte, welche meistens unabhängig von der Einbettungslänge des SWCNTs sind. Dieses Verhalten wird mit einer inkommensurablen Konfiguration der Kristallstrukturen an der Grenzfläche von SWCNTs und der einbettenden Edelmetalle interpretiert.
Zur Qualifizierung der Existenz von carboxylatischen Oberflächengruppen auf dem genutzten SWCNT-Material wurden analytische Untersuchungen mittels Fluoreszenzmarkierung von Oberflächengruppen durchgeführt. In Übereinstimmung mit Literaturstellen zum gesicherten Nachweis von SFGs, bedingt durch technologische Behandlungen, weisen diese Experimente stark auf das Vorhandensein von carboxylatischen Oberflächengruppen auf dem genutzten SWCNT-Material hin. Demnach kann der dominante SWCNT-Bruch Fehler durch die Grenzflächenverstärkung auf Grund von SFGs erklärt werden. / In the light of future sensors, that are based upon the piezoresistive effect of singlewalled carbon nanotubes (SWCNTs), this work presents comprehensive results of studies on the mechanical behavior of interfaces between SWCNTs and noble metals using the examples of Pd and Au. With this contribution, the focus is on a synergy between computational and experimental approaches involving molecular dynamics (MD) simulations, nanoscale testing, and analytics (1) to predict to a good degree of accuracy maximum forces of pulled SWCNTs embedded in a noble metal matrix and (2) to provide valuable input to understand the underlying mechanisms of failure.
A MD model of a SWCNT embedded in a single crystalline matrix with pull-out test boundary conditions was developed. With this model, force-displacement relations and energy evolutions for a quasi-static displacement controlled test can be computed. The model provides critical forces for failure of the system. Furthermore, the influence of SWCNT type, embedding length, temperature, intrinsic defects and surface functional groups (SFGs) on the interface behavior can be studied using this model.
For comparison, critical forces were experimentally determined by conducting pull-out tests in situ, inside a scanning electron microscope. A very good agreement of computational and experimental values was discovered. The dominant failure mode in the experiment was a SWCNT rupture, although several pull-out failures were also observed.
From MD simulations, it was found that SFGs act as small anchors in the metal matrix and significantly enhance the maximum forces. This interface reinforcement can lead to tensile stresses sufficiently high to initiate SWCNT rupture. In contrast, pull-out test simulations of ideal SWCNTs show only small pull-out forces, which are mostly independent on SWCNT embedding length. This behavior is interpreted with an incommensurate configuration of crystal structures at the interface between SWCNTs and embedding noble metals.
To qualify the existence of carboxylic SFGs on the used SWCNT material, an analytical investigation by means of fluorescence labeling of surface species was performed. In agreement with literature reports on the secured verification of SFGs due to necessary technological treatments, these experiments strongly indicate the presence of carboxylic SFGs on the used SWCNT material. Thus, the dominant SWCNT rupture failure is explained with an interface reinforcement by SFGs.
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Approche expérimentale in-situ de la signature sismique du rôle des fluides dans la rupture des zones de faille : application à la rupture des grands versants rocheux fracturés / In-situ experimental study of the seismic signatures of the role of fluids in the rupture of fault zones : application to large rockslides failure studiesDerode, Benoît 01 July 2013 (has links)
Cette thèse s’intéresse à la signature sismique du rôle des fluides dans les mécanismes de déformation des roches fracturées de la croûte supérieure, et plus précisément les failles et les glissements de terrain. S’il est admis que les fluides sont un facteur déclenchant de la rupture dans le cas d’épisodes de forçages climatiques importants ou de glissements très superficiels, leur rôle dans la déstabilisation des grands volumes associée à des forçages faibles est beaucoup moins bien compris. Ainsi, il apparaît nécessaire d’acquérir de nouvelles données synchrones des pressions/débits de fluides, de la déformation et de la sismicité sur le terrain dans des conditions de chargement hydraulique contrôlées pour progresser dans la compréhension des liens entre processus hydromécaniques et sismiques participant à la nucléation de la rupture des roches en partie associée à la réactivation de fractures existantes. Motivé par ce besoin de nouvelles observations, ce travail de thèse concerne l’interprétation de la sismicité produite lors d’expériences originales de stimulation hydraulique (0.3 à 3.5 MPa et 10 à 3000 secondes) de petites zones de faille ou de fractures de taille décamétrique, situées en zones non saturées profonde de versants rocheux. Ces expériences consistaient à produire des déformations menant à l’activation du glissement le long des fractures préexistantes. Le protocole expérimental combine des mesures de déformations/pressions distribuées dans les structures géologiques à des capteurs sismologiques proches (échelle métrique à décamétrique) des zones sources. / This PhD dissertation focuses on the seismic signatures of the role of fluids in the deformation mechanisms of fractured rocks in the upper crust, mainly faults and landslides. While it is generally admitted that fluids are a triggering mechanism for rupture in the cases of episodic and major climate forcing events on shallow landslides, their role in the destabilization of large volumes of rocks, associated to weak forcing, is less understood. Thus, it is primordial to acquire new synchronous data of fluid pressure/flow, deformation and induced seismicity in the field, under controlled conditions of the hydraulic loading, in order to better understand the relationship between seismic and hydromechanical processes involved in the nucleation of rock ruptures, in part associated to the reactivation of existing fractures. Motivated by the need for new observations, this PhD thesis concerns the interpretation of the induced seismicity within unsaturated zones of deep rocky slopes, during original and controlled hydraulic stimulation experiments (0.3 to 3.5 MPa and from 10 to 3000 seconds) of small areas of decameter size. These experiments consisted in triggering rock deformations which lead to the activation of rock sliding along pre-existing fractures where deformation/pressure measurements and seismic sensors were distributed. These experiments were carried out in the Low Noise Underground Laboratory (France), which allows the access to fault zones within a rocky slope (at 250 m depth) and enables accurate geophysical measurements in conditions of very low environmental noise.
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Thermo-Mechanische Charakterisierung von Grenzflächen zwischen Einwandigen Kohlenstoffnanoröhren und Metallen mittels Auszugsversuchen / Thermo-Mechanical Characterization of Interfaces between Single-WalledCarbon Nanotubes and Metals by Pull-Out TestingHartmann, Steffen 04 February 2016 (has links)
Vor dem Hintergrund zukünftiger Sensoren, basierend auf dem piezoresistiven Effekt von einwandigen Kohlenstoffnanoröhren (SWCNT), werden in dieser Arbeit umfangreiche Ergebnisse zum mechanischen Verhalten von Grenzflächen zwischen SWCNTs und edlen Metallen am Beispiel von Pd und Au präsentiert. Im Fokus steht dabei die Synergie von rechnerischen und experimentellen Methoden Molekulardynamik (MD), nanoskalige Tests und Analytik , um (1) mit guter Genauigkeit maximale Kräfte von gezogenen SWCNTs, welche in Metall eingebettet sind, vorauszuberechnen und (2) einen wertvollen Beitrag zum Verständnis der zu Grunde liegenden Fehlermechanismen zu liefern.
Es wurde ein MDModell eines in eine einkristalline Matrix eingebetteten SWCNTs mit Randbedingen eines Auszugsversuchs entwickelt. Mit diesem Modell können Kraft-Weg-Beziehungen und Energieverläufe für einen quasistatischen verschiebungsgesteuerten Auszugsversuch errechnet werden. Das Modell liefert kritische Kräfte bei Versagen des Systems. Des Weiteren können mit diesem Modell der Einfluss des SWCNT-Typus, der Einbettungslänge, der Temperatur, von intrinsischen Defekten und Oberflächengruppen (SFGs) auf das Grenzflächenverhalten untersucht werden.
Zum Vergleich wurden kritische Kräfte experimentell durch in situ Auszugsversuche in einem Rasterelektronenmikroskop bestimmt. Es wurde eine sehr gute Übereinstimmung von rechnerischen und experimentellen Daten festgestellt. Der vorherrschende Fehler im Experiment ist der SWCNT-Bruch, jedoch wurden auch einige SWCNT-Auszüge beobachtet.
Mit Hilfe der MD-Simulationen wurde gefunden, dass die SFGs als kleine Anker in der umgebenden metallischen Matrix wirken und somit die maximalen Kräfte signifikant erhöhen. Diese Grenzflächenverstärkung kann Zugspannungen verursachen, die genügend hoch sind, so dass SWCNT-Bruch initiert wird. Im Gegensatz dazu zeigten Simulationen von Auszugstests mit idealen SWCNTs nur kleine Auszugskräfte, welche meistens unabhängig von der Einbettungslänge des SWCNTs sind. Dieses Verhalten wird mit einer inkommensurablen Konfiguration der Kristallstrukturen an der Grenzfläche von SWCNTs und der einbettenden Edelmetalle interpretiert.
Zur Qualifizierung der Existenz von carboxylatischen Oberflächengruppen auf dem genutzten SWCNT-Material wurden analytische Untersuchungen mittels Fluoreszenzmarkierung von Oberflächengruppen durchgeführt. In Übereinstimmung mit Literaturstellen zum gesicherten Nachweis von SFGs, bedingt durch technologische Behandlungen, weisen diese Experimente stark auf das Vorhandensein von carboxylatischen Oberflächengruppen auf dem genutzten SWCNT-Material hin. Demnach kann der dominante SWCNT-Bruch Fehler durch die Grenzflächenverstärkung auf Grund von SFGs erklärt werden. / In the light of future sensors, that are based upon the piezoresistive effect of singlewalled carbon nanotubes (SWCNTs), this work presents comprehensive results of studies on the mechanical behavior of interfaces between SWCNTs and noble metals using the examples of Pd and Au. With this contribution, the focus is on a synergy between computational and experimental approaches involving molecular dynamics (MD) simulations, nanoscale testing, and analytics (1) to predict to a good degree of accuracy maximum forces of pulled SWCNTs embedded in a noble metal matrix and (2) to provide valuable input to understand the underlying mechanisms of failure.
A MD model of a SWCNT embedded in a single crystalline matrix with pull-out test boundary conditions was developed. With this model, force-displacement relations and energy evolutions for a quasi-static displacement controlled test can be computed. The model provides critical forces for failure of the system. Furthermore, the influence of SWCNT type, embedding length, temperature, intrinsic defects and surface functional groups (SFGs) on the interface behavior can be studied using this model.
For comparison, critical forces were experimentally determined by conducting pull-out tests in situ, inside a scanning electron microscope. A very good agreement of computational and experimental values was discovered. The dominant failure mode in the experiment was a SWCNT rupture, although several pull-out failures were also observed.
From MD simulations, it was found that SFGs act as small anchors in the metal matrix and significantly enhance the maximum forces. This interface reinforcement can lead to tensile stresses sufficiently high to initiate SWCNT rupture. In contrast, pull-out test simulations of ideal SWCNTs show only small pull-out forces, which are mostly independent on SWCNT embedding length. This behavior is interpreted with an incommensurate configuration of crystal structures at the interface between SWCNTs and embedding noble metals.
To qualify the existence of carboxylic SFGs on the used SWCNT material, an analytical investigation by means of fluorescence labeling of surface species was performed. In agreement with literature reports on the secured verification of SFGs due to necessary technological treatments, these experiments strongly indicate the presence of carboxylic SFGs on the used SWCNT material. Thus, the dominant SWCNT rupture failure is explained with an interface reinforcement by SFGs.
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