Bibliografías temáticas / In situ TEM nanoindentation / Tesis
Siga este enlace para ver otros tipos de publicaciones sobre el tema: In situ TEM nanoindentation.

Tesis sobre el tema "In situ TEM nanoindentation"

Autor: Grafiati
Publicado: 4 de junio de 2021
Última modificación: 1 de febrero de 2022

Crea una cita precisa en los estilos APA, MLA, Chicago, Harvard y otros

Elija tipo de fuente:

Consulte los 50 mejores tesis para su investigación sobre el tema "In situ TEM nanoindentation".

Junto a cada fuente en la lista de referencias hay un botón "Agregar a la bibliografía". Pulsa este botón, y generaremos automáticamente la referencia bibliográfica para la obra elegida en el estilo de cita que necesites: APA, MLA, Harvard, Vancouver, Chicago, etc.

También puede descargar el texto completo de la publicación académica en formato pdf y leer en línea su resumen siempre que esté disponible en los metadatos.

Explore tesis sobre una amplia variedad de disciplinas y organice su bibliografía correctamente.

1

Calvié, Emilie. "Contribution de la nanoindentation in situ en Microscopie Electronique en Transmission à l'étude des céramiques". Thesis, Lyon, INSA, 2012. http://www.theses.fr/2012ISAL0098.

Texto completo
Resumen
La connaissance du comportement et des propriétés des matériaux est d’une grande importance pour optimiser leur mise en forme et adapter leur utilisation. Pour étudier ces propriétés de nombreuses techniques sont couramment utilisées : les essais de traction, la microindentation, la nanoindentation instrumentée… Aujourd’hui, un intérêt particulier est porté sur les nanomatériaux et matériaux nanostructurés car ils présentent souvent des propriétés différentes et plus intéressantes. La nanoindentation instrumentée, notamment, permet de déterminer des paramètres matériaux de manière locale. Cependant, le comportement en temps réel ne peut être observé et l’échantillon ne doit pas être de dimension trop faible (typiquement, l’étude de nanoparticules n’est pas envisageable). Le principal atout de la nanoindentation in situ en Microscopie Electronique en Transmission vis-à-vis des autres techniques existantes est la possibilité d’étudier le comportement de nano-objets ou des comportements très locaux et en temps réel, tout en observant les transformations subies par le matériau. Dans cette étude, nous avons évalué les potentialités de cette nouvelle technique via l’analyse de céramiques très étudiées au laboratoire notamment en tant que biomatériaux : la zircone stabilisée et l’alumine. Dans le cas de la zircone (stabilisée à l’yttrium ou au cérium), le but était de localiser à l’échelle nanométrique les contraintes responsables ou inhérentes à la transformation de phase quadratique-monoclinique, phénomène ayant une très grande influence sur les propriétés du matériau massif. Pour ce faire, après avoir déterminé une technique de préparation adaptée, nous proposons une voie d’étude pour la localisation des contraintes liées à la transformation de phase : le CBED (Convergent Beam Electron Diffraction) couplé à la nanoindentation in situ. Dans le cas de l’alumine, l’objectif était d’étudier le matériau (commercial et non un matériau modèle) dans sa forme originelle à savoir sous forme de nanoparticules d’alumine de transition. L’idée était d’étudier le comportement de ces nanoparticules sous compression. Nous avons notamment constaté que ces particules pouvaient subir une grande déformation plastique à température ambiante. Nous avons pu également, sur quelques particules, obtenir une série d’images en cours de compression ainsi que la courbe de charge-déplacement correspondante. Ces résultats ont ensuite été soumis à une analyse des images couplée à une simulation de type Eléments Finis (réalisées par le LAMCOS)
Knowledge of the behavior and properties of materials is of great importance to optimize their processing and adapt their use. To study these properties, many techniques are commonly used: tensile tests, microindentation, instrumented nanoindentation ... Today, particular interest is focused on nanomaterials and nanostructured materials because they often have different and more interesting properties. Instrumented nanoindentation allow to determine material parameters. However, the real-time behavior can not be observed and the study of nano-objects is difficult (nanoparticles for example). The main advantage of in situ TEM (Transmission Electron Microscopy) nanoindentation is the ability to study the behavior of nano-objects in real time. In this study, we evaluated the potential of this new technique by analyzing ceramics extensively studied in the laboratory such as biomaterials: stabilized zirconia and alumina. In the case of zirconia (stabilized with yttrium or cerium), the goal was to locate at the nanoscale, the constraints responsible for the tetragonal to monoclinic phase transformation. This phenomenon having a great influence on the bulk material properties. To do this, after having determined a suitable preparation method, we suggest a way to study the localization of constraints: the CBED (Convergent Beam Electron Diffraction) coupled with in situ TEM nanoindentation. In the case of alumina, the goal was to study the material in its original form (nano powder of transition alumina). The idea was to study the behavior of these nanoparticles under compression. We particularly observed that these particles could undergo large plastic deformation at room temperature. We have also obtained during compression on few particles, series of images and the corresponding load-displacement curve. These results were then analyzed by image analysis coupled with Finite Element simulations (performed in LAMCOS lab)
Los estilos APA, Harvard, Vancouver, ISO, etc.
2

Guitton, Antoine. "Mécanismes de déformation des phases MAX : une approche expérimentale multi-échelle". Thesis, Poitiers, 2013. http://www.theses.fr/2013POIT2280/document.

Texto completo
Resumen
Il est couramment admis que la déformation plastique des phases MAX est dueau glissement de dislocations dans les plans de base s'organisant en empilements et murs. Cesderniers peuvent former des zones de désorientation locale appelées kink bands. Cependant, lesmécanismes élémentaires et le rôle exact des défauts microstructuraux sont encore mal connus. Cemanuscrit présente une étude expérimentale multi-échelle des mécanismes de déformation de laphase MAX Ti2AlN. A l'échelle macroscopique, deux types d'expériences ont été menés. Des essaisde compression in-situ à température et pression ambiantes couplés à la diffraction neutroniqueont permis de mieux comprendre le comportement des différentes familles de grains dans le Ti2AlNpolycristallin. Des essais de compression sous pression de confinement ont également été réalisés dela température ambiante jusqu'à 900 °C. À l'échelle mésoscopique, les microstructures des surfacesdéformées ont été observées par MEB et AFM. Ces observations complétées par des essais denanoindentation ont montré que la forme des grains et leur orientation par rapport à la directionde sollicitation gouvernent l'apparition de déformations intra- et inter-granulaires ainsi que lalocalisation de la plasticité. Finalement à l'échelle microscopique, une étude détaillée par METdes échantillons déformés sous pression de confinement a révélé la présence de configurations dedislocations inédites dans les phases MAX, telles que des réactions entre dislocations, des dipôleset des dislocations hors plan de base. À la vue de ces résultats nouveaux, les propriétés mécaniquesdes phases MAX sont rediscutées
It is commonly believed that plastic deformation mechanisms of MAX phases consistin basal dislocation glide, thus forming pile-ups and walls. The latter can form local disorientationareas, known as kink bands. Nevertheless, the elementary mechanisms and the exact role ofmicrostructural defects are not fully understood yet. This thesis report presents a multi-scale experimentalstudy of deformation mechanisms of the Ti2AlN MAX phase. At the macroscopic scale,two kinds of experiments were performed. In-situ compression tests at room temperature coupledwith neutron diffraction brought new insight into the deformation behavior of the different grainfamilies in the polycrystalline Ti2AlN. Compression tests from the room temperature to 900 °Cunder confining pressure were also performed. At the mesoscopic scale, deformed surface microstructureswere observed by SEM and AFM. These observations associated with nanoindentationtests showed that grain shape and orientation relative to the stress direction control formationof intra- and inter- granular strains and plasticity localization. Finally, at the microscopic scale,a detailed dislocation study of samples deformed under confining pressure revealed the presenceof dislocation configurations never observed before in MAX phases, such as dislocation reactions,dislocation dipoles and out-of-basal plane dislocations. In the light of these new results, mechanicalproperties of MAX phases are discussed
Los estilos APA, Harvard, Vancouver, ISO, etc.
3

Johnson, Lars. "Nanoindentation in situ a Transmission Electron Microscope". Thesis, Linköping University, Department of Physics, Chemistry and Biology, 2007. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-8333.

Texto completo
Resumen

The technique of Nanoindentation in situ Transmission Electron Microscope has been implemented on a Philips CM20. Indentations have been performed on Si and Sapphire (α-Al2O3) cut from wafers; Cr/Sc multilayers and Ti3SiC2 thin films. Different sample geometries and preparation methods have been evaluated. Both conventional ion and Focused Ion Beam milling were used, with different ways of protecting the sample during milling. Observations were made of bending and fracture of samples, dislocation nucleation and dislocation movement. Basal slip was observed upon unloading in Sapphire. Dislocation movement constricted along the basal planes were observed in Ti3SiC2. Post indentation electron microscopy revealed kink formation in Ti3SiC2 and layer rotation and slip across layers in Cr/Sc multilayer stacks. Limitations of the technique are presented and discussed.

Los estilos APA, Harvard, Vancouver, ISO, etc.
4

Hummelgård, Magnus. "In-situ TEM Probing of Nanomaterials". Doctoral thesis, Mittuniversitetet, Institutionen för naturvetenskap, teknik och matematik, 2009. http://urn.kb.se/resolve?urn=urn:nbn:se:miun:diva-8998.

Texto completo
Resumen
Nanomaterials because of their small size, may have special properties unlikely to be seen in ordinary types of materials. Nanomaterials like nanotubes,nanowires and nanoparticles are best studied at the nanoscale, vital but also problematic. In this thesis we use a transmission electron microscope (TEM)combined with a scanning tunneling microscope probe. This system allows TEM images to be captured and recorded into a movie together with recordedelectrical data for real time analysis. Using this method we found that the electrical conductivity of molybdenumbased nanowires Mo6S3I6 can be improved by current induced transformation. This might be a general method of improving nanowires which is of high valueif the wires are to be used in electrical circuits or field emission devices. The bending modulus for these nanowires were also determined, by an electromechanical resonance method, to 4.9 GPa. The sintering phase of silver nanoparticles, used in electrical conductive ink for printing electrical circuits, were studied by the in-situ TEM probing method. We observed that percolation path ways are formed and that the dispersive agent of the particles can be pyrolysed into a net of carbon with characteristics similar to graphite. We also developed a method for decorating nanowires and nanotubes with gold nanoparticles. Nanowire particle composites are often used in assembling more complex devices (electronic circuits) or for linking to organic molecules (biosensor applications) and existing particle decoration methods are either difficult or with low yield. By in situ TEM probing we found that carbon nanocages can be grown onto these gold nanoparticles. The size of the gold nanoparticles is controllable an thus the size of the nanocages. These nanocages may be used in medicine- or hydrogen storage-applications.
Nanomaterial har givits stort intresse under det senaste årtiondet, detta på grund av deras unika egenskaper som gör att de i många hänseenden överträffar traditionella material. Egenskaperna beror till största del på storlek och därför är det nödvändigt att studera dessa material på nanonivå, något som är problematiskt. För sådana studier krävs ett instrument med tillräckligt hög upplösning på nanonivå samt ett system med en prob som möjligör selektion och karakterisering utav individuella byggstenar. I denna avhandling används ett transmissionselektronmikroskop (TEM) tillsammans med ett sveptunnelmikroskop (STM) där det senare används som prob. Systemet medger studier på nanonivå och karakterisering av enskilda byggstenar under realtids avbildning (in situ). Metoden medger en bättre överblick och hanterbarhet vid nanomanipulering än vad till exempel atomkraftmikroskopi medger. Piezodrivna probar kan även användas i svepelektronmikroskop men dessa medger inte samma upplösning som transmissionselektronmikroskopet. Nanotrådar av Mo6S3I6 är ett alternativt material till kolnanorör och överträffar dessa i form av löslighet i båda organiska såväl som polära lösningsmedel. De är enkla att syntetisera men deras elektriska konduktivitet är låg. Mo6S3I6 nanotrådar studerades med in situ TEM probing. Vi fann att genom att driva en tillräckligt hög elektrisk ström genom nanotråden så resulterade detta i en omvandling till en solid metallisk molybden nanotråd med en konduktivitet nära värdet för bulkmaterialet. Resultat är intressant då nanotrådar kan användas i t.ex. fältemission, men resultatet visar också på att det kan vara en generell metod för att förbättra nanotrådar överlag. På dessa nanotrådar har även en elektromekanisk resonans studie utförts där böjmodulen för materialet bestämdes till 4.9 GPa. Med in situ-TEM-probing metoden har även silvernanobläck studerats under en sintringsprocess. Studien visade att vid sintringen så bildas perkulativa vägar genom bläckets silvernanopartiklar samt att vid hög sinteringstemperatur förkolnades det lösningsmedel som silvernanopartiklarna är lösta i. Förkolningen av lösningsmedlet resulterade i ett kolnät med liknande egenskaper som för grafit. Förståelse utav sinteringsprocessen är nödvändig eftersom vid tryckning av elektriskt ledande banor på papper används sintring för att höja ledningsförmågan. Genom att växa nanopartiklar på nanotrådar förändras deras egenskaper och tillämpningar. Existerande metoder är endera komplicerade eller ger dåligt ut- byte. Ett enkelt recept för att växa guldnanopartiklar på kolnanorör och Mo6S3I6 nanotrådar har därför tagits fram. Dessa kolnanorör och nanotrådar har sedan studerats med in-situ-TEM-probing metoden som visade att utanpå dessa guldnanopartiklar kan burar av kol skapas. Eftersom partiklarnas storlek kan kontrolleras kan även kolnanoburarnas storlek kontrolleras. Burarna har användningsområden t.ex. inom medicin och vid lagring av vätgas.
The thesis covers six scientific papers
Los estilos APA, Harvard, Vancouver, ISO, etc.
5

Barnoush, Afrooz. "Hydrogen embrittlement, revisited by in situ electrochemical nanoindentation". Aachen Shaker, 2007. http://d-nb.info/992479851/04.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
6

Sylvain, Wilgens. "Étude de la plasticité du monocristal de phase MAX par déformation aux petites échelles". Thesis, Poitiers, 2016. http://www.theses.fr/2016POIT2307/document.

Texto completo
Resumen
L'objectif de cette thèse est l'étude de la déformation, à l'échelle microscopique, de la phase MAX Ti2AlN, synthétisée par métallurgie des poudres. Ce travail se divise en trois parties : une première dans laquelle l'accent a été mis sur l'hystérèse mécanique des phases MAX via des essais cyclés, en nanoindentation sphérique et compression ex-situ de micro-piliers, sur des grains d'orientations différentes déterminées par l'EBSD. Dans la deuxième nous nous sommes intéressés à la déformation de micropiliers via des essais de compression cyclés in-situ couplés à la micro-diffraction Laue. L'objectif a été d'analyser les taches diffraction au cours de la déformation du pilier afin de mettre en évidence les mécanismes de déformation élémentaires mis en jeu et d'observer les structures finales via des images MEB post-mortem des piliers. Enfin, une dernière dans laquelle l'objectif a été l'étude des mécanismes de déformation en température à l'échelle microscopique via des essais de nano-indentation allant jusqu'à 800°C. La caractérisation des lignes de glissement en surface et des configurations microstructurales sous l'empreinte a été réalisée par AFM et MET respectivement. Toutes les données recueillies par ces divers essais aux petites échelles, ont permis d'affiner notre compréhension des mécanismes de déformation du monocristal de phase MAX, notamment vis à vis des modèles usuellement proposés dans la littérature
The thesis's goal is to study the deformation, at microscopic scale, of the MAX phase Ti2AlN synthesized by powder metallurgy. This work is divided into three parts: in the first part, the interest has been put on the hysteretic behavior of the MAX phases via cyclic mechanical solicitations, during spherical indentation tests and ex-situ compression of micro-pillars, on differently orientated grains beforehand determined by EBSD. In the second part, we were interested into the micro-pillar's deformation via insitu cyclic compression tests coupled with Laue micro-diffraction. The goal was to analyse the evolution diffraction lines during the pillar's deformation in order to highlight the elementary deformation mechanisms and to observe the finale structures via the post-mortem SEM imaging of the pillars. Finally, a last part was devoted to study the deformation mechanisms in temperature at microscopic scale via nano-indentation tests up to 800°C. The characterization of the slip lines on the surface has been revealed by AFM and that of t he microstructural configurations (dislocations) under the indent has been done by TEM. All data collected by these various tests at the small scales have refined our understanding of the deformation mechanisms of crystal MAX phase, particularly with respect to the models usually proposed in the literature
Los estilos APA, Harvard, Vancouver, ISO, etc.
7

Barnoush, Afrooz [Verfasser]. "Hydrogen embrittlement, revisited by in situ electrochemical nanoindentation / Afrooz Barnoush". Aachen : Shaker, 2009. http://d-nb.info/1161310207/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
8

Hajduček, Jan. "Zobrazování metamagnetických tenkých vrstev pomocí TEM". Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2021. http://www.nusl.cz/ntk/nusl-443233.

Texto completo
Resumen
Komplexní magnetické materiály v nanoměřítku mají své nezastupitelné místo v moderních zařízeních, jako jsou digitální paměti nebo senzory. Moderní technologické procesy vyžadují porozumění a možnost kontroly moderních magnetických materiálů až na atomární úrovni. Jednou z možných cest je magnetická analýza za použití transmisní elektronové mikroskopie (TEM), která je unikátní díky možnosti zobrazování až v subatomárním měřítku. Tato práce popisuje možnosti zobrazování metamagnetických materiálů metodou TEM. Tyto materiály se vyznačují možností stabilizace více magnetických uspořádání najednou za daných vnějších podmínek. Modelovým systémem pro popis zobrazovacích možností metody TEM byly zvoleny tenké vrstvy metamagnetické slitiny FeRh. Tento materiál prochází při zahřívání fázovou přeměnou z antiferomagnetické do feromagnetické fáze. Podrobně jsou rozebrány procesy výroby vzorků, což je zásadní pro úspěšnou TEM analýzu. Pro magnetické zobrazování vzorků v TEMu je využita technika diferenciálního fázového kontrastu (DPC), umožňující přímé mapování rozložení magnetické indukce ve vzorku. Důsledně je diskutován vznik signálu v DPC, což je nezbytné pro porozumění a analýzu výsledných dat. FeRh vrstvy jsou podrobeny analýze struktury, chemického složení a především magnetických vlastností obou magnetických fází. Závěrem je představen proces přímého ohřevu metamagnetických vrstev v TEMu.
Los estilos APA, Harvard, Vancouver, ISO, etc.
9

Vineis, Christopher J. (Christopher Joseph) 1974. "Characterization of OMVPE-grown GaSb-based epilayers using in situ reflectance and ex situ TEM". Thesis, Massachusetts Institute of Technology, 2001. http://hdl.handle.net/1721.1/8452.

Texto completo
Resumen
Thesis (Ph.D.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 2001.
Includes bibliographical references (leaves 227-238).
The focus of this thesis was to investigate and characterize GaSb, GaInAsSb, and AlGaAsSb epilayers grown by organometallic vapor phase epitaxy (OMVPE). These epilayers were principally characterized using in situ spectral reflectance and ex situ transmission electron microscopy (TEM). An in situ spectral (380-1100 nm) reflectance monitoring system was designed and fitted to the OMVPE reactor. It was determined that longer wavelengths are more useful for quantitative growth rate analysis, while shorter wavelengths are more sensitive to the GaSb substrate oxide desorption process. It was also determined that the GaInAsSb and AlGaAsSb alloy compositions could be determined accurately using in situ reflectance ratios. Use of the in situ reflectance monitor to efficiently perform necessary reactor/growth calibrations was also demonstrated. Analytic functions were used to model the refractive indices of GaSb, AlGaAsSb, and GaInAsSb. Specifically, Adachi's Model Dielectric Function [1, 2] was curve-fit to data for GaSb between 400 and 1000 nm, and fourth-order polynomials were fit to data for GaSb and GaInAsSb between 1 and 3 gnm. A linear interpolation of binary functions was used to generate a refractive index model for AlGaAsSb between 1 and 3 m as a function of Al fraction. These models were helpful in interpreting in situ reflectance data, and also in designing distributed Bragg reflectors. Phase separation in GaInAsSb was studied using TEM. A wide range of microstructures was observed, from nearly homogeneous to strongly phase separated.
(cont.) It was seen that in phase separated samples, the composition modulations typically created and coupled to morphological perturbations in the surface. One interesting manifestation of the phase separation was the spontaneous formation of a natural superlattice (period typically 10-30 nm) throughout the epilayer. This superlattice had two variants: one parallel to the growth surface, and one tilted with respect to the growth surface. It was discovered that the tilted superlattice was coupled to surface to relieve surface strain associated with the superlattice ...
by Christopher J. Vineis.
Ph.D.
Los estilos APA, Harvard, Vancouver, ISO, etc.
10

Jia, Xiaoting. "In-situ TEM study of carbon nanomaterials and thermoelectric nanomaterials". Thesis, Massachusetts Institute of Technology, 2011. http://hdl.handle.net/1721.1/69666.

Texto completo
Resumen
Thesis (Ph. D.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 2011.
This electronic version was submitted by the student author. The certified thesis is available in the Institute Archives and Special Collections.
Cataloged from PDF version of thesis.
Includes bibliographical references (p. 103-112).
Graphene nanoribbons (GNRs) are quasi one dimensional structures which have unique transport properties, and have a potential to open a bandgap at small ribbon widths. They have been extensively studied in recent years due to their high potential for future electronic and spintronic device applications. The edge structures - including the edge roughness and chirality - dramatically affect the transport, electronic, and magnetic properties of GNRs, and are of the critical importance. We have developed an efficient way of modifying the edges structures, to produce atomically smooth zigzag and armchair edges by using insitu TEM with a controlled bias. This work provides us with many opportunities for both fundamental studies and for future applications. I also report the use of either furnace heating or Joule heating to pacify the exposed graphene edges by loop formation in the graphitic nanoribbons. The edge energy minimization process involves the formation of loops between adjacent graphene layers. An estimation of the temperature during in-situ Joule heating is also reported based on the melting and evaporation of Pt nanoparticles. In this thesis work, I have also investigated the morphological and electronic properties of GNRs grown by chemical vapor deposition. Our results suggest that the GNRs have a surprisingly high crystallinity and a clean surface. Both folded and open edges are observed in GNRs. Atomic resolution scanning tunneling microscopy (STM) images were obtained on the folded layer and the bottom layer of the GNR, which enables clear identification of the chirality for both layers. We have also studied the electronic properties of the GNRs using low temperature scanning tunneling spectroscopy (STS). Our findings suggest that edges states exist at GNR edges which are dependent on the chiral angles of the GNRs.
by Xiaoting Jia.
Ph.D.
Los estilos APA, Harvard, Vancouver, ISO, etc.
11

Issa, Inas. "In situ TEM nanocompression and mechanical analysis of ceramic nanoparticles". Thesis, Lyon, 2016. http://www.theses.fr/2016LYSEI008/document.

Texto completo
Resumen
Dans cette étude, nous proposons d’utiliser la compression in situ dans le MET afin de caractériser les propriétés mécaniques de nanoparticules céramiques dont la taille caractéristique est de l’ordre de quelques dizaines de nanomètres. Nous appliquerons cette méthode à des nanocubes monocristallins de MgO, une céramique modèle dont la plasticité est bien connue dans le matériau massif. Les essais de nanocompression montrent que les nanocubes de MgO se déforment de façon homogène jusqu’à de grandes déformations (>50%) sans fissure apparente. L’analyse des résultats est assistée par des méthodes de corrélation d’images numériques et simulations de type dynamique moléculaire. Le mécanisme de déformation et l'effet de taille sur la limite élastique sont identifiés. Dans une deuxième partie de la thèse, nous présentons une étude sur des nanoparticules d’alumine de transition compactée en CED (Cellule à Enclumes en Diamant) à température ambiante, sous plusieurs pressions (5 GPa, 15 GPa et 20 GPa). Des lames minces préparées par FIB ont été étudiées en MET. Des images HRTEM montrent une texture cristallographique qui devient plus importante à des pressions plus élevées. Une orientation cristallographique préférentielle est observée, avec les plans {220} de la phase gamma de l’alumine la plupart du temps parallèles à la surface de contact avec une particule voisine. Ce comportement mécanique est cohérent avec un système de glissement, connu pour les structures spinelles. Une corrélation de ce comportement avec les tests in situ MET réalisés sur des nanoparticules similaires, par Emilie Calvié lors de sa thèse, est présentée. Enfin, des clichés de diffraction de type Debye Scherrer sont réalisés sur ces lames minces de nanoparticules d’alumine de transition compactées en CED à différentes pressions. L’analyse quantitative de ces clichés montre une transformation de phase de ces nanoparticules d’alumine de phase gamma en phase delta, de manière croissante avec la pression
In this study, we propose an innovative mechanical observation protocol of ceramics nanoparticles in the 100nm size range. This Protocol consists of in situ TEM nanocompression tests of isolated nanoparticles. Load–real displacements curves, obtained by Digital Image Correlation, are analyzed and these analyses are correlated with Molecular Dynamics simulations. By this protocol a constitutive law with its mechanical parameters (Young modulus, Yield stress...) of the studied material at the nano-scale can be obtained. In situ TEM nano-compression tests on magnesium oxide nanocubes are performed. Magnesium oxide is a model material and its plasticity is very well known at bulk. The MgO nanocubes show large plastic deformation, more than 50% of plastic strain without any fracture. The TEM results are correlated to MD simulations and the deformation mechanism can be identified.The size effect and the electron beam effect on the yield strength are investigated. In a second part of the dissertation, we present a study on transition alumina nanoparticles compacted in a Diamond Anvil Cell at different uniaxial pressures. Thin Foils of these compacted nanoparticles are prepared by FIB for HRTEM Observations. Their analysis reveals the plastic deformation of the nanoparticles. The crystallographic texture observed inthese compacted nanoparticles in DAC shows a preferred orientation of the {110} lattice planes, orientated perpendicular to the compression direction. This is compatible with the slip system. This argument was reinforced with a preferred orientation of slip bands observed during in situ TEM nano-compression tests. Moreover, electron diffraction patterns (Debye Scherrer) analysis on these compacted transition alumina nanoparticles reveals the decrease of the presence of gamma-alumina and the increase of delta-alumina with increasing pressure. This reveals the phase transformation with increasing pressure from gamma to delta* alumina
Los estilos APA, Harvard, Vancouver, ISO, etc.
12

Chang, Huai-Ning. "Electrostatic Feedback for Mems Sensor : Development of in situ TEM instrumentation". Thesis, Linköping University, The Department of Physics, Chemistry and Biology, 2008. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-11649.

Texto completo
Resumen

This thesis work is about further developing an existing capacitive MEMS sensor for in situ TEM nanoindentation developed by Nanofactory Instrument AB. Today, this sensor uses a parallel plate capacitor suspended by springs to measure the applied force. The forces are in the micro Newton range. One major issue using with this measurement technique is that the tip mounted on one of the sensor plates can move out of the TEM image when a force is applied. In order to improve the measurement technique electrostatic feedback has been investigated. The sensor’s electrostatic properties have been evaluated using Capacitance-Voltage measurements and a white light interferometer has been used to directly measure the displacement of the sensor with varying voltage. Investigation of the sensor is described with analytical models with detailed treatment of the capacitive response as function of electrostatic actuation. The model has been tested and refined by using experimental data. The model showed the existence of a serial capacitor in the sensor. Moreover, a feedback loop was tested, by using small beads as load and by manually adjusting the voltage. With the success of controlling the feedback loop manually, it is shown that the idea is feasible, but some modifications and improvements are needed to perform it more smoothly.

Los estilos APA, Harvard, Vancouver, ISO, etc.
13

Qu, Weiguo. "In-situ TEM investigation of the phase transitions in perovskite ferroelectrics". [Ames, Iowa : Iowa State University], 2008.

Buscar texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
14

Knoop, Ludvig de. "Development of quantitative in situ transmission electron microscopy for nanoindentation and cold-field emission". Toulouse 3, 2014. http://thesesups.ups-tlse.fr/3041/.

Texto completo
Resumen
Cette thèse porte sur le développement d'analyse quantitative d'expérience in situ de microscopie électronique en transmission (MET). Nous avons utilisé un porte objet spécial, qui combine les fonctions de polarisation électrique locale et tests de micro-mécanique. La méthode des éléments finis (MEF) a été mise en œuvre afin de comparer les résultats issus de la modélisation avec les résultats expérimentaux. En plus des techniques d'imagerie classique, l'holographie électronique a été employée pour mesurer des champs électriques et de déformation. La première partie traite de l'émission de champ d'une nanopointe faite d'un cône de carbone (CCnT). Ce nouveau type de matériaux pourrait remplacer les pointes de tungstène qui sont utilisés dans les canons d'électrons les plus avancés. Quand un champ électrique suffisamment fort est appliqué au CCnT, les électrons peuvent passer à travers la barrière d'énergie avec le vide par effet tunnel, ce qui correspond au phénomène d'émission de champ. En combinant holographie électronique avec les simulations MEF, une valeur quantitative du champ électrique local a été obtenue pour l'émission (2,5 V/nm). En faisant appel aux équations de Fowler-Nordheim, une valeur de la fonction de travail de sortie du CCnT est déterminée (4,8±0,3 eV). Nous avons également mesuré les charges sur le CCnT, avant et après le début de l'émission de champ. La deuxième partie porte sur la déformation plastique d'un film mince d'Al pour tester les interactions des dislocation - interface. Une dislocation à proximité d'une interface avec un matériau plus rigide doit être repoussée par celle-ci. Ici, nous constatons que les dislocations qui vont vers l'interface oxydée sont absorbées par cette interface rigide, même à température ambiante. La contrainte locale est déterminée par une combinaison de mesures de forces par le capteur et de calculs MEF. Enfin, des résultats préliminaires de combiner indentation in situ et holographie électronique en champ sombre sont présentés
This thesis has focused on the development of quantitative in situ transmission electron microscopy (TEM) techniques. We have used a special nano-probe sample holder, which allows local electrical biasing and micro-mechanical testing. The finite element method (FEM) was used to compare models with the experimental results. In addition to conventional imaging techniques, electron holography has been used to measure electric fields and strains. The first part addresses cold-field emission from a carbon cone nanotip (CCnT). This novel type of carbon structure may present an alternative to W-based cold-field emission sources, which are used in the most advanced electron guns today. When a sufficiently strong electric field is applied to the CCnT, electrons can tunnel through the energy barrier with the vacuum, which corresponds to the phenomenon of cold-field emission. Using electron holography and FEM, a quantified value of the local electric field at the onset of field emission was found (2. 5 V/nm). Combining this with one of the Fowler-Nordheim equations, the exit work function of the CCnT was determined to be 4. 8±0. 3 eV. The number of charges on the CCnT before and after the onset of field emission was also measured. The second part focuses on the plastic deformation of Al thin films to test dislocation-interface interactions. A dislocation close to an interface with a stiffer material should be repelled by it. Here, we find to the contrary that dislocations moving towards the oxidized interface are absorbed, even at room temperature. The stress was derived from a combination of load-cell measurements and FEM calculations. Finally, preliminary experiments to combine in situ indentation and dark-field electron holography are reported
Los estilos APA, Harvard, Vancouver, ISO, etc.
15

Fawey, Mohammed [Verfasser], Horst [Akademischer Betreuer] Hahn y Hans-Joachim [Akademischer Betreuer] Kleebe. "In situ and Ex situ TEM Studies of Fluoride Ion Batteries / Mohammed Fawey ; Horst Hahn, Hans-Joachim Kleebe". Darmstadt : Universitäts- und Landesbibliothek Darmstadt, 2017. http://d-nb.info/114448426X/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
16

Fawey, Mohammed H. [Verfasser], Horst [Akademischer Betreuer] Hahn y Hans-Joachim [Akademischer Betreuer] Kleebe. "In situ and Ex situ TEM Studies of Fluoride Ion Batteries / Mohammed Fawey ; Horst Hahn, Hans-Joachim Kleebe". Darmstadt : Universitäts- und Landesbibliothek Darmstadt, 2017. http://nbn-resolving.de/urn:nbn:de:tuda-tuprints-69330.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
17

Schilling, Sibylle. "Liquid in situ analytical TEM : technique development and applications to austenitic stainless steel". Thesis, University of Manchester, 2017. https://www.research.manchester.ac.uk/portal/en/theses/liquid-in-situ-analytical-tem-technique-development-and-applications-to-austenitic-stainless-steel(fd490551-7d7a-4b2e-9b1f-917b5f8165b3).html.

Texto completo
Resumen
Environmentally-assisted cracking (EAC) phenomena affect the in-service behaviour of austenitic stainless steels in nuclear power plants. EAC includes such degradation phenomena as Stress Corrosion Cracking (SCC) and Corrosion Fatigue (CF). Factors affecting EAC include the material type, microstructure, environment, and stress. This is an important degradation issue for both current and Gen III+ light water reactors, particularly as nuclear power plant lifetimes are extended ( > 60 years). Thus, it is important to understand the behaviour of the alloys used in light water reactors, and phenomena such as SCC to avoid failures. Although there is no agreement on the mechanism(s) of SCC, the importance of localized electrochemical reactions at the material surface is widely recognised. Considerable research has been performed on SCC and CF crack growth, but the initiation phenomena are not fully understood. In this project, novel in situ analytical TEM techniques have been developed and applied to explore localised reactions in Type 304 austenitic stainless steel. In situ transmission electron microscopy has become an increasingly important and dynamic research area in materials science with the advent of unique microscope platforms and a range of specialized in situ specimen holders. In metals research, the ability to image and perform X-ray energy dispersive spectroscopy (XED) analyses of metals in liquids are particularly important for detailed study of the metal-environment interactions with specific microstructural features. To further facilitate such studies a special hybrid specimen preparation technique involving electropolishing and FIB extraction has been developed in this thesis to enable metal specimens to be examined in the liquid cell TEM specimen holder using both distilled H2O and H2SO4 solutions. Furthermore, a novel electrode configuration has been designed to permit the localized electrochemical measurement of electron-transparent specimens in the TEM. These novel approaches have been benchmarked by extensive ex situ experiments, including both conventional electrochemical measurements and microcell measurements. The results are discussed in terms of validation of in situ test data as well as the role of the electron beam in the experiments. In situ liquid cell TEM experiments have also explored the localized dissolution of MnS inclusions in H2O, and correlated the behaviour with ex situ experiments. Based on the research performed in this thesis, in situ liquid cell and in situ electrochemical cell experiments can be used to study nanoscale reactions pertaining to corrosion and localized dissolution leading to "precursor" events for subsequent EAC phenomena.
Los estilos APA, Harvard, Vancouver, ISO, etc.
18

Eva, Hasenhuetl. "Orientation Dependence of Hardening and Microstructural Evolution in Ion-irradiated Tungsten Single Crystal". 京都大学 (Kyoto University), 2017. http://hdl.handle.net/2433/225709.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
19

Melinte, Georgian. "Advanced 3D and in-situ TEM approaches applied to carbon-based and zeolitic nanomaterials". Thesis, Strasbourg, 2015. http://www.theses.fr/2015STRAE009/document.

Texto completo
Resumen
Dans le cadre de cette thèse, des techniques avancées de Microscopie électronique à transmission (MET)ont été utilisées dans le but de caractériser et de fabriquer de nouveaux nanomatériaux pour des applications dans les domaines de la nanoélectronique et de la catalyse. Trois types de matériaux fonctionnalisés sont étudiés: le graphène multifeuillets (FLG– Few-Layer Graphene) avec des nanomotifs,des nanotubes de carbone (CNTs - Carbon Nanotubes en anglais) et des zéolithes mésoporeux. La formation de nanomotifs de tranchées et de tunnels sur des flocons de FLG à l’aide de nanoparticules(NPs) de fer est étudiée dans une approche qui combine la tomographie électronique et la MET environnementale. Le rôle des facettes de la nanoparticule et des paramètres topographiques de FLG a été déterminé du point de vue quantitatif, ce qui a mené à la mise en évidence du mécanisme de formation des nanomotifs de tranchées et de tunnels. Le transfert de nanoparticules à base de métal entre deux nanostructures de carbone a été également étudié, en temps réel, en employant un porte-échantillon MET couplé avec un dispositif STM (Scanning Tunneling Microscope en anglais). Le protocole de contrôle du transfert des nanoparticules, les transformations chimiques et structurales subies par celles-ci, le mécanisme de croissance de nouvelles nanoparticules et d’autres phénomènes liés à ces effets ont été étudiés avec attention. La dernière partie de la thèse est centrée sur l’étude de la tomographie électronique à faible dose de la porosité induite dans deux classes de zéolithes, ZSM-5 et zéolithe Y, en utilisant un traitement chimique novateur à base de fluor
In this thesis, advanced Transmission Electron Microscopy (TEM) techniques are used to characterize and fabricate new nanomaterials with applications in nanoelectronics and catalysis. Three types of functionalized materials are investigated: nanopatterned few-layer graphene (FLG), carbon nanotubes(CNTs) and mesoporous zeolites. The nanopatterning process of FLG flakes by iron nanoparticles (NPs) is studied using an approach combining electron tomography (ET) and environmental TEM. The role of the nanoparticle faceting and of the FLG topographic parameters has been quantitatively determined leading to the first determination of the operating mechanism of the patterning process. The mass transfer of metallic-based NPs between two carbon nanostructures was studied as well in real-time by using a TEMSTMholder. The protocol of controlling the mass transfer, the chemical and structural transformations of the NPs, the growth mechanism of the new NPs and other related phenomena were carefully investigated.The last part deals with the low-dose ET investigation of the porosity induced in two classes of zeolites,ZSM-5 and zeolite Y, by an innovative fluoride-based chemical treatment
Los estilos APA, Harvard, Vancouver, ISO, etc.
20

Amer, Madyan. "Carbure de silicium 4H et 3C : microstructures de déformation dans le domaine fragile". Thesis, Poitiers, 2012. http://www.theses.fr/2012POIT2260/document.

Texto completo
Resumen
L’objectif de cette thèse est d’étudier le comportement plastique du carbure de silicium dans le domaine fragile. A cette fin, des essais de déformation par micro et nanoindentation ont été réalisés sur des échantillons monocristallins de SiC (4H et 3C). Des couches homoépitaxiées de 4H-SiC de différents dopages électroniques ont été étudiées. Ces couches présentent des caractéristiques mécaniques différentes en fonction du dopage : le dopage de type p durcit le matériau par rapport au dopage de type n ou au matériau intrinsèque. De plus, l'analyse des courbes charge-enfoncement obtenue en nanoindentation montre que la nucléation des dislocations est plus difficile lorsque le matériau est dopé de type p par rapport au matériau dopé n ou intrinsèque. Ceci est confirmé par les microstructures de déformation observées en Microscopie Electronique en Transmission (MET). Les observations par MET montrent que les dislocations introduites à l'ambiante autour des empreintes sont parfaites et glissent dans les plans {0001} dans le 4H-SiC et dans les plans {111} dans le 3C-SiC. Elles sont orientées principalement le long de la direction vis. Les sites de nanoindentation à température ambiante des couches 4H homoepitaxiées ont été particulièrement étudiés. On met en évidence que les sites de nucléation des dislocations sont vraisemblablement situés dans les plans {1100}, les dislocations se développant par la suite dans le plan basal. La nature des cœurs des dislocations parfaites a été déterminée par la technique LACBED. Ces dislocations parfaites ont un cœur silicium en mode shuffle. Un changement de mécanisme de plasticité est observé par MET pour les échantillons indentés 800
The aim of this thesis is to study the plastic behaviour of silicon carbide in the brittle domain. For this purpose micro and nanoindentation deformation tests were performed on single crystal specimens of SiC (4H and 3C). Homoepitaxial layers of 4H-SiC with different doping have been studied. These layers show different mechanical characteristics as a function of doping: p-type doping hardens the material as compared to n-type doping or intrinsic material. In addition, load-penetration depthcurves show that the nucleation of dislocations is more difficult in p-doped material as compared to intrinsic or n-doped material. This is confirmed by deformation microstructures observations using Transmission Electron Microscope (TEM). TEM observations show that dislocations introduced around the imprints at room temperature are perfect dislocations gliding in the {0001} plane in 4H-SiC and in the {111} plane in 3C-SiC. They are mostly screw oriented. Room temperature nanoidentation imprints of4H homoepitaxied layers have been extensively studied. It is evidenced that dislocation nucleation sites are likely to be located in {1100} planes and that dislocations bow out subsequently in the basal plane. The core nature of perfect dislocations has been determined using the LACBED technique. Those perfect dislocations have a silicon core in the shuffle mode. TEM observations on specimens indented at 800ºC indicate a change in plastic deformation mechanism. At this temperature, partial dislocations with large stacking faults are observed
Los estilos APA, Harvard, Vancouver, ISO, etc.
21

Comby, Dassonneville Solène. "Développement et application d'un nanoindenteur in situ MEB couplé à des mesures électriques". Thesis, Université Grenoble Alpes (ComUE), 2018. http://www.theses.fr/2018GREAI047/document.

Texto completo
Resumen
L’essor de la demande actuelle pour des matériaux architecturés, en microélectronique par exemple, ou pour des matériaux de structure, nécessite le développement d’outils de caractérisation toujours plus performants. Dans cette optique, un instrument de caractérisation multifonctionnel basé sur un couplage mécanique / électrique, a été développé au laboratoire SIMaP. Le cœur de ce dispositif est un nanoindenteur in situ FEG-SEM (Field Emission Gun Scanning Electron Microscope) couplé à des mesures électriques. Ce travail est porté par trois principales motivations: (1) L’étude du comportement mécanique d’objets petites échelles, (2) L’apport des données électriques à l’analyse quantitative du comportement mécanique pendant l’indentation, en particulier pour obtenir une meilleur estimation de l’aire de contact, (3) L’étude locale des propriétés électroniques d’empilements de films minces. L’intégration in situ SEM a été validée et permet un positionnement des indents avec une précision meilleure que 100 nm, autorisant ainsi l’étude des propriétés mécaniques à l’échelle submicrométrique. La rapidité des essais permet également des mesures statistiques. Des caractérisations mécaniques ont été menées aussi bien sur des échantillons composites massifs que sur des ilots d’or submicrométriques. Pour ce dernier cas, malgré la nature stochastique de leur comportement mécanique, une loi déterministe a pu être extraite des données mécaniques. Des mesures 3D-BCDI (Bragg Coherent Diffraction Imaging) au synchrotron ont été réalisées sur certains ilots avant et après chargement mécanique, révélant une germination de dislocations avant l’avalanche de grandes déformations plastiques. En parallèle de cette étude, des mesures électriques ont été réalisées pendant l’indentation de divers échantillons. Des mesures de nanoindentation résistive ont ainsi été effectuées sur des métaux nobles (Au) ou recouverts de leur oxyde natif (Cu, Al), soit à l’état de monocristal massif ou de film polycristallin. Les résultats quantitatifs soulignent l’importance de la présence d’une couche d’oxyde sur la réponse électrique. En présence d’un oxyde, l’interface pointe / échantillon semble être le lieu d’importantes réactions électrochimiques. En l’absence d’oxyde, la résistance mesurée peut être entièrement décrite par un modèle analytique. Dans ce cas, l’aire de contact électrique peut être prédite à partir des mesures de résistance. Enfin, des mesures capacitives ont été réalisées sur des structures MOS avec différentes épaisseurs d’oxyde. Les résultats expérimentaux sont parfaitement décrits par un modèle analytique, ce qui ouvre la voie à des mesures locales de permittivité diélectrique sous contrainte mécanique
The increasing demand for multifunctional materials has become a recurrent challenge for a wide panel of application fields such as microelectronics and structural applications. Within the frame of this project, a multifunctional characterisation set-up has been developed at SIMaP lab, mainly based on the electrical / mechanical coupling. The heart of this device is an in situ FEG-SEM (Field Emission Gun Scanning Electron Microscope) nanoindenter coupled with an electrical measurement apparatus. This work has threefold objectives: (1) The investigation of mechanical behavior of small scale systems, (2) The input of electrical data to the quantitative analysis of mechanical behavior during indentation, in particular to obtain a better estimation of the contact area (3) The local study of electronic properties of thin film stacks. SEM integration of the device has been validated and indent positioning with a precision better than 100 nm is successfully obtained. This performance allows the studies of mechanical properties at submicrometric length scale, with a high throughput allowing statistical measurements. Various bulk composite materials have been characterized as well as submicrometric gold islands on sapphire. In the latter case, despite the stochastic nature of their mechanical behavior, a deterministic law has been extracted. 3D-BCDI (Bragg Coherent Diffraction Imaging) experiments have been performed on a few islands at synchrotron facility to investigate the crystal state before and after mechanical loading. These experiments reveal initial dislocation nucleation prior to large deformation bursts. In parallel to this study, electrical measurements have been performed during indentation on various cases. Resistive-nanoindentations have been performed on noble metals (Au) and natively oxidized metals (Cu, Al), either as bulk single crystals or as polycrystalline thin films. Qualitative results emphasize the importance of the oxide layer on the electrical response. In the presence of an oxide layer, strong electrochemical reactions seem to occur at the tip-to-sample interface. When no oxide is involved, the measured resistance can be fully described by an analytical model and the computed electrical contact area is successfully validated with residual areas measurements. Finally, capacitive measurements have been performed on MOS structures with various oxide thicknesses. Experimental results have been well described by analytical modelling, which paves the way for quantitative local dielectric permittivity measurements under mechanical loading
Los estilos APA, Harvard, Vancouver, ISO, etc.
22

Pawley, C. "The use of in-situ ion-irradiation/TEM techniques to study radiation damage in SiC". Thesis, University of Salford, 2014. http://usir.salford.ac.uk/32489/.

Texto completo
Resumen
SiC is a material currently under consideration to be used in future generations of fission and fusion reactors where it will be subjected to high temperatures and significant fluxes of energetic neutrons. The work reported in this thesis aims to answer some outstanding issues of the behaviour of SiC at high temperature during irradiation by high-energy neutrons in combination with a build-up of helium (from both transmutation reactions and by direct implantation). These processes have been simulated by in-situ ion-irradiation / TEM at the MIAMI and JANNuS facilities. This thesis contains the results of experiments which investigated the nucleation and growth of helium bubbles in SiC and the behaviour of these helium bubbles under high energy heavy ion-irradiation. Our conclusions are that helium bubbles in SiC are extremely stable at high temperatures and during high-energy ion-irradiation. However, we have discovered that there is a significant effect on the bubbles attributable to either electron beam irradiation alone or the synergistic effect of the electron beam and ionirradiation which causes helium bubbles to shrink.
Los estilos APA, Harvard, Vancouver, ISO, etc.
23

Ronge, Emanuel [Verfasser]. "In-Situ Environmental TEM Studies of Electro- and Photo-Electrochemical Systems for Water Splitting / Emanuel Ronge". Göttingen : Niedersächsische Staats- und Universitätsbibliothek Göttingen, 2021. http://d-nb.info/1228364729/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
24

Berthier, Rémy. "Development of characterization methods for in situ annealing and biasing of semiconductor devices in the TEM". Thesis, Université Grenoble Alpes (ComUE), 2018. http://www.theses.fr/2018GREAY014/document.

Texto completo
Resumen
Dans cette thèse, nous abordons les défis rencontrés lors de la caractérisation des mémoires non volatiles par microscopie en transmission in situ. Les innovations récentes menées sur les porte-objets de TEM in situ basés sur l'utilisation de puces en silicium apportent de grands avantages comparée aux précédents modèles. Cependant, cette technique reste complexe et les expériences de MET in situ sont difficiles à mener à terme. Ce manuscrit tente d'apporter de nouvelles solutions pour permettre l'observation à l'échelle atomique pendant le recuit, ou la polarisation d'un échantillon dans le MET. Ce projet a été mené à travers plusieurs améliorations effectuées au cours des différentes étapes des expériences de MET in situ. Cette thèse se focalise plus particulièrement sur les problèmes rencontrés lors de la polarisation de dispositifs de mémoires résistives de taille nanométrique. Ces travaux furent conduits à travers une étude des instruments utilisés, le développement de nouvelles méthodes de préparation d'échantillons, et une analyse de l'impact de l'imagerie électronique sur le fonctionnement d'un dispositif dans le MET.Tout d’abord, une nouvelle méthode est développée spécifiquement pour les expériences de MET in situ en température. Grâce à ces développements, la cristallisation de mémoires à changement de phase en GeTe est observée en temps réel. Ces résultats ont notamment permis d'obtenir des informations utiles pour le développement de mémoires à changement de phase de type chalcogénure. Ensuite, de nouvelles puces en silicium dédiées à la polarisation in situ sont développées et produites. Une étude est ensuite menée sur la préparation d'échantillons par FIB afin d'améliorer la qualité des contacts électriques pour la polarisation in situ, ainsi que la technique de préparation elle-même. La qualité de cette méthode est ensuite démontrée à travers des mesures quantitatives obtenues pendant la polarisation in situ d'un échantillon de référence de type jonction PN. Ces développements sont ensuite appliqués afin d’observer des dispositifs de mémoires résistives de type CBRAM en fonctionnement dans le microscope électronique en transmission. Ces résultats ont permis d'apporter de nouvelles informations sur les mécanismes de fonctionnement des mémoires résistives, ainsi que sur la technique de polarisation in situ
In this work, we address the current challenges encountered during in situ Transmission Electron Microscopy characterization of emerging non volatile data storage technologies. Recent innovation on in situ TEM holders based on silicon micro chips have led to great improvements compared to previous technologies. Still, in situ is a particularly complicated technique and experiments are extremely difficult to implement. This work provides new solutions to perform live observations at the atomic scale during both heating and biasing of a specimen inside the TEM. This was made possible through several improvements performed at different stages of the in situ TEM experiments. The main focus of this PhD concerned the issues faced during in situ biasing of a nanometer size resistive memory device. This was made possible through hardware investigation, sample preparation method developments, and in situ biasing TEM experiments.First, a new sample preparation method has been developed specifically to perform in situ heating experiments. Through this work, live crystallization of a GeTe phase change Memory Material is observed in the TEM. This allowed to obtain valuable information for the development of chalcogenide based Phase Change Resistive Memories. Then, new chips dedicated to in situ biasing experiments have been developed and manufactured. The FIB sample preparation is studied in order to improve electrical operation in the TEM. Quantitative TEM measurements are then performed on a reference PN junction to demonstrate the capabilities of this new in situ biasing experimental setup. By implementing these improvements performed on the TEM in situ biasing technique, results are obtained during live operation of a Conductive Bridge Resistive Memory device. This allowed to present new information on the resistive memories functioning mechanisms, as well as the in situ TEM characterization technique itself
Los estilos APA, Harvard, Vancouver, ISO, etc.
25

Boniface, Maxime. "Suivi à l'échelle nanométrique de l'évolution d'une électrode de silicium dans un accumulateur Li-ion par STEM-EELS". Thesis, Université Grenoble Alpes (ComUE), 2017. http://www.theses.fr/2017GREAY051/document.

Texto completo
Resumen
L’accroissement des performances des accumulateurs Li-ion sur les 25 dernières années découle principalement de l’optimisation de leurs composants inactifs. Aujourd’hui, l’urgence environnementale impose de développer de nouveaux matériaux actifs d’électrode pour proposer la prochaine génération d’accumulateur qui participera à la transition énergétique. A cet effet, le silicium pourrait avantageusement remplacer le graphite des électrodes négatives à moyen terme. Cependant la rétention de capacité des électrodes de silicium est mise à mal par l’expansion volumique que le matériau subit lors sa réaction d’alliage avec le lithium, qui mène à la déconnexion des particules de Si et à une réduction continue de l’électrolyte. Une compréhension de ces phénomènes de vieillissement à l’échelle de la nanoparticule est nécessaire à la conception d’électrodes de silicium viables. Pour ce faire, la technique STEM-EELS a été optimisée de manière à s’affranchir des problèmes d’irradiation qui empêchent l’analyse des matériaux légers d’électrode négative et de la Solid electrolyte interface (SEI), grâce à l’analyse des pertes faibles EELS. Un puissant outil de cartographie de phase est obtenu et utilisé pour mettre en lumière la lithiation cœur-coquille initiale des nanoparticules de silicium cristallin, la morphologie hétérogène et la composition de la SEI, ainsi que la dégradation du silicium à l’issue de cyclages prolongés. Enfin, un modèle de vieillissement original est proposé, en s’appuyant notamment sur un effort de quantification des mesures STEM-EELS sur un grand nombre de nanoparticules
Over the last 25 years, the performance increase of lithium-ion batteries has been largely driven by the optimization of inactive components. With today’s environmental concerns, the pressure for more cost-effective and energy-dense batteries is enormous and new active materials should be developed to meet those challenges. Silicon’s great theoretical capacity makes it a promising candidate to replace graphite in negative electrodes in the mid-term. So far, Si-based electrodes have however suffered from the colossal volume changes silicon undergoes through its alloying reaction with Li. Si particles will be disconnected from the electrode’s percolating network and the solid electrolyte interface (SEI) continuously grows, causing poor capacity retention. A thorough understanding of both these phenomena, down to the scale of a single silicon nanoparticle (SiNP), is critical to the rational engineering of efficient Si-based electrodes. To this effect, we have developed STEM-EELS into a powerful and versatile toolbox for the study of sensitive materials and heterogeneous systems. Using the low-loss part of the EEL spectrum allows us to overcome the classical limitations of the technique.This is put to use to elucidate the first lithiation mechanism of crystalline SiNPs, revealing Li1.5Si @ Si core-shells which greatly differs from that of microparticles, and propose a comprehensive model to explain this size effect. The implications of that model regarding the stress that develops in the crystalline core of SiNPs are then challenged via stress measurements at the particle scale (nanobeam precession electron diffraction) for the first time, and reveal enormous compressions in excess of 4±2 GPa. Regarding the SEI, the phase-mapping capabilities of STEM-EELS are leveraged to outline the morphology of inorganic and organic components. We show that the latter contracts during electrode discharge in what is referred to as SEI breathing. As electrodes age, disconnection causes a diminishing number of SiNPs to bear the full capacity of the electrode. Overlithiated particles will in turn suffer from larger volumes changes and cause further disconnection in a self-reinforcing detrimental effect. Under extreme conditions, we show that SiNPs even spontaneously turn into a network of thin silicon filaments. Thus an increased active surface will compound the reduction of the electrolyte and the accumulation of the SEI. This can be quantified by summing and averaging STEM-EELS data on 1104 particles. In half-cells, the SEI volume is shown to increase 4-fold after 100 cycles without significant changes in its composition, whereas in full cells the limited lithiation performance understandably leads to a mere 2-fold growth. In addition, as the operating potential of the silicon electrodes increases in full cells – potential slippage – organic products in the SEI switch from being carbonate-rich to oligomer-rich. Finally, we regroup these findings into an extensive aging model of our own, based on both local STEM-EELS analyses and the macro-scale gradients we derived from them as a whole
Los estilos APA, Harvard, Vancouver, ISO, etc.
26

Serege, Matthieu. "Développement d'une nouvelle technique d'analyse pour les nanosctructures gravées par plasmas : (S)TEM EDX quasi in-situ". Thesis, Université Grenoble Alpes (ComUE), 2017. http://www.theses.fr/2017GREAT097/document.

Texto completo
Resumen
Avec la diminution perpétuelle des dimensions des circuits intégrés, la gravure de dispositifs à l’échelle nanométrique constitue un véritable défi pour les procédés plasma qui montrent des limites dans le cas d’empilement de couches minces notamment. L’anisotropie de gravure réside sur la formation de couches de passivations sur les flancs des motifs, qui agissent comme film protecteur bloquant la gravure latérale par les radicaux du plasma. Cependant, cette fine couche est responsable de l’apparition de pente dans les profils gravés et il est difficile de contrôler son épaisseur. De plus, une deuxième couche réactive est aussi formée en fond de motifs. Les produits de gravures sont formés au sein de cette couche permettant d’augmenter la vitesse de gravure du substrat. Il a récemment été admis que contrôler l’épaisseur de ces couches réactives constitue le paramètre clé pour obtenir une gravure à très haute sélectivité.Cependant, les couches réactives à analyser hautement réactives, en raison de leur forte concentration en halogènes, s’oxydent immédiatement lors de la remise à l’air.Cette étude se propose de développer une approche originale, simple et extrêmement puissante pour observer ces couches de passivation quasi in-situ (sans contact avec l’air ambiant) : Apres gravure, l’échantillon est transporté sous vide à l’intérieur d’une valise spécifique jusqu’à une enceinte de dépôt, où il est alors encapsulé par une couche métallique (PVD assisté par magnétron). L’échantillon ainsi encapsulé peut être observé ex-situ sans modification chimique grâce à des analyses STEM EDX
As the size of integrated circuit continues to shrink, plasma processes are more and more challenged and show limitations to etch nanometer size features in complex stacks of thin layers. The achievement of anisotropic etching relies on the formation of passivation layers on the sidewalls of the etched features, which act like a protective film that prevents lateral etching by the plasma radicals. However, this layer also generate a slope in the etch profile and it’s difficult to control its thickness. Another thin layer called “reactive layer” is also formed at the bottom of the features. Etch products are formed in this layer allowing a high etch rate of the substrate. It starts to be realized that controlling the thickness of this reactive layer is the key to achieve very high selective processes.However, the layers to be analyzed are chemically highly reactive because they contain large concentrations of halogens and they get immediately modified (oxidized) when exposed to ambient atmosphere.In this work we develop an original, simple and extremely powerful approach to observe passivation layers quasi in-situ (i.e. without air exposure): After plasma etching, the wafer is transported under vacuum inside an adapted suitcase to a deposition chamber where it is encapsulated by a metallic layer (magnetron sputtering PVD). Then, the encapsulated features can be observed ex situ without chemical / thickness modification thanks to (S)TEM-EDX analysis
Los estilos APA, Harvard, Vancouver, ISO, etc.
27

Tromas, Christophe. "Etude par AFM et TEM des premiers stades de plasticité induits par un essai de nanoindentation sur une face (001) d'un monocristal d'oxyde de magnésium". Poitiers, 2000. http://www.theses.fr/2000POIT2251.

Texto completo
Resumen
Cette etude a pour but de contribuer a une meilleure comprehension des mecanismes de deformation elementaire aboutissant a la formation d'une empreinte lors d'un essai de nanoindentation. Des empreintes de nanoindentation ont ete effectuees sur une face clivee (001) de mgo. Les deformations de surface autour des empreintes, et en particulier les lignes de glissement, ont ete observees a l'echelle nanometrique par afm (microscopie a force atomique). Cette etude de surface a ete completee par tem (microscopie electronique en transmission) afin de preciser la nature des dislocations et leur repartition en volume. Une synthese bibliographique concernant la structure de mgo ainsi que les principaux resultats des precedentes etudes par microindentation est tout d'abord proposee. Les resultats experimentaux sont ensuite presentes. Les differents stades de deformation, identifies sur les courbes de charge, sont detailles et notamment le declenchement de la plasticite par un phenomene de pop-in, ainsi que la poursuite de la deformation elastoplastique. Les deformations de surface autour des empreintes ainsi que les distributions de dislocations, associees a ces differents regimes, sont ensuite detailles. Ces resultats sont rapproches de ceux obtenus par microindentation sous plus forte charge tant dans le cadre de cette etude que dans la litterature. Enfin, une discussion sur l'origine des deformations et sur le mecanisme de formation des empreintes fait l'objet de la derniere partie de ce travail. Un modele a trois dimensions est propose pour rendre compte du phenomene de pop-in par nucleation de boucles de dislocations interstitielles sous l'indenteur. Plusieurs mecanismes detailles, prenant en compte les reactions entre les dislocations reparties autour des empreintes, et mettant en jeu un systeme de glissement inhabituel, sont exposes pour rendre compte de la poursuite de la deformation.
Los estilos APA, Harvard, Vancouver, ISO, etc.
28

Andersen, Ingrid Marie. "2D and 3D quantitative TEM mapping of CoNi nanowires". Thesis, Toulouse 3, 2020. http://www.theses.fr/2020TOU30205.

Texto completo
Resumen
Les nanofils magnétiques constituent un domaine de recherche en plein essor. De section cylindrique, ils permettent la propagation des parois de domaines magnétiques à très grandes vitesses et des interactions fortes avec les ondes de spin, ce qui les rend particulièrement intéressants pour le développement de futurs composants de la spintronique. L'objectif de ce travail de thèse est de fournir une analyse quantitative et qualitative complète de la configuration magnétique locale dans des nanofils magnétiques cylindriques d'alliage CoNi à anisotropie magnétocristalline perpendiculaire en utilisant les techniques d'imagerie magnétique avancées de la microscopie électronique à transmission (MET), principalement axées sur l'holographie électronique (HE). Une étude corrélative entre les propriétés structurales, les variations locales de composition et les configurations magnétiques de ces nanofils a été réalisée. De plus, les configurations tridimensionnelles (3D) complexes des domaines et des parois magnétiques ont été analysées par tomographie holographique de champ vectoriel (THCV) afin d'obtenir les trois composantes de l'induction magnétique. Enfin, un protocole a été développé pour étudier in situ par microscopie de Lorentz la configuration magnétique de ces nanofils lors de l'injection d'impulsions de courant. La première partie de ce travail est focalisée sur la corrélation des configurations magnétiques de nanofils individuels de CoNi avec les propriétés structurales et chimiques locales. L'orientation de la phase cristalline a été cartographiée en diffraction électronique par précession et combinée à des mesures de composition par spectroscopie de perte d'énergie des électrons. Les résultats révèlent une coexistence de grains de phase cfc et de phase hcp, cette dernière présente sa direction cristallographique c orientée presque perpendiculairement à l'axe du nanofil. Cette coexistence de phases cristallographiques est à l'origine de variations localisées et abruptes de la configuration magnétique. Deux nanofil configurations principales ont été observées : une chaîne d'états transversaux par rapport à l'axe du, de type vortex, et un état longitudinal. Nous avons observé que les états transversaux sont liés à la phase hcp possédant une forte anisotropie magnétocristalline perpendiculaire, ce que confirment les simulations micromagnétiques. Une autre partie de ce travail concerne l'étude de la structure magnétique 3D des domaines et des parois de domaines dans la phase hcp. Cette étude a été menée pour des états rémanents différents en fonction de l'application d'un champ de saturation perpendiculaire et parallèle à l'axe du nanofil. Les mesures ont été réalisées par la méthode THCV afin d'extraire les trois composantes de l'induction magnétique et reconstruire en 3D la configuration magnétique locale du nanofil. Les résultats montrent une stabilisation d'une chaîne de vortex dans le cas d'une saturation perpendiculaire, et des états d'enroulement longitudinaux séparés par des parois de domaine transversales après l'application d'un champ externe parallèle à l'axe du fils. La dernière partie du manuscrit présente les résultats obtenus en microscopie de Lorentz in situ démontrant la possibilité de manipuler les parois des domaines magnétiques d'un nanofil de CoNi par injection d'impulsions électriques. Cette preuve de concept est considérée comme le précurseur des observations in situ de la dynamique des parois de domaines en EH. Un protocole précis, axé sur les étapes cruciales de préparation des échantillons et les développements à poursuivre pour réaliser ces expériences délicates, est détaillé
Cylindrical magnetic nanowires (NWs) are currently subjects of high interest due to fast domain wall velocities and interaction with spin-waves, which are considered interesting qualities for developing future spintronic devices. This thesis aims to provide a wholesome quantitative and qualitative analysis of the local magnetic configuration in cylindrical Co-rich CoNi NWs with perpendicular magnetocrystalline anisotropy using state-of-the-art transmission electron microscopy (TEM) magnetic imaging techniques, mainly focused on two-dimensional (2D) and three-dimensional (3D) electron holography (EH). A correlative study between the NW's texture, modulation in composition, and magnetic configuration has been conducted. Further, the complex 3D nature of the domain and domain wall configurations have been analyzed using holographic vector field electron tomography (VFET) to retrieve all three components of the magnetic induction. Finally, I have successfully manipulated the magnetic configuration observed by Lorentz microscopy in Fresnel mode by the in situ injection of a current pulse. A TEM study comparing the magnetic configuration to the local NW structure was performed on single NWs. The crystal phase analysis was done by precession electron diffraction assisted automated crystal orientation mapping in the TEM combined with compositional analysis by scanning-TEM (STEM) electron energy loss spectroscopy (EELS) for a detailed correlation with the sample's magnetic configuration. The results reveal a coexistence of fcc grains and hcp phase with its c-axis oriented close to perpendicular to the wire axis in the same NW, which is identified as the origin of drastic local changes in the magnetic configuration. Two main configurations are observed in the NW region: a chain of transversal vortex-like states and a longitudinal curling state. The chain or vortices are linked to the hcp grain with the perpendicular magnetocrystalline anisotropy, as confirmed by micromagnetic simulations. The 3D magnetic structure of the domains and domain walls observed in the hcp grain of the NWs has been studied for two different remnant states: after the application of a saturation field perpendicular (i) and parallel (ii) to the NW axis. The measurements were done using state-of-the-art holographic VFET to extract all three components of the magnetic induction in the sample, as well as a 3D reconstruction of the volume from the measured electric potentials, giving insight into the local morphology of the NW. The results show a stabilization of a vortex chain in the case of perpendicular saturation, but longitudinal curling states separated by transversal domain walls after applying a parallel external field. Finally, preliminary Lorentz microscopy results are presented, documenting the manipulation of magnetic domain walls by the in situ injection of electrical pulses on a single cylindrical CoNi nanowire contacted by focused ion beam induced deposition. This is believed to be the forerunner for quantitative electrical measurements and in situ observations of domain wall dynamics using EH at the CEMES. A detailed protocol focusing on the crucial steps and challenges ahead for such a delicate experiment is presented, together with suggestions for future work to continue the developments
Los estilos APA, Harvard, Vancouver, ISO, etc.
29

Surrey, Alexander. "Preparation and Characterization of Nanoscopic Solid State Hydrogen Storage Materials". Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-217904.

Texto completo
Resumen
Die Speicherung von Wasserstoff in Form von Hydriden im festen Aggregatzustand hat den Vorteil einer hohen volumetrischen und gravimetrischen Wasserstoffspeicherdichte, die sowohl für die stationäre als auch die mobile Anwendung nötig ist. Um die Anforderungen dieser Anwendungen erfüllen zu können, müssen die Speichereigenschaften dieser Materialien weiter verbessert werden. Als zentrales Konzept dieser Dissertation wird die Nanostrukturierung verfolgt, die eine vielversprechende Strategie zur Modifizierung der thermodynamischen und kinetischen Eigenschaften von Hydriden darstellt. Die Transmissionselektronenmikroskopie (TEM) stellt dabei eine unverzichtbare Untersuchungsmethode solch nanoskopischer Materialien dar. Als problematisch erweist sich dabei die durch Radiolyse hervorgerufene Zersetzung der meisten Hydride bei der Beleuchtung mit dem abbildenden Elektronenstrahl. Im ersten Teil dieser Arbeit wird eine Methodik entwickelt um dieses Phänomen quantitativ mit Hilfe von Valenzelektronenenergieverlustspektroskopie zu untersuchen. Hierzu kommt kugelgemahlenes MgH2 als Modellsystem zum Einsatz. Die Dehydrierung kann quantitativ durch die inelastische Streuung der hochenergetischen Elektronen am MgH2-Plasmon erklärt werden. Eine Lösung dieses grundlegenden Problems wird theoretisch an Hand von Multislice TEM-Kontrastsimulationen untersucht. Hierbei wird ein TEM Experiment unter Wasserstoff bei Umgebungsdruck anstatt unter Vakuum simuliert, was mit Hilfe eines speziellen TEM Halters, in dem das Gas durch elektronentransparente Fenster eingeschlossen ist, realisiert werden kann. Im zweiten Teil wird der Einfluss des Nanoconfinements (Nanoeinschließung), einer speziellen Form der Nanostrukturierung, des komplexen Hydrids LiBH4 auf dessen Wasserstoffspeichereigenschaften untersucht, wofür eine neuartige nanoporöse aerogel-ähnliche Kohlenstoff-Gerüststruktur zum Einsatz kommt. Diese wird durch Salt Templating synthetisiert - einer simplen und nachhaltigen Methode zur Herstellung nanoporöser kohlenstoffbasierter Materialien mit großen Porenvolumina. Es wird gezeigt, dass durch das Nanoconfinement die Wasserstoffdesorptionstemperatur, die für makroskopisches LiBH4 bei über 400 °C liegt, auf 310 °C sinkt und die Desorption bereits bei 200 °C einsetzt. Eine teilweise Rehydrierung ist unter moderaten Bedingungen (100 bar und 300 °C) möglich, wobei die Reversibilität durch eine partielle Oxidation des amorphen Bor gehemmt ist. Im Gegensatz zu Beobachtungen einer aktuellen Veröffentlichung von in hoch geordnetem, nanoporösen Kohlenstoff eingebetteten LiBH4 deuten die in-situ TEM-Heizexperimente der vorliegenden Arbeit darauf hin, dass beide Reaktionsprodukte (B und LiH) in den Poren des aerogel-ähnlichen Kohlenstoffs verbleiben
Storing hydrogen in solid hydrides has the advantage of high volumetric and gravimetric hydrogen densities, which are needed for both stationary and mobile applications. However, the hydrogen storage properties of these materials must be further improved in order to meet the requirements of these applications. Nanostructuring, which represents one of the central approaches of this thesis, is a promising strategy to tailor the thermodynamic and kinetic properties of hydrides. Transmission electron microscopy (TEM) is an indispensable tool for the structural characterization of such nanosized materials, however, most hydrides degrade fast upon irradiation with the imaging electron beam due to radiolysis. In the first part of this work, a methodology is developed to quantitatively investigate this phenomenon using valence electron energy loss spectroscopy on ball milled MgH2 as a model system. The dehydrogenation can be quantitatively explained by the inelastic scattering of the incident high energy electrons by the MgH2 plasmon. A solution to this fundamental problem is theoretically studied by virtue of multislice TEM contrast simulations of a windowed environmental TEM experiment, which allows for performing the TEM analysis in hydrogen at ambient pressure rather than vacuum. In the second part, the effect of the nanoconfinement of the complex hydride LiBH4 on its hydrogen storage properties is investigated. For this, a novel nanoporous aerogel-like carbon scaffold is used, which is synthesized by salt templating - a facile and sustainable technique for the production of nanoporous carbon-based materials with large pore volumes. It is shown that the hydrogen desorption temperature, which is above 400 °C for bulk LiBH4, is reduced to 310 °C upon this nanoconfinement with an onset temperature as low as 200 °C. Partial rehydrogenation can be achieved under moderate conditions (100 bar and 300 °C), whereby the reversibility is hindered by the partial oxidation of amorphous boron. In contrast to recent reports on LiBH4 nanoconfined in highly ordered nanoporous carbon, in-situ heating in the TEM indicates that both decomposition products (B and LiH) remain within the pores of the aerogel-like carbon
Los estilos APA, Harvard, Vancouver, ISO, etc.
30

Wuttke, Timo Verfasser], Cynthia A. [Akademischer Betreuer] [Volkert, Cynthia A. [Gutachter] Volkert y Michael [Gutachter] Seibt. "TEM in-situ Untersuchungen an Ti-Ni basierten Formgedächtnislegierungen / Timo Wuttke ; Gutachter: Cynthia Volkert, Michael Seibt ; Betreuer: Cynthia Volkert". Göttingen : Niedersächsische Staats- und Universitätsbibliothek Göttingen, 2018. http://d-nb.info/1157094627/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
31

Kraus, Ines Elise [Verfasser] y Matthias [Akademischer Betreuer] Hannig. "Untersuchung der In-situ-Pellikelbildung auf verschiedenen Substraten mittels AFM, TEM und Ellipsometrie / Ines Elise Kraus. Betreuer: Matthias Hannig". Saarbrücken : Saarländische Universitäts- und Landesbibliothek, 2012. http://d-nb.info/1052557414/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
32

Roos, Burkhard Verfasser], Cynthia A. [Akademischer Betreuer] [Volkert y Michael [Akademischer Betreuer] Seibt. "In-situ Zugversuche an einkristallinen Gold-Nanodrähten im TEM / Burkhard Roos. Gutachter: Cynthia Volkert ; Michael Seibt. Betreuer: Cynthia Volkert". Göttingen : Niedersächsische Staats- und Universitätsbibliothek Göttingen, 2012. http://d-nb.info/1043609385/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
33

Izadi, Sina. "Al/Ti Nanostructured Multilayers: from Mechanical, Tribological, to Corrosion Properties". Scholar Commons, 2016. https://scholarcommons.usf.edu/etd/6265.

Texto completo
Resumen
Nanostructured metallic multilayers (NMMs) are well-known for their high strength in smaller bilayer thicknesses. Six Al/Ti (NMM) with different individual layer thickness were tested for their mechanical hardness using a nanoindentation tool. Individual layer thicknesses were chosen carefully to cover the whole confined layer slip (CLS) model. Nano-hardness had a reverse relation with the square root of individual layer thickness and reached a steady state at ~ 5 nm bilayer thickness. Decreasing the layer bilayer thickness from ~ 104 nm to ~ 5 nm, improved the mechanical hardness up to ~ 101%. Residual stresses were measured using grazing incident X-ray diffraction (GIXRD). Effect of residual stress on atomic structure and dislocation propagation was then investigated by comparing the amount and type of stresses in both aluminum and titanium phases. Based on the gathered data from GIXRD scans tensile stress in Ti phases, and compressive stress in Al would increase the overall coherency of structure. Wear rate in coatings is highly dependent on design and architect of the structure. NMM coatings are known to have much better wear resistance compare to their monolithic constituent phases by introducing a reciprocal architect. In current study wear rate of two Al/Ti NMMs with individual layer thicknesses of ~ 2.5 nm and ~ 30 nm were examined under normal loads of 30 µN, 60 µN, and 93 µN. Wears strokes were performed in various cycles of 1, 2, 3, 4 5 and 10. Wear rates were then calculated by comparing the 3D imaging of sample topology before and after tests. Nano-hardness of samples was measured pre and post each cycle of wear using a nanoindentation tool. The microstructure of samples below the worn surface was then characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), focus ion beam (FIB) and an optical profilometer. Orientation mapping was performed to analyze the microstructure of layers beneath the nano indents. TEM imaging from the cross section of worn samples indicated severely plastically deformed layer (SPDL) below the worn surface. Shear bands and twins are visible after wear and below the worn surface. Decreasing the layer thickness from 30 nm to 2.5 nm resulted in ~ 5 time’s better wear resistance. Nanowear caused surface hardening which consequently increased nano hardness up to ~ 30% in the sample with 2.5 nm individual layer thickness. Increasing the interfaces density of NMMs will significantly improve the corrosion resistance of coating. Reciprocal layers and consequently interfaces will block the path of aggressive content toward the substrate. Corrosion rate evolution of Al/Ti multilayers was investigated through DC corrosion potentiodynamic test. Results seem to be very promising and demonstrate up to 30 times better corrosion resistance compared to conventional sputtered monolithic aluminum. Corrosion started in the form of pitting and then transformed to the localized galvanic corrosion. Decreasing the bilayer thickness from ~ 10.4 nm to ~ 5 nm will decrease the corrosion current density (icorr) of ~ 5.42 × 10-7 (A/cm2) to ~ 6.11 × 10-10 (A/cm2). No sign of corrosion has been seen in the sample with ~ 2.5 nm individual layer thickness. Further AFM and TEM analysis from surface and cross section of NMMs indicate that a more coherent layer by layer structure improves the corrosion rate. Interfaces have a significant role in blocking the pores and imperfections inside coating.
Los estilos APA, Harvard, Vancouver, ISO, etc.
34

Sorensen, Daniel David. "Dissimilar Metal Joining in the Medical Device Industry". The Ohio State University, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=osu1494157928729494.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
35

Stuckner, Joshua Andrew. "Investigating the origin of localized plastic deformation in nanoporous gold by in situ electron microscopy and automatic structure quantification". Diss., Virginia Tech, 2019. http://hdl.handle.net/10919/100733.

Texto completo
Resumen
Gold gains many useful properties when it is formed into a nanoporous structure, but it also becomes macroscopically brittle due to flow localization and may therefore be unreliable for many applications. The goal of this work was to establish processing/structure/property relationships of nanoporous gold, discover controllable structure features, and understand the role of structure on flow localization. The nanoporous gold structure, consisting of a 3D network of nanoscale gold ligaments, was quantified with an automatic software developed for this work called AQUAMI, which uses computer vision techniques to make statistically reliable numbers of repeatable and unbiased measurements per image. AQUAMI increased the efficiency and accuracy of characterization in this work, allowed for the conduction of more experiments, and provided better confidence in morphology and size distribution of the complex NPG microstructural features. Nanoporous gold was synthesized while varying numerous processing factors such as dealloying time, annealing time, and mechanical agitation. Through the expanded scope of synthesis experiments and detailed analysis, it was discovered that the curvature of the ligaments and the distribution width of ligament diameters could be controlled through processing. In situ tensile experiments in SEM and TEM revealed that large ligaments arrested crack propagation while curved ligaments increase ductility by straightening in the tensile direction and forming geometrically required defects, which inhibit dislocation activity. Through synthesis and microstructure characterization, two new controllable structure features were discovered experimentally. In situ mechanical testing revealed the role these structures play on the deformation behavior and flow localization of nanoporous gold.
Doctor of Philosophy
Los estilos APA, Harvard, Vancouver, ISO, etc.
36

Berlin, Katja. "In-situ transmission electron microscopy on high-temperature phase transitions of Ge-Sb-Te alloys". Doctoral thesis, Humboldt-Universität zu Berlin, 2018. http://dx.doi.org/10.18452/19219.

Texto completo
Resumen
Das Hochtemperaturverhalten beeinflusst viele verschiedene Prozesse von der Materialherstellung bis hin zur technologischen Anwendung. In-situ Transmissionselektronenmikroskopie (TEM) bietet die Möglichkeit, die atomaren Prozesse während struktureller Phasenübergänge direkt und in Realzeit zu beobachten. In dieser Arbeit wurde in-situ TEM angewendet, um die Reversibilität des Schmelz- und Kristallisationsprozesses, sowie das anisotropen Sublimationsverhaltens von Ge-Sb-Te (GST) Dünnschichten zu untersuchen. Die gezielte Probenpräparation für die erfolgreiche Beobachtung der Hochtemperatur-Phasenübergänge wird hervorgehoben. Die notwendige Einkapselung für die Beobachtung der Flüssigphase unter Vakuumbedingungen und die erforderliche sauberer Oberfläche für den Sublimationsprozess werden detailliert beschrieben. Außerdem wird die Elektronenenergieverlustspektroskopie eingesetzt um die lokale chemische Zusammensetzung vor und nach den Übergängen zu bestimmen. Die Untersuchung der Grenzflächenstruktur und Dynamik sowohl beim Phasenübergang fest-flüssig als auch flüssig-fest zeigt Unterschiede zwischen den beiden Vorgängen. Die trigonale Phase von GST weist beim Schmelzen eine teilweise geordnete Übergangszone an der fest-flüssig-Grenzfläche auf, während ein solcher Zwischenzustand bei der Erstarrung nicht entsteht. Außerdem läuft der Schmelzvorgang zeitlich linear ab, während die Kristallisation durch eine Wurzelabhängigkeit von der Zeit mit überlagerter Start-Stopp-Bewegung beschrieben werden kann. Der Einfluss der Substrat-Grenzfläche wird diskutiert und die Oberflächenenergie von GST bestimmt. Die anisotrope Dynamik führt beim Phasenübergang fest-gasförmig der kubischen Phase von GST zur Ausbildung stabiler {111} Facetten. Dies erfolgt über die Bildung von Kinken und Stufen auf stabilen Terrassen. Die Keimbildungsrate und die bevorzugten Keimbildungsorte der Kinken wurden identifiziert und stimmen mit den Voraussagen des Terrassen-Stufen-Kinken Modells überein.
High-temperature behavior influence many different processes ranging from material processing to device applications. In-situ transmission electron microscopy (TEM) provides the means for direct observation of atomic processes during structural phase transitions in real time. In this thesis, in-situ TEM is applied to investigate the reversibility of the melting and solidification processes as well as the anisotropic sublimation behavior of Ge-Sb-Te (GST) thin films. The purposeful sample preparation for the successful observation of the high-temperature phase transitions is emphasized. The required encapsulation for the observation of the liquid phase inside the vacuum conditions and the necessary clean surface for sublimation process are discussed in detail. Additionally electron energy-loss spectroscopy in the TEM is used to determine the local chemical composition before and after the phase transitions. The analysis of the interface structure and dynamic during the solid-to-liquid as well as the liquid-to-solid phase transition shows differences between both processes. The trigonal phase of GST exhibits a partially ordered transition zone at the solid-liquid interface during melting while such an intermediate state does not form during solidification. Additionally the melting process proceeds with linear dependence on time, whereas crystallization can be described as having a square-root time-dependency featuring a superimposed start-stop motion. The influence of the interface is addressed and the surface energies of GST are determined. The anisotropic dynamic of the solid-to-gas phase transition of the cubic GST phase leads to the formation of stable {111} facets. This happens via kink and step nucleation on stable terraces. The nucleation rates and the preferred kink nucleation sites are identified and are in accordance with the predictions of terrace-step-kink model.
Los estilos APA, Harvard, Vancouver, ISO, etc.
37

Han, Ruixin. "SYNTHESIS, AND STRUCTURAL, ELECTROCHEMICAL, AND MAGNETIC PROPERTY CHARACTERIZATION OF PROMISING ELECTRODE MATERIALS FOR LITHIUM-ION BATTERIES AND SODIUM-ION BATTERIES". UKnowledge, 2018. https://uknowledge.uky.edu/chemistry_etds/90.

Texto completo
Resumen
Iron oxides, have been widely studied as promising anode materials in lithium-ion batteries (LIBs) for their high capacity (≈ 1000 mA h g-1 for Fe2O3 and Fe3O4,), non-toxicity, and low cost. In this work, β-FeOOH has been evaluated within a LIB half-cell showing an excellent capacity of ≈ 1500 mA h g-1 , superior to Fe2O3 or Fe3O4. Reaction mechanism has been proposed with the assistance of X-ray photoelectron spectroscopy (XPS). Various magnetic properties have been suggested for β-FeOOH such as superparamagnetism, antiferromagnetism and complex magnetism, for which, size of the material is believed to play a critical role. Here, we present a size-controlled synthesis of β-FeOOH nanorods. Co-existing superparamagnetism and antiferromagnetism have been revealed in β-FeOOH by using a Physical Property Measurement System (PPMS). Compared with the high price of lithium in LIBs, sodium-ion batteries (SIBs) have attracted increasing attentions for lower cost. Recent studies have reported Na0.44MnO2 to be a promising candidate for cathode material of SIBs. This thesis has approached a novel solid-state synthesis of Na0.44MnO2 whiskers and a nano-scaled open cell for in situ TEM study. Preliminary results show the first-stage fabrication of the cell on a biasing protochip.
Los estilos APA, Harvard, Vancouver, ISO, etc.
38

Sapezanskaia, Ina. "Deformation mechanisms of metastable stainless steels accessed locally by monotonic and cyclic nanoindentation". Doctoral thesis, Universitat Politècnica de Catalunya, 2016. http://hdl.handle.net/10803/398401.

Texto completo
Resumen
Metastable austenitic stainless steels feature an abundance of different deformation mechanisms, which contribute to the distinguished mechanical properties of these alloys. However, these properties are known to depend on the local microstructure and also are highly anisotropic. Furthermore, deformation is expected to be different for the bulk and the surface of a sample. In this sense, a discrete study is not trivial. The present work aims at investigation of the main deformation mechanisms and their gradual evolution, by employing controlled deformation of individual austenite grains via monotonic and cyclic nanoindentation. The corresponding loading–unloading curves have given extensive information about underlying mechanical properties, which could be related to an exhaustive reconstruction of the deformation substructure, both in surface and bulk, by different small scale characterization techniques. Amongst others, features such as time-dependent deformation, reversible phase transformation under load, crystalline anisotropy and grain size influences, besides plasticity transmission and fatigue behavior have been found and analyzed.
Los aceros inoxidables austeníticos metaestables pueden experimentar una amplia gama de mecanismos de deformación diferentes, los cuales contribuyen a sus extraordinarias propiedades mecánicas. Sin embargo, estas propiedades dependen de la microestructura y son altamente anisotrópicas. Además, la deformación es diferente en la superficie y en el interior de una muestra. Por lo tanto, un estudio detallado no resulta trivial. El objetivo de este trabajo es el estudio de los principales mecanismos de deformación, así como de su desarrollo gradual. Para ello se han realizado ensayos de nanoindentación, tanto monotónica como cíclica, los cuales han permitido la deformación controlada de granos austeníticos preseleccionados. Las curvas de carga y descarga de los ensayos de nanoindentación han proporcionado amplia información sobre el comportamiento mecánico del acero, la cual se ha podido correlacionar con la reconstrucción detallada de las subestructuras de deformación, tanto a nivel superficial como en el interior, la cual se ha llevado a cabo mediante técnicas de caracterización a escala microscópica. Entre otros, se encontraron y estudiaron fenómenos como las transformaciones de fase reversibles bajo carga, la influencia tanto de la anisotropía cristalina como del tamaño de grano, mecanismos dependientes del tiempo, junto con la transmisión de plasticidad y la respuesta a fatiga.
Les aciers inoxydables austénitiques métastables sont le siège de différents mécanismes de déformation qui sont à l'origine des propriétés mécaniques qui distinguent ce type d’alliages. Cependant, ces dernières, dépendant de la microstructure locale, sont fortement anisotropes. Par ailleurs, la déformation d'un échantillon massif serait différente de celle obtenue en surface. De ce fait, une étude détaillée trouve tout son intérêt. Le présent travail vise donc à identifier les principaux mécanismes de déformation et de leur évolution progressive, en se basant sur une déformation contrôlée de grains austénitiques individuels par des tests mécaniques de nanoindentation monotoniques et cycliques. Les courbes correspondantes au chargement-déchargement révèlent des informations détaillées sur les propriétés mécaniques sous-jacentes qui pourraient être liées à une étude complète de la structure de déformation en surface et en volume par différentes techniques de caractérisation à une échelle très fine. La déformation en fonction du temps, les phénomènes de transformation de phase réversible sous charge, l'anisotropie cristalline, l'influences de la taille des grains, la transmission de la plasticité et la tenue en fatigue ont été mis en évidence et étudiés.
Los estilos APA, Harvard, Vancouver, ISO, etc.
39

Gonzalez, Martinez Ignacio Guillermo. "Novel thermal and electron-beam approaches for the fabrication of boron-rich nanowires". Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-218019.

Texto completo
Resumen
Pursuing the development and implementation of novel synthesis techniques to produce nanostructures with an interesting set of properties is a goal that advances the frontiers of nanotechnology. Also of fundamental importance is to revisit well-established synthesis techniques employing a new set of materials as precursors, substrates and catalysts. Fundamental breakthroughs in the field of nanotechnology can be achieved by developing new synthesis procedures as well as by adapting known procedures to new materials. This thesis focuses on both kinds of experiments. A variant of chemical vapor deposition (CVD) has been used to produce Al5BO9 nanowires out of sapphire wafers without the need of a catalyst material. The novelty of the work relies on the formation mechanism of the Al5BO9 nanowires. Essentially, the process can be described as a large-scale topological transformation taking place on the substrate’s surface as its chemical composition changes due to the arrival of precursor molecules. Dense mats of Al5BO9 nanowires cover large areas of the substrate that were previously relatively flat. The process is enhanced by a high temperature and the presence of pre-existing superficial defects (cracks, terraces, etc.) on the substrates. Al5BO9 nanowires as well as B/BOX nanowires and BOX nanotubes were also produced via a novel in-situ electron beam-induced synthesis technique. The process was carried out at room temperature and inside a transmission electron microscope. Au nanoparticles were used as catalyst for the case of B/BOX nanowires and BOX nanotubes, while the Al5BO9 nanowires were synthesized without the need of a catalyst material. The formation and growth of the nanostructures is solely driven by the electron beam. The growth mechanism of the B/BOX nanowires and BOX nanotubes relies on interplay between electrostatic charging of the precursor material (to produce and transport feedstock material) and electron stimulated desorption of oxygen which is able to activate the catalytic properties of the Au nanoparticles. For the case Al5BO9 nanowires a nucleation process based on massive atomic rearrangement in the precursor is instigated by the e-beam, afterwards, the length of some of the nanowires can be extended by a mechanism analogous to that of the growth of the B/BOX nanowires.
Los estilos APA, Harvard, Vancouver, ISO, etc.
40

Edmondson, Philip D. "An in-situ TEM study of the formation and annealing of the damage resulting from single ion impacts in crystalline silicon". Thesis, University of Salford, 2007. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.490283.

Texto completo
Resumen
The work presented in this thesis describes both the thermal annealing of damage created in silicon due to low fluence ion implantation and the accumulation of that damage (to full amorphousness) at higher fluences. The technique utilised was in situ transmission electron microscopy (TEM).
Los estilos APA, Harvard, Vancouver, ISO, etc.
41

Chethala, Neelakandhan Shyam Kumar [Verfasser], Ralph [Akademischer Betreuer] Krupke y Christian [Akademischer Betreuer] Kübel. "In situ TEM studies on the graphitization and growth of nanocrystalline graphene from polymers / Shyam Kumar Chethala Neelakandhan ; Ralph Krupke, Christian Kübel". Darmstadt : Universitäts- und Landesbibliothek Darmstadt, 2019. http://d-nb.info/1201086515/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
42

Vailhé, Christophe N. P. "Deformation mechanisms in B2 aluminides: shear faults and dislocation core structures in FeAl, NiAl, CoAl and FeNiAl". Diss., Virginia Tech, 1996. http://hdl.handle.net/10919/38075.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
43

Löffler, Markus. "Nanomanipulation and In-situ Transport Measurements on Carbon Nanotubes". Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2010. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-33242.

Texto completo
Resumen
With the advent of microelectronics and micromechanical systems, the benefits of miniaturized technology became evident. With the discovery of carbon nanotubes by Iijima in 1991, a material has been found that offers superior porperties such as high tensile strength, excellent electrical and heat conductivity while being lightweight, flexible and tunable by the specific atomic arrangement in its structure. The first part of this thesis deals with a new synthesis approach, which combines the known routes of chemical vapour deposition and laser ablation. The results concerning diameter and yield fit well within an established model for the nucleation and growth of carbon nanotubes and extend it by considering a larger parameter space. Furthermore, conventional laser ablation has been used to synthesize C-13 augmented carbon nanotubes, whose diameters depend among the usual synthesis parameters also on the C-13 content, an influence which is in line with the changed thermal conductivities of isotope mixtures. Manipulation of carbon nanotubes inside a transmission electron microscope forms the second part of this thesis. With the help of an in-situ nanomanipulator, several experiments involving the mechanical and electrical properties of carbon nanotubes have been performed. Two-probe resistances of individual nanotubes have been measured and the observation of individual shell failures allowed for the determination of current limits per carbon shell. With the help of electrical current, a nanotube was modified in its electrical characteristics by reshaping its structure. By application of DC-currents or square current pulses, the filling of iron- or cementite-filled multi-wall carbon nanotubes has been found to move in a polarity-defined direction guided by the nanotube walls. Depending on the current, nanotube shape, and composition of the filling different regimes of material transport have been identified, including the reworking of the inner nanotube shells. The application of a high driving current leads to a complete reworking of the host nanotube and the current-induced growth of carbonaceous nanostructures of changed morphology. Utilizing the obtained results, a transport mechanism involving momentum transfer from the electron wind to the filling atoms and a solid filling core during transport is developed and discussed. Finally, measurements of mechanical properties using electrically induced resonant or non-resonant vibrations inside the transmission electron microscope have been observed and important mechanical parameters have been determined with the help of a modified Euler-Bernoulli-beam approach
Mit dem Aufkommen von Mikroelektronik und mikromechanischen Systemen wurden die Vorteile miniaturisierter Geräte augenscheinlich. Mit der Entdeckung von Kohlenstoff-Nanoröhren durch Iijima 1991 wurde ein Material gefunden, welches überlegene Eigenschaften wie hohe Festigkeit, exzellente elektrische und Wärmeleitfähigkeit zeigt, während es zeitgleich leicht und flexibel ist. Diese Eigentschaften können durch eine Änderung der spezifischen atomaren Anordnung in der Nanoröhrenhülle beeinflusst werden. Der erste Teil dieser Dissertationsschrift behandelt einen neuartigen Syntheseansatz, welche die bekannten Syntheserouten der chemischen Gasphasenabscheidung und Laserablation kombiniert. Die Ergebnisse bezüglich des Durchmessers und der Ausbeute lassen sich gut mit einem etablierten Modell der Nukleation und des Wachstums von Kohlenstoff-Nanoröhren beschreiben - sie erweitern es, indem sie einen größeren Parameterraum berücksichtigen. Des Weiteren wurde konventionelle Laserablation benutzt, um C-13 angereicherte Kohlenstoff-Nanoröhren herzustellen, deren Durchmesser nicht nur von den üblichen Parametern, sondern auch vom C-13 Anteil abhängt. Diese Abhängigkeit geht mit der veränderten thermischen Leitfähigkeit von Isotopenmischungen einher. Die Manipulation von Kohlenstoff-Nanoröhren in einem Transmission-Elektronenmikroskop formt den zweiten Teil der Dissertationschrift. Mit Hilfe eines in-situ Manipulators wurden vielfältige Experimente durchgeführt, um die mechanischen und elektrischen Eigenschaften der Kohlenstoff-Nanoröhren zu bestimmen. Zweipunktmessungen des Widerstands einzelner Nanoröhren und die Beobachtung des Versagens einzelner Kohlenstoffschichten erlaubte die Bestimmung der Stromtragfähigkeit einzelner Hüllen. Mit Hilfe eines elektrischen Stromes konnte eine Nanoröhre durch die veränderung der Struktur in ihren elektrischen Eigenschaften verändert werden. Unter Verwendung dauerhaften oder gepulsten Gleichstroms konnte die Eisen- oder Zementit-Füllung der Kohlenstoff-Nanoröhren in eine polaritätsabhängige Richtung bewegt werden. Die Füllung wurde dabei durch die Wände der Nanoröhre geführt. Abhängig von Strom, Form der Nanoröhre und Zusammensetzung der Füllung ließen sich verschiedene Bereiche des Materialtransports identifizieren, u.a. das Umarbeiten einiger innerer Kohlenstoffschichten. Ein hoher Strom hingegen bewirkt eine Umarbeitung der kompletten Nanoröhre und strominduziertes Wachstum von Kohlenstoff-Nanostrukturen mit veränderter Morphologie. Mit Hilfe der gewonnenen Resultate wurde ein Transportmodell entwickelt, welches den Impulstransfer von Elektronen an Füllungsatome sowie einen festen Füllungskern während des Transports diskutiert. Messungen der mechanischen Eigenschaften, welche mit Hilfe von resonanter oder nicht-resonanter elektrischer Anregung von Schwingungen im Transmissions-Elektronenmikroskop durchgeführt wurden bilden den Abschluss der Arbeit. Durch die Beobachtungen konnten mit einem modifizierten Euler-Bernoulli-Balkenmodell wichtige mechanische Eigenschaften bestimmt werden
Los estilos APA, Harvard, Vancouver, ISO, etc.
44

Mierwaldt, Daniel Joachim [Verfasser], Christian [Akademischer Betreuer] Jooß, Christian [Gutachter] Jooß y Simone [Gutachter] Techert. "In Situ X-ray Spectroscopy and Environmental TEM Study on Manganite Water Oxidation Catalysts / Daniel Joachim Mierwaldt ; Gutachter: Christian Jooß, Simone Techert ; Betreuer: Christian Jooß". Göttingen : Niedersächsische Staats- und Universitätsbibliothek Göttingen, 2017. http://d-nb.info/1149959045/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
45

Sun, Ye. "LINKING THE STRUCTURE AND MECHANICAL BEHAVIOR OF NANOPOROUS GOLD". UKnowledge, 2008. http://uknowledge.uky.edu/gradschool_diss/678.

Texto completo
Resumen
The structure of nanoporous gold (np-Au) provides a very limited volume for deformation to occur, and thus offers an opportunity to study the role of defects such as dislocations in nanoscale metal volumes. A practical goal is to understand mechanical properties of np-Au so that it can be can produced in stable form, for use in applications that require some mechanical integrity. Bulk and thin film np-Au have been fabricated and studied here. Bulk np-Au was prepared by electrochemically dealloying Au-Ag alloys with 25 and 30 at.% Au. In the lower Au content material, cracks always formed during dealloying. When Au content increased to 30 at.% and a two-step electrochemical dealloying method was used (first using diluted electrolyte and then concentrated acid), bulk np-Au with no volume change and minimal cracking was successfully fabricated. Thermal and mechanical behavior of np-Au was studied by heat treatment and microindentation. During annealing in air, Ostwald ripening governed ligament coarsening, while annealing of ligaments in vacuum was more likely a sintering process. Nanoporous Au thin films were produced by dealloying sputtered Au-Ag alloy films. Residual stresses in np-Au films were measured with wafer curvature. Similar to bulk materials, np-Au thin films made from 25 at.% Au alloy films exhibited extensive cracking during dealloying, whereas films from 30 at.% Au precursor alloys were completely crack-free. 25 at.% Au np-Au films carried almost no stress because of extensive cracking, whereas stress in 30 at.% Au np-Au films was up to ~230 MPa. Ligament coarsening followed a t1/8 time dependence for stress-free films, versus t1/4 in films under stress. It was proposed that bulk diffusion was responsible for formation of larger pits at grain centers during the incipient stages of dealloying. In situ nanoindentation experiments inside the transmission electron microscope were performed to investigate deformation of np-Au films and dislocation motion within ligaments. Dislocations were generated easily and moved along ligament axes, after which they interacted with other dislocations in the nodes of the porous network. It was found that slower displacement rates caused load drops to occur at shorter distance intervals and longer time intervals.
Los estilos APA, Harvard, Vancouver, ISO, etc.
46

Yu, Lei. "DECONVOLVING THE STEPS TO CONTROL MORPHOLOGY, COMPOSITION, AND STRUCTURE, IN THE SYNTHESIS OF HIGH-ASPECT-RATIO METAL OXIDE NANOMATERIALS". UKnowledge, 2017. http://uknowledge.uky.edu/chemistry_etds/82.

Texto completo
Resumen
Metal oxides are of interest not only because of their huge abundance but also for their many applications such as for electrocatalysts, gas sensors, diodes, solar cells and lithium ion batteries (LIBs). Nano-sized metal oxides are especially desirable since they have larger surface-to-volume ratios advantageous for catalytic properties, and can display size and shape confinement properties such as magnetism. Thus, it is very important to explore the synthetic methods for these materials. It is essential, therefore, to understand the reaction mechanisms to create these materials, both on the nanoscale, and in real-time, to have design control of materials with desired morphologies and functions. This dissertation covers both the design of new syntheses for nanomaterials, as well as real-time methods to understand their synthetic reaction mechanisms. It will focus on two parts: first, the synthesis of 1-dimension (1-D) featured nanomaterials, including manganese-containing spinel nanowires, and tin dioxide and zinc oxide-based negative nanowire arrays; and second, a mechanistic study of the synthetic reactions of nanomaterials using in situ transmission electron microscopy (TEM). The work presented here demonstrates unique synthetic routes to single crystalline “positive” and “negative” metal oxide nanowires, and introduces a new mechanism for the formation of single-crystalline hollow nanorods.
Los estilos APA, Harvard, Vancouver, ISO, etc.
47

Ramdon, Sanjay Kiran. "Nanoscale Characterization of Aged Li-Ion Battery Cathodes". The Ohio State University, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=osu1376625747.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
48

Subedi, Samikshya. "Evaluation of Microstructural and Mechanical Properties of Multilayered Materials". Research Showcase @ CMU, 2017. http://repository.cmu.edu/dissertations/802.

Texto completo
Resumen
Microstructure controls many physical properties of a material such as strength, ductility, 1density, conductivity, which, in turn, determine the application of these materials. This thesis work focuses on studying microstructural features (such as grain size, shape, defects, orientation gradients) and mechanical properties (such as hardness and yield strength) of multilayered materials that have undergone different loading and/or operating conditions. Two materials that are studied in detail are 18 nm Cu-Nb nanolaminates and 3D printed Inconel 718. Copper-Niobium (Cu-Nb) nanolaminate is a highly stable, high strength, nuclear irradiation resistant composite, which is destabilized with application of high pressure torsion (HPT). This work focuses on understanding the deformation and failure behavior of Cu-Nb using a novel orientation mapping technique in transmission electron microscopy in (TEM) called Automated Crystal Orientation Mapping (ACOM) and Digistar (ASTARTM) or Precession Electron Diffraction (PED). A new theory is postulated to explain strengthening mechanisms at the nanoscale using a data analytics approach. In-situ TEM compression and tensile testing is performed to image dislocation movement with the application of strain. This experiment was performed by Dr. Lakshmi Narayan Ramasubramanian at Xi’an Jiaotong University in China. Another major aspect of this research focuses on the design, fabrication, and microstructural characterization of 3D printed Inconel 718 heat exchangers. Various heat exchanger designs, machine resolution, printing techniques such as build orientation, power, and velocity of the laser beam are explored. Microstructural and mechanical properties of printed parts (before and after heat treatment) are then analyzed to check consistency in grain size, shape, porosity, hardness in relation to build height, scan parameters, and design. Various tools have been utilized such as scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), x-ray computed microtomography (at Advanced Photon Source at Argonne National Lab), hardness and micro-pillar compression testing for this study.
Los estilos APA, Harvard, Vancouver, ISO, etc.
49

Masliuk, Liudmyla [Verfasser], Robert [Akademischer Betreuer] Schlögl, Reinhard [Akademischer Betreuer] Schomäcker, Robert [Gutachter] Schlögl, Malte [Gutachter] Behrens y Michael [Gutachter] Lehmann. "Exploring the local differences of M1-type mixed oxides by quasi in-situ (S)TEM / Liudmyla Masliuk ; Gutachter: Robert Schlögl, Malte Behrens, Michael Lehmann ; Robert Schlögl, Reinhard Schomäcker". Berlin : Technische Universität Berlin, 2018. http://d-nb.info/1171306237/34.

Texto completo
Los estilos APA, Harvard, Vancouver, ISO, etc.
50

Sundberg, Jill. "Triboactive Low-Friction Coatings Based on Sulfides and Carbides". Doctoral thesis, Uppsala universitet, Oorganisk kemi, 2014. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-230989.

Texto completo
Resumen
For sustainable development, it is highly important to limit the loss of energy and materials in machines used for transportation, manufacturing, and other purposes. Large improvements can be achieved by reducing friction and wear in machine elements, for example by the application of coatings. This work is focused on triboactive coatings, for which the outermost layer changes in tribological contacts to form so-called tribofilms. The coatings are deposited by magnetron sputtering (a physical vapor deposition method) and thoroughly chemically and structurally characterized, often theoretically modelled, and tribologically evaluated, to study the connection between the composition, structure and tribological performance of the coatings. Tungsten disulfide, WS2, is a layered material with the possibility of ultra-low friction. This work presents a number of nanocomposite or amorphous coatings based on WS2, which combine the low friction with improved mechanical properties. Addition of N can give amorphous coatings consisting of a network of W, S and N with N2 molecules in nanometer-sized pockets, or lead to the formation of a metastable cubic tungsten nitride. Co-deposition with C can also give amorphous coatings, or nanocomposites with WSx grains in an amorphous C-based matrix. Further increase in coating hardness is achieved by adding both C and Ti, forming titanium carbide. All the WS2-based materials can provide very low friction (down to µ<0.02) by the formation of WS2 tribofilms, but the performance is dependent on the atmosphere as O2 and H2O can be detrimental to the tribofilm functionality. Another possibility is to form low-friction tribofilms by tribochemical reactions between the two surfaces in contact. Addition of S to TiC/a-C nanocomposite coatings leads to the formation of a metastable S-doped carbide phase, TiCxSy, from which S can be released. This enables the formation of low-friction WS2 tribofilms when a Ti-C-S coating is run against a W counter-surface. Reduced friction, at a moderate level, also occurs for steel counter-surfaces, likely due to formation of beneficial iron sulfide tribofilms. The studied coatings, whether based on WS2 or TiC, are thus triboactive, with the ability to form low-friction tribofilms in a sliding contact.
Los estilos APA, Harvard, Vancouver, ISO, etc.
También puede estar interesado en las bibliografías sobre el tema "In situ TEM nanoindentation" para otros tipos de fuentes:
Artículos de revistas
Ofrecemos descuentos en todos los planes premium para autores cuyas obras están incluidas en selecciones literarias temáticas. ¡Contáctenos para obtener un código promocional único!

Pasar a la bibliografía