Littérature scientifique sur le sujet « Fib-Sem-Dic »

Ga-ion micro-ring-core FIB-DIC evaluation of residual stresses in shot peened VT6 (Ti-6Al-4V) alloy was carried out and cross-validated against other non-destructive and semi-destructive residual stresses evaluation techniques, namely, the conventional sin2ψ X-ray diffraction and mechanical hole drilling. The Korsunsky FIB-DIC method of Ga-ion beam micro-ring-core milling within FIB-SEM with Digital Image Correlation (DIC) deformation analysis delivered spatial resolution down to a few micrometers, while the mechanical drilling of circular holes of ~2 mm diameter with laser speckle interferometry monitoring of strains gave a rough spatial resolution of a few millimeters. Good agreement was also found with the X-ray diffraction estimates of residual stress variation profiles as a function of depth. These results demonstrate that FIB-DIC provides rich information down to the micron scale, it also allows reliable estimation of macro-scale residual stresses.

New challenges for design, manufacturing and packaging of MEMS/NEMS arise from the ongoing miniaturization process. Therefore there is a demand on detailed information on thermo-mechanical material properties of the applied materials. Because of size effects and the strong dependency of the thermo-mechanical behavior of active and passive components on process parameters often unsolved questions of residual stresses lead to system failure due to crack formation. With the fibDAC (Focused Ion Beam based Deformation Analysis by Correlation) method which is presented in this paper the classical hole drilling method for stress release measurement has been downscaled to the nanoscale. The ion beam of the FIB station is used as a milling tool which causes the stress release at silicon microstructures of MEMS devices. The analysis of the stress release is achieved by digital image correlation (DIC) applied to load state SEM images captured in a cross beam equipment (combination of SEM and FIB). The results of the DIC analysis are deformation fields which are transferred to stress solution by application of finite element analysis. In another step the resolution of the method has been improved by the application of trench milling instead of hole milling. Thereby deformation measurements in the nm range are established. The method is also a powerful tool for the analysis of sub-grain stresses of engineering materials.

This study investigated the mechanical properties and the residual stress of high-power impulse magnetron sputtering (HiPIMS) titanium nitride (TiN) thin film capping on cold spray titanium (Ti) coating. This TiN/Ti duplex coating was deposited on the Ti substrate, and the cold spray titanium (Ti) coating was prepared in three cases with different numbers of layers. The study determined Young’s modulus, hardness, and roughness of TiN thin film and cold spray Ti coatings by nano-indentation and AFM. The residual stress measurement of TiN/Ti duplex coating was conducted using the ring-core drilling method. A focused ion beam (FIB) drilled the TiN/Ti duplex coating with various milling depth steps. The corresponding images were obtained with a scanning electron microscope (SEM). The relationship between surface deformations and relaxation stress after each milling depth step was obtained using the digital image correlation (DIC) method. The results showed TiN/Ti duplex coating exhibited excellent mechanical properties, and the residual stresses were not significantly changing with different Ti cold spray substrates, showing the feasibility of coating technology for the future applications in the aerospace industry.

The residual stress of thin films during the deposition process can cause the components to have unpredictable deformation and damage, which could affect the service life and reliability of the microsystems. Developing an accurate and reliable method for measuring the residual stress of thin films at the micrometer and nanometer scale is a great challenge. To analyze the residual stress regarding factors such as the mechanical anisotropy and preferred orientation of the materials, information related to the in-depth lattice strain function is required when calculating the depth profiles of the residual strain. For depth-resolved measurements of residual stress, it is strategically advantageous to develop a measurement procedure that is microstructurally independent. Here, by performing an incremental focused ion beam (FIB) ring-core drilling experiment with various depth steps, the digital image correlation (DIC) of the specimen images was obtained. The feasibility of DIC to FIB images was evaluated after the translation test, and an appropriate procedure for reliable results was established. Furthermore, the condition of the film in the function of residual stress was assessed and compared to elucidate the applicability of this technology.

Le travail qui suit est divisé en trois grandes parties. Premièrement, lorsque nous souhaitons réaliser des études à des échelles plus petites telles que l’échelle micrométrique, nous devons non seulement utiliser un moyen d’observation plus complexe, tel que le microscope électronique à balayage «MEB-FEG» pour obtenir des images exploitables en métrologie optique, mais aussi avoir un marquage (mouchetis) à ces échelles.Actuellement, la corrélation d’images numériques est la technique de mesure de champs cinématique la plus utilisée pour étudier le comportement mécanique des matériaux et des structures sur une zone d’intérêt allant de l’échelle du mètre à l’échelle millimétrique. Ces derniers peuvent être obtenus par diverses techniques comme par exemple en utilisant le Dual-Beam «FIB».Pour la démarche scientifique adoptée nous avons commencé par développer un mouchetis artificiel, avec une profondeur de gravure de l’ordre de 100 nanomètres. Nous nous sommes appuyés également sur des outils statistiques tels que la gamme des niveaux de gris, l’auto corrélation, le nombre de passes et la variation de grossissement qui s’avèrent nécessaires pour valider le marquage et avoir de meilleurs résultats. Ceci a constitué la première partie de cette thèse.Dans la seconde partie, la méthode DIC a été adoptée en utilisant un microscope électronique à balayage (MEB) et un marquage réalisé grâce à un faisceau d’ions focalisés (FIB). Afin de construire une solution métrologique maîtrisée et fiable pour observer et quantifier les mouvements et les déformations de la matière à ces échelles, différents essais ont été réalisés sur deux métaux différents, à savoir, l’Acier 3041 et l’Inconel 718, et ce pour s’assurer de la répétabilité et de la reproductibilité de la procédure.Dans ces essais, nous avons proposé de calculer les déplacements horizontaux et verticaux ainsi que l’erreur liée à ces déplacements. La même démarche a été menée sur les champs de déformations. Différents résultats ont été obtenus en fonction de la variation de l’écart type trouvé dans les données acquises permettant de quantifier les erreurs de mesure ainsi que la répétabilité et la dérive dans le temps.La dernière partie du travail proposé porte sur l’adaptation des méthodes de mesure aux mécanismes particuliers de déformation à ces échelles, comme la localisation de fractures et l’endommagement.Pour étudier le comportement mécanique et prendre en compte les fractures locales, nous avons procédé à l’extraction des déformations d’un matériau fracturé à l’aide d’une méthode de mesure de champ de déplacement.L’approche proposée consistait à extraire les déformations résiduelles des premiers gradients locaux de HDIC les moins perturbés par la fracture. Différents tests ont été effectués pour évaluer la validité de cette nouvelle approche proposée.Une application pour étudier le comportement mécanique d’un composite métallique (Al /ω-Al-Cu-Fe) a été proposée. Une exploitation particulière de tous les champs réside dans la bonne séparation des champs de déformation et de la partie fissurée.Une discussion sur la comparaison entre une analyse DIC conventionnelle et son extension a été présentée sur les zones avec et sans fractures
This work is divided into three main parts. Initially, in order to order to carry out our studies at smaller scales such as micrometric scale, we must not only use a more complex means of observation, for example, scanning electron microscope "MEB-FEG" to obtain images usable in metrology optical, but also have to mark (speckle) on these scales. More recently, digital image correlation is the most widely used kinematic field measurement technique to study the mechanical behavior of materials and structures over an area of interest ranging from the meter scale to the millimeter one. This can be obtained by using a dual-focused ion beam technique. Furthermore, we have adopted a scientific approach by first developing an artificial speckle, with an engraving depth of the order of 100 nanometers. We also relied on statistical tools such as the range of gray levels, autocorrelation, the number of passes and the variation of magnification, which were necessary to validate the marking and to generate better results.In the second part, we coupled the DIC by utilizing the scanning electron microscope and the focused ion beam as the labelling techniques. In order to build a controlled and reliable metrological solution to observe and quantify the movements and deformations of matter at these scales. Several tests have been carried out on two metals ; Steel 304l and Inconel 718, toensure the repeatability and reproducibility of the procedure. In these tests, we proposed to calculate the horizontal and vertical displacements as well as the error related to these displacements.We demonstrate the same approach on the deformation fields. Different results have been obtained depending on the variation of the standard deviation found in the acquired data making it possible to quantify measurement errors as well as repeatability and drift over time.The last part of the proposed work is about the adaptation of measurement methods to the particular mechanisms of deformation at different scales, such as the location of fractures and damage. To study mechanical behavior and taking into account local fractures, we extract the deformations of a fractured material using a displacement field measurement method. The proposed approach consists of extracting the residual deformations of the first local gradients of H-DIC, the least disturbed by the fractures. Various tests have been carried out to assess the validity of this proposed new approach. An application to study the mechanical behavior of a metallic composite (Al / ω -Al-Cu-Fe) is proposed. Particular exploitation of all the fields lies in the good separation of the deformation fields and the cracked part. A discussion on the comparison between a conventional DIC analysis and its extension is presented on the zones without and with fractures