Academic literature on the topic 'SEM-EBSD analysis'
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Journal articles on the topic "SEM-EBSD analysis"
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Goehner, R. P., and J. R. Michael. "Microdiffraction phase identification in the scanning electron microscope (SEM)." Powder Diffraction 19, no. 2 (2004): 100–103. http://dx.doi.org/10.1154/1.1757450.
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The identification of crystallographic phases in the scanning electron microscope (SEM) has been limited by the lack of a simple way to obtain electron diffraction data of an unknown while observing the microstructure of the specimen. With the development of charge coupled device (CCD)-based detectors, backscattered electron Kikuchi patterns, alternately referred to as electron backscattered diffraction (EBSD) patterns, can be easily collected. Previously, EBSD has been limited to crystallographic orientation studies due to the poor pattern quality collected with video rate detector systems. With CCD detectors, a typical EBSD can now be acquired from a micron or submicron sized crystal using an exposure time of 1–10 s with an accelerating voltage of 10–40 kV and a beam current as low as 0.1 nA. Crystallographic phase analysis using EBSD is unique in that the properly equipped SEM permits high magnification images, EBSDs, and elemental information to be collected from bulk specimens. EBSD in the SEM has numerous advantages over other electron beam-based crystallographic techniques. The large angular view (∼70°) provided by EBSD and the ease of specimen preparation are distinct advantages of the technique. No sample preparation beyond what is commonly used for SEM specimens is required for EBSD.
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Picard, Yoosuf N., Ranga Kamaladasa, Marc De Graef, et al. "Future Prospects for Defect and Strain Analysis in the SEM via Electron Channeling." Microscopy Today 20, no. 2 (2012): 12–16. http://dx.doi.org/10.1017/s1551929512000077.
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Electron diffraction in both SEM and TEM provides a contrast mechanism for imaging defects as well as a means for quantifying elastic strain. Electron backscatter diffraction (EBSD) is the commercially established method for SEM-based diffraction analysis. In EBSD, Kikuchi patterns are acquired by a charge-coupled device (CCD) camera and indexed using commercial software. Phase and crystallographic orientation information can be extracted from these Kikuchi patterns, and researchers have developed cross-correlation methods to measure strain as well.
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KUBUSHIRO, Keiji, Yohei SAKAKIBARA, and Toshihiro OHTANI. "Creep Strain Analysis of Austenitic Stainless Steel by SEM/EBSD." Journal of the Society of Materials Science, Japan 64, no. 2 (2015): 106–12. http://dx.doi.org/10.2472/jsms.64.106.
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ISHIDA, Kyoichi, Ritsu HIROHARA, and Muneyuki IMAFUKU. "Texture analysis of fine-grained stainless steel by SEM/EBSD." Proceedings of Conference of Kanto Branch 2017.23 (2017): 902. http://dx.doi.org/10.1299/jsmekanto.2017.23.902.
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Guilmeau, E., Catherine Henrist, Tohru Suzuki, et al. "Texture of Alumina by Neutron Diffraction and SEM-EBSD." Materials Science Forum 495-497 (September 2005): 1395–400. http://dx.doi.org/10.4028/www.scientific.net/msf.495-497.1395.
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The orientation distributions of α-Al2O3 textured ceramics are determined from neutron diffraction and SEM-EBSD. A curved position-sensitive detector coupled to a tilt angle (χ) scan allowed the whole neutron diffraction pattern treatment in the combined Rietveld-WIMV-Popa algorithm. Analyses from neutron and electron diffraction data gave similar results if EBSD data are smoothed to account for grain statistics. Four textured alumina ceramics were prepared by slipcasting under a high magnetic field and sintered at 800°C, 1300°C, 1400°C and 1600°C. The inverse pole figures and EBSD-mapping highlights the influence of the magnetic field and sintering temperature on the texture development. The inverse pole figures calculated for the fiber direction show a major (001) component for all the samples. With the increasing sintering temperature, the texture strength is enhanced and the c-axis distribution is sharper. The effectiveness of the combined approach for determining the crystallite size is also evident. As a global trend, the calculated crystallite size and observed grain size are similar and increase with the increasing sintering temperature. The mechanism of the texture development in the sintered specimens is certainly initiated from the preferred orientation of the green body after slip-casting under a high magnetic field. The basal texture is enhanced during sintering by selective anisotropic grain growth. We evidenced here the powerfulness of the Rietveld texture analysis correlated to SEM-EBSD calculation to provide a basis for the correlation of texture, microstructural parameters and anisotropic properties.
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Kojima, Yohei, Yuta Matsumoto, Daniel Goran, John Gilbert, and Naoki Kikuchi. "Crystalline analysis by W-SEM using a newly developed EBSD detector." BIO Web of Conferences 129 (2024): 05029. http://dx.doi.org/10.1051/bioconf/202412905029.
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UETSUJI, Yasutomo, Hideyuki NAGAKURA, Yu SATO, and Eiji NAKAMACHI. "308 Crystal Orientation Analysis of Piezoelectric Ceramics by SEM・EBSD Technique." Proceedings of The Computational Mechanics Conference 2006.19 (2006): 149–50. http://dx.doi.org/10.1299/jsmecmd.2006.19.149.
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Strehle, S., S. Menzel, H. Wendrock, J. Acker, and K. Wetzig. "SEM/EBSD Texture Analysis of Electrochemically Deposited CuAg-Alloy Thin Films." Microscopy and Microanalysis 9, S03 (2003): 272–73. http://dx.doi.org/10.1017/s1431927603023304.
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Lyman, Charles. "Small, Focused Technical Conferences." Microscopy Today 18, no. 2 (2010): 5. http://dx.doi.org/10.1017/s1551929510000210.
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The feature article in this issue is a prelude to the Microbeam Analysis Society (MAS) Topical Conference on electron backscatter diffraction (EBSD) to be held at the University of Wisconsin, May 24–26, 2010. The popularity of the EBSD technique is growing rapidly. This analytical method is capable of both identifying crystalline phases and determining the orientation of grains and second phases. Phase analysis by EBSD combined with elemental analysis by x-ray emission spectrometry provides the SEM with extraordinary analytical power. Maps of crystal grain orientations are widely used in metallurgical and geological research.
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Zasada, Dariusz, Wojciech Polkowski, and Robert Jasionowski. "Analysis of the Effect of the Wearing Type on Surface Structural Changes of Ni3Al-Based Intermetallic Alloy." Solid State Phenomena 225 (December 2014): 25–32. http://dx.doi.org/10.4028/www.scientific.net/ssp.225.25.
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Results of an analysis of effect of wearing type on surface structural changes of a Ni3Al intermetallic alloy, are shown in the present paper. A microstructure evaluation was carried out by Quanta 3D FEG field emission gun scanning electron microscope (FEG SEM) equipped with an integrated EDS/WDS/EBSD system. The Ni3Al-based intermetallic alloy with an addition of boron, zirconium and chromium was examined. The investigated material had γ’ single-phase, ordered solid solution structure with 20 μm grain size. An electron backscatter diffraction (EBSD) method was applied to visualize surface structural changes upon an abrasive, a cavitational and a tribological wearing of the material.An observation of surface layer after the abrasive wear was carried out on samples examined in loose abradant by T-07 tester and according to GOST 23.2008-79 norm. An analysis of cavitational wear on changes in the near surface area of Ni3Al-based alloy was performed on an impact-jet stand. Observed structural changes were described based on results of the SEM/EBSD complex structural examination and hardness measurements. It was found, that the EBSD is an effective and sensitive method that allows estimating surface strain introduced during analyzed wearing types.
Dissertations / Theses on the topic "SEM-EBSD analysis"
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Kacher, Joshua Peter. "Cross-Correlation-Based Texture Analysis Using Kinematically Simulated EBSD Patterns." BYU ScholarsArchive, 2009. https://scholarsarchive.byu.edu/etd/1746.
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The development and example applications of a new EBSD-based texture analysis system are presented. This new system uses the cross-correlation function to compare two EBSD patterns at a number of corresponding regions in each pattern to calculate the deformation gradient tensor. Bragg's Law-based simulated EBSD patterns are used as reference patterns in the cross-correlation method to enable the measurements of absolute elastic strain and lattice orientation at discrete points in a crystalline sample. The resolution limits of this new method are explored using a variety of computational and physical experiments. The simulated pattern method is estimated to be able to measure lattice orientations to within +/-0.02° and elastic strains to within +/-3.6x10-4 for small strains and +/-1x10-3 for large strains. Two example applications are demonstrated. The first demonstration is estimating the dislocation density in a 5.5% compressed Mg-based AZ91 alloy. Nye's and Kröner's formulations are used to estimate the dislocation density. Comparisons are made with traditional OIM measurements and it is found that the simulated pattern method offers an order of magnitude improvement in dislocation density estimations over OIM. The second demonstration is tetragonality measurements of HSLA 65 steel along the weld line of a friction stir welded plate. Accurate tetragonality measurements in the bainite phase of the steel can be made using information from the diagonal components of the elastic strain tensor. The measured tetragonality can be related to the concentration of interstitial carbon atoms in the iron lattice to find the carbon distribution in the sample. From these experiments, it is demonstrated that the simulated pattern method presents a new and powerful methodology for texture analysis that exhibits both ease of use and access to high resolution orientation and elastic strain data.
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Yuan, Hui. "3D morphological and crystallographic analysis of materials with a Focused Ion Beam (FIB)." Thesis, Lyon, INSA, 2014. http://www.theses.fr/2014ISAL0134/document.
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L’objectif principal de ce travail est d’optimise la tomographie par coupe sériée dans un microscope ‘FIB’, en utilisant soit l’imagerie électronique du microscope à balayage (tomographie FIB-MEB), soit la diffraction des électrons rétrodiffusés (tomographie dite EBSD 3D). Dans les 2 cas, des couches successives de l’objet d’étude sont abrasées à l’aide du faisceau ionique, et les images MEB ou EBSD ainsi acquises séquentiellement sont utilisées pour reconstruire le volume du matériau. A cause de différentes sources de perturbation incontrôlées, des dérives sont généralement présentes durant l'acquisition en tomographie FIB-MEB. Nous avons ainsi développé une procédure in situ de correction des dérives afin de garder automatiquement la zone d'intérêt (ROI) dans le champ de vue. Afin de reconstruction le volume exploré, un alignement post-mortem aussi précis que possible est requis. Les méthodes actuelles utilisant la corrélation-croisée, pour robuste que soit cette technique numérique, présente de sévères limitations car il est difficile, sinon parfois impossible de se fier à une référence absolue. Ceci a été démontré par des expériences spécifiques ; nous proposons ainsi 2 méthodes alternatives qui permettent un bon alignement. Concernant la tomographie EBSD 3D, les difficultés techniques liées au pilotage de la sonde ionique pour l'abrasion précise et au repositionnement géométrique correct de l’échantillon entre les positions d'abrasion et d’EBSD conduisent à une limitation importante de la résolution spatiale avec les systèmes commerciaux (environ 50 nm)3. L’EBSD 3D souffre par ailleurs de limites théoriques (grand volume d'interaction électrons-solide et effets d'abrasion. Une nouvelle approche, qui couple l'imagerie MEB de bonne résolution en basse tension, et la cartographie d'orientation cristalline en EBSD avec des tensions élevées de MEB est proposée. Elle a nécessité le développement de scripts informatiques permettant de piloter à la fois les opérations d’abrasion par FIB et l’acquisition des images MEB et des cartes EBSD. L’intérêt et la faisabilité de notre approche est démontrée sur un cas concret (superalliage de nickel). En dernier lieu, s’agissant de cartographie d’orientation cristalline, une méthode alternative à l’EBSD a été testée, qui repose sur l’influence des effets de canalisation (ions ou électrons) sur les contrastes en imagerie d’électrons secondaires. Cette méthode corrèle à des simulations la variation d’intensité de chaque grain dans une série d’images expérimentales obtenues en inclinant et/ou tournant l’échantillon sous le faisceau primaire. Là encore, la méthode est testée sur un cas réel (polycritsal de TiN) et montre, par comparaison avec une cartographie EBSD, une désorientation maximale d'environ 4° pour les angles d’Euler. Les perspectives d’application de cette approche, potentiellement beaucoup plus rapide que l’EBSD, sont évoquées<br>The aim of current work is to optimize the serial-sectioning based tomography in a dual-beam focused ion beam (FIB) microscope, either by imaging in scanning electron microscopy (so-called FIB-SEM tomography), or by electron backscatter diffraction (so-called 3D-EBSD tomography). In both two cases, successive layers of studying object are eroded with the help of ion beam, and sequentially acquired SEM or EBSD images are utilized to reconstruct material volume. Because of different uncontrolled disruptions, drifts are generally presented during the acquisition of FIB-SEM tomography. We have developed thus a live drift correction procedure to keep automatically the region of interest (ROI) in the field of view. For the reconstruction of investigated volume, a highly precise post-mortem alignment is desired. Current methods using the cross-correlation, expected to be robust as this digital technique, show severe limitations as it is difficult, even impossible sometimes to trust an absolute reference. This has been demonstrated by specially-prepared experiments; we suggest therefore two alternative methods, which allow good-quality alignment and lie respectively on obtaining the surface topography by a stereoscopic approach, independent of the acquisition of FIB-SEM tomography, and realisation of a crossed ‘hole’ thanks to the ion beam. As for 3D-EBSD tomography, technical problems, linked to the driving the ion beam for accurate machining and correct geometrical repositioning of the sample between milling and EBSD position, lead to an important limitation of spatial resolution in commercial softwares (~ 50 nm)3. Moreover, 3D EBSD suffers from theoretical limits (large electron-solid interaction volume for EBSD and FIB milling effects), and seems so fastidious because of very long time to implement. A new approach, coupling SEM imaging of good resolution (a few nanometres for X and Y directions) at low SEM voltage and crystal orientation mapping with EBSD at high SEM voltage, is proposed. This method requested the development of computer scripts, which allow to drive the milling of FIB, the acquisition of SEM images and EBSD maps. The interest and feasibility of our approaches are demonstrated by a concrete case (nickel super-alloy). Finally, as regards crystal orientation mapping, an alternative way to EBSD has been tested; which works on the influence of channelling effects (ions or electrons) on the imaging contrast of secondary electrons. This new method correlates the simulations with the intensity variation of each grain within an experimental image series obtained by tilting and/or rotating the sample under the primary beam. This routine is applied again on a real case (polycrystal TiN), and shows a max misorientation of about 4° for Euler angles, compared to an EBSD map. The application perspectives of this approach, potentially faster than EBSD, are also evoked
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Tryblom, Axel. "Optimizing Transmission Kikuchi Diffraction for Analysing Grain Size and Orientation of Nanocrystalline Coatings." Thesis, Uppsala universitet, Tillämpad materialvetenskap, 2015. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-266442.
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In order to increase efficiency and lifetime of cutting tools it is typical to apply thin coatings by physical or chemical vapour deposition. Applying coatings on cutting tools has shown an increase in both efficiency and lifetime and are of large interest in further development. The study of coatings and their mechanical properties is a very active research area and produces tools extensively used in the industry. The behaviour of materials on a macroscopic scale can typically be related to microscopic properties. Some coatings produced by Chemical Vapour Deposition (CVD) but especially Physical Vapour deposition (PVD) have crystal structures which are difficult to analyse by conventional methods due to crystal sizes in the nanometre scale. For nanocrystalline materials standard methods fall short due to a limited resolution of the methods. Recently a method for electron diffraction of crystalline samples was suggested to be used differently in order to achieve a higher resolution. Unlike earlier when electrons were reflected from the sample, using Electron Backscattering Diffraction (EBSD), the electrons were transmitted through thin samples with thicknesses in the magnitude of 100 nm, which enabled the crystal structure to be determined. The new method is typically referred to as either Transmission Kikuchi Diffraction (TKD) or transmission EBSD (t-EBSD) with a resolution down to approximately 10 nm. The goal with this master thesis has been to evaluate sample preparation methods and TKD studies on PVD samples. Each step has been divided into parameters which govern the sample preparation and analysis and optimized accordingly in order to achieve best possible results of the crystal structure of PVD coatings. From this it has been possible to show how TKD is optimally performed and which difficulties and limitations that are present. In this thesis two coatings, TiN and (Ti,Al)N, have been studied with TKD and two different preparation methods have been attempted. These were precision mechanical polishing and in-situ lift out with a Dual Beam System. Mechanical polishing did not succeed in producing samples for TKD but was not ruled out as a possibility while the in-situ lift out method could both produce samples and achieve a crystallographic indexing around 80 %. The only areas which were difficult to index were crystal boundaries and crystal clusters where individual crystals were in the range of <30 nm. In these areas overlapping Kikuchi patterns were observed due to the resolution limit of TKD.
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Chu, Lin-Yi, and 褚陵逸. "Analysis about the effect of initial grain size on Cu's DRX with SEM-EBSD." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/32362572389693070704.
Full textBook chapters on the topic "SEM-EBSD analysis"
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de Kloe, René, Hubert Schulz, and Felix Reinauer. "Advances in 3-dimensional material characterisation using simultaneous EDS and EBSD analysis in a combined FIB-SEM microscope." In EMC 2008 14th European Microscopy Congress 1–5 September 2008, Aachen, Germany. Springer Berlin Heidelberg, 2008. http://dx.doi.org/10.1007/978-3-540-85156-1_338.
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Schoß, Johannes Paul, Andreas Keßler, Claudia Dommaschk, Michal Szucki, and Gotthard Wolf. "Precipitation of Iron-Containing Intermetallic Phases from Aluminum Alloys by Metal Melt Filtration." In Multifunctional Ceramic Filter Systems for Metal Melt Filtration. Springer International Publishing, 2024. http://dx.doi.org/10.1007/978-3-031-40930-1_31.
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AbstractIron (Fe) provides a non-reactive dissolved impurity in aluminum (Al) alloys, which forms a coarse, plate-shaped intermetallic β-phase during solidification. This β-phase is detrimental to the mechanical and casting properties. Therefore, the reduction of Fe by binding in Fe-containing intermetal-lics (sludge phase) was realized via a two-stage procedure, which consisted of conditioning of the melt by manganese (Mn) and chromium (Cr) with subsequent-ly applied metal melt filtration. For this purpose, the formation characteristics of the Fe-rich intermetallic phases were investigated regarding the temperature, time, and initial chemical composition to separate these intermetallics from the residual melt. To evaluate the different process parameters of Fe removal for a potential implementation in lightweight metal foundries, a process technology on an indus-trial scale was developed in cooperation with an industrial partner. The examina-tion of samples in optical microscopy (OM) using image analysis were conducted to determine the area fractions of Fe-rich intermetallics. In addition, optical emis-sion spectrometer (OES) measurements were performed. Complementary investi-gations were achieved by scanning electron microscopy (SEM), with energy dis-persive spectroscopy (EDS), and electron backscatter diffraction (EBSD) to measure the partial chemical composition and for phase identification. The for-mation characteristics of the Fe-containing phases were investigated using DSC cooling curves and selective sampling in quenching experiments. In the experi-mental trials, a maximum reduction of iron of ≈50% was revealed compared to the unfiltered sample, whereby greater influence on the formation of α-intermetallics was inferred by temperature than by time. Moreover, the elements Mn and Cr were reduced by about 66% and 86% at 620 °C, respectively, thus, the element contents in the filtered samples approached the chemical composition of the standard alloy (EN-AC-AlSi9Cu3(Fe)).
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Field, David P., and Mukul Kumar. "Electron Backscatter Diffraction." In Encyclopedia of Aluminum and Its Alloys. CRC Press, 2019. http://dx.doi.org/10.1201/9781351045636-140000410.
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Electron backscatter diffraction (EBSD) is a scanning electron microscope (SEM) based technique that is used to obtain local information on the crystallographic character of bulk crystalline and polycrystalline materials. Topics discussed in this article include: EBSD system overview, multiphase analysis, and application to aluminum integrated circuit interconnects, dislocation structure analysis, analysis of grain boundary networks, and application to friction stir welding of aluminum alloys.
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Brito, Elizângela de Macêdo, Ângela Maria de Arruda, Ayrton de Sá Brandim, et al. "Microstructural and mechanical analysis of GMAW short-circuit welding on dual phase DP1000 steels for automotive applications." In Interconnections of Knowledge: Multidisciplinary Approaches. Seven Editora, 2024. http://dx.doi.org/10.56238/sevened2024.010-048.
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The article investigates welding methods applied to Dual Phase (DP) steels, with emphasis on the DP1000 class, aimed at the automotive industry. DP steels, known for their high mechanical resistance due to their specific microstructure, are attractive for manufacturing lighter, stronger and safer vehicles. The welding method chosen was GMAW by conventional short circuit, due to its efficiency and low cost. The characterization used advanced optical microscopy techniques, scanning electron microscopy with EDS, EBSD, in addition to tensile and hardness tests. Microstructural analyzes using optical microscopy (OM), scanning electron microscopy (SEM) and EBSD confirmed the presence of ferrite, martensite and, occasionally, austenite in the base metal, as specified by the DP1000 steel manufacturer. The molten zone (ZF) showed variations in hardness, with values close to the thermally affected zone (TAZ) due to decarburization and the presence of alloying elements in the steel. Microstructural analysis of the weld beads by SEM identified proeutectoid ferrite, martensite and retained austenite. The changes in the microstructural and mechanical properties observed did not compromise the essential characteristics of the material, confirming that the short-circuit GMAW process proved to be suitable for applications in the automotive industry.
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Aringozhina, Zarina, Bauyrzhan Rakhadilov, Didar Yeskermessov, Yerkezhan Tabiyeva, and Waqar Ahmed. "Electrolytic Plasma Treatment of Turkurite-Phase in High-Speed Steels." In Innovations in Materials Chemistry, Physics, and Engineering Research. IGI Global, 2023. http://dx.doi.org/10.4018/978-1-6684-6830-2.ch006.
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Scanning electron microscopy (SEM), EBSD-analysis, and X-ray structure (XRD) analysis were used to investigate the microstructure, morphology, elemental composition, phase composition, and crystal structure of M2 high speed steel after standard thermal treatment. It has been shown that the microstructure of the M2 high speed steel after hardening and three-time tempering consists of tempered martensite and solid carbide M6C-type and MC spherical shape. The volume fraction of carbides and their distribution have been defined. The main carbides in the study of steel after heat treatment – M6C and MС carbides who have a complex FCC lattice and space group Fd3m, have been established by X-ray structural analysis. Carbides are homogeneous and single crystal. EBSD-analysis method with the support of X-ray structural analysis has established that the bright carbides spherical shape M6C correspond to the composition Fe3W3C, and grey carbides spherical shape MC correspond to the composition of the VC.
Conference papers on the topic "SEM-EBSD analysis"
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He, Wenle, Raveendra Siriki, and Jerry Lindkvist. "Failure Analyses on a Super Duplex Stainless Steel Tube Material before and after Slow Strain Rate Testing in Sour Conditions – Part 1: SCC Susceptibility." In CONFERENCE 2022. AMPP, 2022. https://doi.org/10.5006/c2022-17998.
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Abstract For safely using duplex stainless steel and super duplex stainless steel, temperature-pH domains of stress corrosion cracking (SCC) resistance were provided by using slow strain rate testing (SSRT) screening in sour conditions in an earlier study. To follow-up the study, a failure analysis has been performed on the tube material of UNS S32750 and the specimens after the SSRT in a sour environment in pH 2.8, pH 3.5 at 80 °C. Scanning electron microscope (SEM) equipped by energy-dispersive X-ray spectrometer (EDS) analysis and Electron backscatter diffraction (EBSD) measurements have been used for the investigation on specimen surface, fracture surface and cross-sections of the SSRT specimens. Initiation of selective dissolution (SD) and cracking has been identified. EBSD reveals that cracking initiated in ferrite with enhanced strain/deformation in frontend of selectively dissolved austenite, where possible SCC mechanism seems to be hydrogen embrittlement. It observed that SD stopped in the brittle-ductile transition area in the fracture surface, which probably attributed to repassivation of the material in the condition of pH 3.5. Combined SSRT and analysis methods by SEM and EBSD showed a good way for the material evaluation before decision making for the materials selections and supplementary long-term exposures.
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He, Wenle, Raveendra Siriki, and Jerry Lindkvist. "Failure Analyses on a Super Duplex Stainless Steel Tube Material before and after Slow Strain Rate Testing in Sour Conditions – Part 2: a Case Study on Local Corrosion." In CONFERENCE 2022. AMPP, 2022. https://doi.org/10.5006/c2022-18320.
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Abstract A failure analysis has been performed and discussed in Part 1 on the tube material of UNS S32750 and the specimens which showed SCC susceptible after the SSRT in a sour environment in pH 2.8, pH 3.5 at 80 °C. In this Part 2, a case study has been performed on local corrosion on surface corrosion attack observed on two specimens. Scanning electron microscope (SEM) equipped by energy-dispersive X-ray spectrometer (EDS) analysis and Electron backscatter diffraction (EBSD) measurements have been used. On a specimen tested in pH 2.0 at 50 °C, selective dissolution (SD) has been identified in austenite and thin uniform corrosion on the surface in ferrite, no crack has been observed under the corrode surface. On a specimen tested in pH 4.5 at 80 °C, both SD and cracking have been observed under the line corrosion in shoulder area. EBSD revealed that micro cracks initiated in ferrite with enhanced strain/deformation in frontend of selectively dissolved austenite. Dry-wet condition is supposed, which would make the local condition of a thin liquid layer more severe compared to the bulk liquid testing condition. The surface analysis methods showed a good way for failure analysis, which might be helpful in other complicated cases.
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Galliopoulou, Eirini C., Christopher Jones, Lawrence Coghlan, et al. "Creep Cavitation Imaging and Analysis in 9%Cr-1%Mo P91 Steels." In AM-EPRI 2024. ASM International, 2024. http://dx.doi.org/10.31399/asm.cp.am-epri-2024p0219.
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Abstract The current research adopts a novel approach by integrating correlative microscopy and machine learning in order to study creep cavitation in an ex-service 9%Cr 1%Mo Grade 91 ferritic steel. This method allows for a detailed investigation of the early stages of the creep life, enabling identification of features most prone to damage such as precipitates and the ferritic crystal structure. The microscopy techniques encompass Scanning Electron Microscopy (SEM) imaging and Electron Back-scattered Diffraction (EBSD) imaging, providing insights into the two-dimensional distribution of cavitation. A methodology for acquiring and analysing serial sectioning data employing a Plasma Focused Ion Beam (PFIB) microscope is outlined, complemented by 3D reconstruction of backscattered electron (BSE) images. Subsequently, cavity and precipitate segmentation was performed with the use of the image recognition software, DragonFly and the results were combined with the 3D reconstruction of the material microstructure, elucidating the decoration of grain boundaries with precipitation, as well as the high correlation of precipitates and grain boundaries with the initiation of creep cavitation. Comparison between the 2D and 3D results is discussed.
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Park, Gyutae, Jinseok Seo, Majid Abbasi, and Yunjo Ro. "Failure of Light Naphtha Discharge Pump in a 2-Stage Overhead System of Condensate Splitting Unit." In CORROSION 2018. NACE International, 2018. https://doi.org/10.5006/c2018-10871.
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Abstract Corrosion of overhead system in the distillation unit has been a chronic and unresolved issue even with the injection of neutralizer and corrosion inhibitors. Recently, a light naphtha discharge pump (made of UNS J91150 casing and impeller) malfunctioned, which caused severe damage to the impeller. It was subsequently realized that, prior to the malfunction of the impeller, the pH of the water at the second overhead accumulator unexpectedly dropped to 2.6 with simultaneous increase of Fe concentration. Preliminary analysis of the impeller revealed that it had failed from a combination of corrosion and cavitation. To understand the origin of corrosion, extensive water chemistry analysis was performed, which revealed the presence of corrosive species such as sulfate and nitrate ions, presumably from the flue gas, which would have caused pH to drop. Autoclave corrosion tests also revealed that these species would cause significant corrosion of UNS S41000 which is similar to UNS J91150 used in the pump. In-depth electron microscope study (i.e., SEM, EBSD) on corrosion scale and damaged impeller surface was performed to confirm that the damage mechanism was corrosion-induced cavitation. Details of the analysis will be presented and discussed.
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Abraham, Geogy J., Kushal Singhla, and Vivekanand Kain. "Characteristics of Oxide Film Formed on UNS N08800 at High Temperature." In CORROSION 2014. NACE International, 2014. https://doi.org/10.5006/c2014-4209.
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Abstract UNS N08800 plate was subjected to cold working and machining operations and then exposed to high temperature steam for oxidation studies. The as-received, machined and cold worked specimens of UNS N08800 were characterized by electron back scattered diffraction (EBSD). Formation of nano-grains on the machined surface was clearly evident. The oxide film morphology was characterized by scanning electron microscopy (SEM) and micro laser Raman technique to understand the morphology and composition of the oxides formed at 400 °C steam. The oxide film formed was characterized by electrochemical impedance spectroscopy (EIS) to understand the film characteristics in terms of its defect density. The Raman analysis of oxide films showed broadening of the peaks which was attributed to formation of nano-grains on the machined UNS N08800 and due to stress from the cold working operation. The defect density from EIS for the oxide film formed on as-received was lower than cold worked sample. With machining, the oxide film defect density further increased suggesting a change in the nature of oxide film.
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Saithala, Janardhan Rao, Tim Illson, Mohammed Hachicha, and Sabrina Abdollah. "Corrosion Related Tube Failures in Amine Reboiler Units." In CORROSION 2013. NACE International, 2013. https://doi.org/10.5006/c2013-02368.
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Abstract Premature failure of tubes during service can be a major cause for the shutdown of refineries and gas processing plants. These failures not only cause a major delay in the production process and considerable financial losses, but also initiate emergency repair and maintenance. Amine waste heat reboilers in gas processing plant are critical as they regenerate the amine used for acid gas removal from sales quality gas. Failures in amine heating units can severely affect plant availability. This paper presents two case studies of tube failures related to amine waste heat reboiler units in a gas processing plant. The primary causes and mechanisms involved in the failures are investigated in detail using scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDX), x-ray diffraction (XRD), and electron backscattered diffraction techniques (EBSD) to determine the root cause. Results showed that several mechanisms were involved in tube failures. Pitting, stress corrosion cracking, oxidation, and softening due to spheroidization type corrosion mechanisms are involved in the final failure process. Remedial actions to avoid recurrent failures were also discussed.
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Chen, Lin, and Raymundo Case. "The Susceptibility of Nanostructured Steel to Sulfide Stress Corrosion Cracking as a Function of H2S Concentration, pH and Heat Treatment." In CORROSION 2021. AMPP, 2021. https://doi.org/10.5006/c2021-16365.
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Abstract The present work evaluates the sulfide corrosion cracking susceptibility of nanostructured bainitic steel with a dual-phase structure of bainite and retained austenite. Notch Tensile Slow Strain Rate Testing (NTSSRT) method was employed to assess the threshold stress intensity values (KISSCC). Microscopic morphology and analysis of fracture surface were carried out by scanning electronic microscope (SEM). Hydrogen sulfide (H2S) concentration with the range from 0.02 mole% to 35 mole% and pH value of 3.5 and 5.5 were controlled in 1% sodium chloride (NaCl) solution using sodium acetate/acetic acid buffer solution. The results show that KISSCC values are much lower in a more acidic environment. Heat treatment makes nanostructured steel more susceptible to SSC. Many secondary cracks were observed on the fracture surface, which may initiate from quasi cleavage caused by hydrogen in brittle fracture region. Inclusions can accelerate the crack propagation and failure process. Microscopic observation shows cracks can initiate from or arrested in austenite. Further relation between crack propagation and microstructure can be explored by employing Electron Backscatter Diffraction (EBSD) technique.
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Park, Hyunjoon, Sungyong Jang, Ihho Park, Hyungjin Lee, and Sungsu Cho. "A Study on Preferential Weld Metal Corrosion in UNS S31600 Austenitic Stainless Steels in HCl Containing Environment." In CORROSION 2019. NACE International, 2019. https://doi.org/10.5006/c2019-13248.
Full textAbstract:
Abstract UNS S31600 austenitic stainless steels have been routinely used to handle dry hydrogen chloride gases in petrochemical processes due to low corrosion rate. However, the presence of moisture increases the corrosion behavior by the formation of liquid hydrochloric acid. When UNS S31600 weld metals are exposed to hydrochloric acid solution, it is often found that weldments undergo severe corrosion compared to the base material. In order to clarify the mechanism of preferential UNS S31600 weldment corrosion, microstructural analysis was performed using SEM, TEM, and EBSD. In addition, laboratory immersion test was also conducted to understand the corrosion behavior in aerated hydrochloric acid solution. Corrosion attack preferentially occurred either at austenite in dendrite cores or ferrite in inter-and intra-dendritic boundary depending on the concentration of hydrochloric acid in solution. It is suggested that ferrite is more corrosion resistant to low concentration of hydrochloric acid solution than austenite due to the stability of passive film. On the other hand, in highly reducing hydrochloric acid solution, ferrite has inferior corrosion resistance compare to austenite. Galvanic corrosion between the two constituent phases is proposed to lead to selective weld metal corrosion.
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Huczkowski, P., A. Chyrkin, L. Singheiser, W. Nowak, and W. J. Quadakkers. "Corrosion Behavior of Candidate Heat Exchanger Materials in Oxidizing and Reducing Gases, Relevant to Oxyfuel Combustion." In CORROSION 2016. NACE International, 2016. https://doi.org/10.5006/c2016-07391.
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Abstract The so-called oxyfuel process is frequently considered as a promising technology for CO2 capture from the exhaust gas in fossil fuel fired power plants. In the present paper, the oxidation behavior of potentially suitable construction materials for heat exchanging components in coal fired power plants was studied at 650°C. The selected materials (martensitic steels, austenitic steels and a Ni-base alloy) were exposed in a simulated atmosphere typical for oxyfuel combustion and the results were compared with the behavior in a test gas simulating air-firing flue gas. Additionally a set of corrosion tests was performed in the simulated oxyfuel gas with addition of CO to simulate locally occurring reducing operating conditions. The oxidation/corrosion behavior was studied by gravimetry in combination with a number of characterization methods such as optical microscopy, scanning electron microscopy with energy dispersive x-ray analysis (SEM/EDS) and (for selected specimens) glow discharge optical emission spectroscopy (GDOES), x-ray diffraction (XRD) and electron backscatter diffraction (EBSD). The obtained results are interpreted on the basis of thermodynamic considerations comparing equilibrium activities of the main species in the gas atmospheres with the thermodynamic stabilities of various possibly forming solid and volatile corrosion products.
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Marchebois, Hervé, Bruce Cowe, and Thierry Cassagne. "Local Hard Zones on TMCP Large Diameter Line Pipes: What Do We Know about Their Metallurgy and Microstructure?" In CONFERENCE 2022. AMPP, 2022. https://doi.org/10.5006/c2022-17565.
Full textAbstract:
Abstract The manufacturing and field experience of steel plates used to manufacture line pipes produced by Thermo-mechanically Controlled Processing (TMCP) are well defined in industry standards and literature. Compared to the Quenched & Tempered heat treatment process, TMCP plates are designed with a leaner chemical composition combining micro-alloying elements, precipitation, recrystallization and phase transformation during rolling and accelerated cooling. Technical challenges and process improvements moved older generation TMCP pipes from coarse microstructures and presence of non-metallic inclusions and/or mid-thickness segregation, to finer, homogenized microstructures and improved properties typically present in modern TMCP pipes. Despite such an improvement, local hard zones (LHZ) have recently been experienced in the Oil & Gas industry on large diameter line pipes manufactured from TMCP plates. These LHZ must be distinguished from regular hard spot formation mechanisms known for years and highlighted in industry standards such as API† Spec. 5L / ISO‡ 3183. The current paper deals with a thorough analysis of these newly recognized LHZ with Scanning Electron Microscope (SEM) and Electron Back Scattering Diffraction (EBSD) investigations through the wall thickness of pipes. Internal diameter (ID) surface, intermediate zone and bulk metal microstructures showed an increase of a strong misorientation while approaching the ID. Thus, LHZ is characterized by the presence of lath and especially lower bainite type microstructures associated to high local hardness above the NACE MR 0175 / ISO 15156 limits for sour service applications.