The evaluation of the impact of plasma-facing components damage on subsequent plasma operation is an important issue for ITER. During the first phase of the operation of WEST, a few ITER-like divertor plasma-facing units (PFUs) have been installed on the lower divertor. One PFU was pre-damaged under electron beam gun thermal loading, before its installation in WEST, and the subsequent evolution of the damage was studied after the WEST plasma exposure. This paper presents the procedure followed to get the pre-damaged PFU. It consists of the characterization of the response of tungsten samples representative of WEST PFU under high heat flux (HHF) loading, the selection of damage (namely, small cracks, crack network, crack network, and W melt droplets). Finally, according to the WEST plasma loading conditions, the blocks with damage within the PFU and the position of the pre-damaged PFU on the WEST lower divertor are attributed. The first results obtained after an initial plasma exposure in WEST lead to the assessment, as expected with regard to the heat loading conditions, that no major surface aspect modification was found. This result emphasized the possibility of implementing as pre-damaged small droplets of melted tungsten in a high heat-loaded zone for a future WEST experimental campaign.
Aluminum alloys have a strong tendency to form alumina layers on their surfaces when exposed to atmospheric air, even at room temperature. This is a severe challenge for brazing aluminum alloys as the alumina layer acts as a diffusion barrier and hinders the interactions between the filler metal and the base material. In order to achieve a good metallurgical bond between the filler metal and the aluminum alloy, it is of crucial importance to remove the alumina layer as well as to simultaneously prevent further oxidation of the aluminum alloy. The current investigation focuses on the detailed microstructural changes that occur during in-situ brazing of liquid filler metal, 95Sn-5Cu (wt.%) on an aluminum alloy, Al-7Si-0.3Mg. These in-situ studies were performed in a large chamber scanning electron microscope in order to monitor the interactions of the filler metal and the base material, particularly the role of Cu on alumina detachment. After the in-situ experiments, the local surface and cross-sectional regions were analyzed by scanning electron microscopy in conjunction with energy dispersive X-ray spectroscopy to understand the variation in chemistry across the wetted region, which includes the interfacial region between filler metal and the base material. As the alumina scale present on the aluminum alloy is very thin (<50 nm), nanoscale characterization techniques such as transmission electron microscopy in scanning mode, including selected area electron diffraction for crystal structure determination, were performed. From this investigation, it was found that the Cu in liquid filler metal diffuses into the base material via the oxide layer, resulting in the formation of Al2Cu intermetallic precipitates.
The present study demonstrates that in situ heating experiments in a LC-SEM are capable to provide hitherto not accessible insights into the kinetics of the brazing process. Continuous video documentation and temperature logging of the entire experiment yielded the on-set time of the wetting of the base material and the upper time limit that should not be exceeded to avoid quality losses of the joint. For the here investigated system of 75Sn20Cu5Ge filler metal with aluminum alloy EN AW-42100 base metal, the maximum holding time has been determined as 3.5 min at 450 ºC. The wetting point at this temperature is reached after one minute, which proves the effectiveness of the here investigated system.
Ferromagnetism is of increasing importance in the growing field of electromobility and data storage. In stable austenitic steels, the occurrence of ferromagnetism is not expected and would also interfere with many applications. However, ferromagnetism in austenitic stainless steels after low‐temperature nitriding has already been shown in the past. Herein, the presence of ferromagnetism in austenitic steels is discovered after low‐temperature carburization (Kolsterizing), which represents a novel and unique finding. A zone of expanded austenite is established on various austenitic stainless steels by low‐temperature carburization and the respective ferromagnetism is investigated in relation to the alloy composition. The ferromagnetism occurring is determined by means of a commercial magnetoinductive sensor (Feritscope). Ferromagnetic domains are visualized by magnetic force microscopy and a ferrofluid. X‐ray diffraction measurements indicate a clear difference in the lattice expansion of the different alloys. Furthermore, a different appearance of the magnetizable microstructure regions (magnetic domain structure) is detected depending on the grain orientation determined by electron backscatter diffraction (EBSD). Strongly pronounced magnetic domains show no linear lattice defects, whereas in small magnetizable areas linear lattice defects are detected by electron channeling contrast imaging and EBSD.
The non-proportional loading path describes a strain-dependent development of stress triaxiality and Lode parameter during metal forming processes. Existing studies suggest a strong dependence of damage evolution on the non-proportional loading path. This work focuses on investigating the influence of non-proportional loading paths observed in hot caliber rolling of the case-hardening steel 16MnCrS5 using laboratory scale experiments. The applied torsion plastometer is highly flexible as it can apply combined loading types (tension, compression and torsion) on notched round specimen and enables deformation at elevated temperature. In this study, two characteristic non-proportional loading paths in caliber rolling and the maximal achievable non-proportional loading path variation were recreated in the torsion plastometer based on both FE simulations and experiments. After deformation, the specimen were further analyzed using Scanning Electron Microscopy (SEM) to quantify the damage. The results indicate an influence of the non-proportional loading path on damage evolution. Furthermore, fatigue tests were employed to characterize the fatigue performance of the deformed specimens. In the torsion plastometer trials carried out no clear correlation of performance and damage was observed. This is most likely due to differences in residual dislocation density after static recrystallization and deviations in the microstructure after hot working. Thus, the superposition of microstructure evolution and damage needs to be considered carefully when testing at elevated temperature.
The amount of damage induced during hot forming depends not only on the stress state but also on material softening due to dynamic recrystallization (DRX), which can be used to delay or reduce damage initiation. An extension to the Gurson–Tvergaard–Needleman (GTN) model has been proposed recently that includes a new coupled DRX-damage nucleation criterion taking DRX and the stress state into account. In the present paper, a 4-pass caliber rolling process is considered where the bar stock is rotated by 90° after each rolling pass. The extended GTN model is applied to the caliber rolling process to predict the internal damage induced during the rolling process. The simulation results show that the highest void volume fraction (VVF) occurs during the first rolling pass. However, the variations of stress state during each pass assist in reducing the damage in the subsequent passes. The material softening due to increasing DRX in subsequent passes also helps to reduce the void nucleation. The microscopic analysis of the rolled bar confirms the damage distribution predicted by the simulations.
In modern multiphase materials, damage initiation and growth during plastic deformation is a commonly observed and technologically relevant process. To reliably assess the state of damage in a specimen or, ultimately, a formed product, precise and comparable damage quantification is required. Furthermore, the key to understanding the initiation and evolution of voids in such materials is the characterization of the initiating microstructural mechanisms in a statistically relevant way over a large number of damage sites. In this work, we present the results of large-scale scanning electron microscopy methods for automated damage recognition and analytical characterization, together with a concept for joining the available void size statistics to micromechanical experiments such as micro-cantilever tests. These tests are able to determine a critical crack length for various types of void initiation processes, leading to an improved understanding of the consequences of ductile damage evolution and void growth, and their subsequent interaction leading to material failure. In this way, a framework for quantification and high-resolution characterization of damage mechanisms is constructed, enabling new insights on damage evolution in forming processes.
The anticoagulation treatment of cardiovascular patients, which is mandatory after implantation of heart valves or stents, has significantly adverse effects on life quality. This treatment can be reduced or even circumvented by developing novel antithrombogenic surfaces of blood-contacting implants. Thus, we aim to discover materials exhibiting outstanding hemocompatibility compared to other available synthetic materials. We present promising surficial characteristics of single crystalline alumina in terms of platelet activation inhibition. In order to elucidate the relation between its crystallographic properties including the plane orientation and blood cell behavior, we examined endothelialization, cytocompatibility, and platelet activation at the blood-alumina interfaces in a controlled experimental setup. We observed that the cell response is highly sensitive to the plane orientation and differs significantly for (0001) and (11-20) planes of Al2O3. Our results reveal for the first time the dependence of platelet activation on crystallographic orientation, which is assumed to be a critical condition controlling the thrombogenicity. Additionally, we used an endothelial cell monolayer as an internal control since endothelial cells have an impact on vessel integrity and implant acceptance. We successfully demonstrate that Al2O3(11-20) exhibits enhanced hemocompatibility in contrast to Al2O3(0001) and is comparable to the physiological endothelial monolayer in vitro.
In addition to strain hardening and residual stress, damage influences the product performance of forward rod extruded parts. Damage is usually neglected and difficult to quantify. The evolution of ductile damage in metal forming is closely correlated to the load path. An experimental approach using automated energy dispersive X-ray spectroscopy (EDX) particle analysis in scanning electron microscopy (SEM) is used to successfully quantify the void area fraction and obtain information on ductile damage. The method is performed on forward rod extruded 16MnCrS5 workpieces with varying extrusion strains and shoulder opening angles (and thus varying underlying load paths). The quantified damage is directly correlated to the load path, which can be described by the stress triaxiality evolution during forming. Density measurements were performed to further validate the results. By observing the change of strain-weighted stress triaxiality and maximum stress triaxiality, it is shown, that the maximum stress triaxiality is the decisive parameter enabling void nucleation.
The zinc coating layer fracture properties of a galvannealed steel and an electrolytically galvanized steel are analyzed by conducting the in-situ bending test with newly designed samples. It is found that the fracture develops much earlier in the coating layers of the galvannealed steel than that of the electrolytically galvanized steel. Using transmission electron microscope and energy dispersive X-ray spectroscopy, the intermetallic phases of the coating layers are characterized and it is found that the early crack initiation in a galvannealed steel is mainly triggered in the gamma phase. Combining with nanoindentation tests and corresponding simulation, the deformability of intermetallic phases are analyzed to explain the failure behavior of coating layers in the two steels.
Materialwissenschaft und WerkstofftechnikVolume 48, Issue 12 p. 1203-1205 Contents/InhaltFree Access Mat.-wiss. u. Werkstofftech. 12/2017 First published: 10 January 2018 https://doi.org/10.1002/mawe.201781211AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume48, Issue12December 2017Pages 1203-1205 RelatedInformation
This chapter contains five sections related to advances in technology and characterization. The first section investigates influence of Ti top electrodes on the oxidation state of epi-taxially grown STO thin films and the corresponding resistive switching devices. The second section shows comparison of work diode- and CO2-laser heater versions. The third section reviews the influence of ALD processing and different top electrodes on the structural, morphological and electrical properties of ZrO2. The fourth section views the resistance switching characteristic of Nb2O5 thin films integrated into Pt/Nb2O5/Ti/Pt micro cross bar structures on Si/SiO2 substrates. The fifth section considers the investigations of CDW in Dy5Ir4Si10 at different temperatures using transmission electron microscopy (TEM) techniques including electron diffraction and dark-field imaging. Controlled Vocabulary Terms electron diffraction; switching; thin films; transmission electron microscopy
Background: Coral reef aorta is a rare vascular disease with intraluminal calcifications of the dorsal part of the visceral aorta. The pathogenesis of this disease with its topographic and morphologic characteristics is unknown. The aim of our study was to investigate calcification inhibitors and the ultrastructure of calcifications in patients with coral reef aorta.Methods: Ten patients with coral reef aorta were examined. Calcified specimens were investigated by immunohistochemical techniques for the expression of the calcification inhibitors matrix gla protein (MGP) and fetuin-A. Vessel walls were also assessed by electron microscopic techniques including electron energy-lost spectroscopy, electron dispersive spectroscopy, and electron diffraction. Sera of patients were analyzed for fetuin-A, uncarboxylated MGP (ucMGP), and osteoprotegerin.Results: As assessed by immunohistochemistry, most MGP was detected in the vicinity of calcified regions. Serum levels of the calcification inhibitors ucMGP, fetuin-A, and osteoprotegerin were 370 +/- 107 nmol/L, 0.57 +/- 0.03 g/L, and 5.64 +/- 0.79 pmol/L, respectively. Ultrastructural analysis of calcified specimens showed a core-shell structure with multiple calcification nuclei. calcifications displayed a. ne-crystalline character, and elemental analysis revealed hydroxyl apatite as the chemical compound.Conclusion: The coral reef aorta represents an extreme exophytic growth of vascular calcification with multiple nuclei which resemble typical media calcification. Positive vascular immunostaining and low serum levels of both fetuin-A and ucMGP suggest a pathophysiologic role of these calcification inhibitors in the development of coral reef aorta.
Accelerated intimal and medial calcification and sclerosis accompany the increased cardiovascular mortality of dialysis patients, but the pathomechanisms initiating microcalcifications of the media are largely unknown. In this study, we systematically investigated the ultrastructural properties of medial calcifications from patients with uremia. We collected iliac artery segments from 30 dialysis patients before kidney transplantation and studied them by radiography, microcomputed tomography, light microscopy, and transmission electron microscopy including electron energy loss spectrometry, energy dispersive spectroscopy, and electron diffraction. In addition, we performed synchrotron x-ray analyses and immunogold labeling to detect inhibitors of calcification. Von Kossa staining revealed calcification of 53% of the arteries. The diameter of these microcalcifications ranged from 20 to 500 nm, with a core-shell structure consisting of up to three layers (subshells). Many of the calcifications consisted of 2- to 10-nm nanocrystals and showed a hydroxyapatite and whitlockite crystalline structure and mineral phase. Immunogold labeling of calcification foci revealed the calcification inhibitors fetuin-A, osteopontin, and matrix gla protein. These observations suggest that uremic microcalcifications originate from nanocrystals, are chemically diverse, and intimately associate with proteinaceous inhibitors of calcification. Furthermore, considering the core-shell structure of the calcifications, apoptotic bodies or matrix vesicles may serve as a calcification nidus.
Conclusion L’aorte de type « coral reef » représente une croissance exophytique vasculaire extrême de calcifications à noyaux multiples, mimant les calcifications typiques de la média. Un marquage positif en immunohistochimie et des niveaux sériques bas en fétuine-A et ucMGP suggèrent un rôle physiopathologique de ces inhibiteurs de calcification dans le développement de lésions de type « coral reef ».
The serum protein fetuin-A is a potent systemic inhibitor of soft tissue calcification. Fetuin-A is highly effective in the formation and stabilization of protein-mineral colloids, referred to as calciprotein particles (CPPs). These particles ripen in vitro in a two-step process, indicated by a morphological conversion from spheres to larger prolate ellipsoids. Using a combined light scattering and electron microscopic imaging approach we determined that the second-stage particles resulted from a highly anisotropic outgrowth of the first-stage particles. Electron microscopy of ascites fluid from a patient with calcifying peritonitis revealed particles reminiscent of secondary CPPs. Thus, CPPs form in the body and undergo the two-step ripening at least in pathological conditions. Unlike in vitro generated CPPs, ascites-derived CPPs contained little fetuin-A but large amounts of albumin. This prompted us to study the role of fetuin-A combined with other serum proteins in CPP formation. Fetuin-A was indispensable for primary CPP formation. Albumin and acidic proteins in general greatly enhanced the fetuin-A triggered formation of secondary CPPs and, thus, substituted substantial amounts of fetuin-A without loss of inhibition of calcium phosphate precipitation. Thus, direct mineral deposition from solute in the body is unlikely even at low fetuin-A serum levels as long as sufficient bulk acidic protein is available. Collectively fetuin-A and other acidic bulk plasma proteins may be considered as mineral chaperones mediating the stabilization, safe transport, and clearance in the body of calcium and phosphate as colloidal complexes, thus, preventing ectopic calcification.