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- X-ray refraction (23)
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While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture.
For the first time, synchrotron X-ray refraction radiography (SXRR) has been paired with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to disintegrate and spherodize into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state.
Using SXRR to Probe the Nature of Discontinuities in SLM Additive Manufactured Inconel 718 Specimens
(2020)
The utilization of additive manufacturing (AM) to fabricate robust structural components relies on understanding the nature of internal anomalies or discontinuities, which can compromise the structural integrity. While some discontinuities in AM microstructures stem from similar mechanisms as observed in more traditional processes such as casting, others are unique to the AM process. Discontinuities in AM are challenging to detect, due to their submicron size and orientation dependency. Toward the goal of improving structural integrity, minimizing discontinuities in an AM build requires an understanding of the mechanisms of formation to mitigate their occurrence. This study utilizes various techniques to evaluate the shape, size, nature and distribution of discontinuities in AM Inconel 718, in a non-hot isostatic pressed (HIPed) as-built, non-HIPed and direct age, and HIPed with two step age samples. Non-destructive synchrotron radiation refraction and transmission radiography (SXRR) provides additional information beyond that obtained with destructive optical microscopy. SXRR was able to distinguish between voids, cracks and lack of melt in, due to its sensitivity to the orientation of the discontinuity.
The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments.
Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphological features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in two aluminum titanate ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity content implies a larger isotropy of both the crystal texture and the porosity orientation. We also found that, analogous to cordierite, crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it.
Porosity in additively manufactured materials, such as laser powder bed fusion Ti-Al6-V4, can play an important role in their mechanical performance. Not only the total porosity but also the shape/morphology of the individual pores need to be considered. Therefore, it is necessary to determine the distributions of different defect types (especially fusing defects and keyhole pores) and their dependence on process parameters. We show that synchrotron X-ray refraction radiography allows analysis of large samples (up to several millimeters) without compromising the detectability of submicrometer defects. Correspondingly, a classification tool is introduced that is able to quantitatively distinguish defects such as keyhole pores and binding defects with a confidence level of 94 %, even when the shape cannot be discerned because of limited spatial resolution.
Um das Material- und Schädigungsverhalten von additiv gefertigtem Polyamid 12 (PA12) unter quasistatischer Belastung zu charakterisieren, wurden mechanische Tests und Röntgenverfahren zur Bestimmung der Mikrostruktur eingesetzt. Die Proben wurden nach dem Prinzip des Selektiven Lasersinterns (SLS) hergestellt. Unter quasistatischer Belastung mit Haltezeiten ergab sich ein viskoplastisches Materialverhalten. Im Zugversuch wurde eine maximale Zugfestigkeit von 40.6 MPa und eine Bruchdehnung von 7.4% beobachtet. Mittels Röntgenrefraktion wurde eine Erhöhung von inneren Oberflächen beobachtet, die senkrecht zur Zugrichtung orientiert sind. Die Analyse der Gesamtporosität aus Computertomographie-Messungen ergab keine Änderung infolge der Zugbelastung. Jedoch wurde eine bimodale Porengrößenverteilung und eine steigende Sphärizität festgestellt. Das Materialverhalten wurde mit dem Chaboche-Modell simuliert und ergab eine sehr gute Übereinstimmung mit den experimentellen Ergebnissen. Allerdings gestattet dieses Modell nicht, das Schädigungsverhalten abzubilden. Daher wurde zur Simulation des Schädigungsverhaltens das Modell gemäß dem Ansatz von Gurson, Tvergaard und Needleman unter Berücksichtigung der mikrostrukturellen Parameter erweitert. Der Schwerpunkt des Beitrags liegt auf den Röntgenverfahren zur experimentellen Bestimmung der Mikrostruktur.
Die Degradation von Wärmedämmschichten(thermal barrier coatings - TBCs) in Gasturbinen durch glasartige Calcium-Magnesium-Aluminiumsilikat (CMAS)Ablagerungen aus verschiedenen Quellen istseit vielen Jahren ein anhaltendes Problem. In dieser Studie wurde mit Hilfe derSynchrotron-Röntgen-Refraktions-Radiographie (SXRR), und vergleichend mit der Elektronenmikroskopie, das Eindringen von CMAS in die poröse Struktur von atmosphärisch plasmagespritzten (APS)TBCs sowie die Bildung und das Wachstum von Rissen unter thermisch zyklischer Belastung untersucht. Die Ergebnisse deuten darauf hin, dass die Infiltration sowie deren Kinetik im Brenner-Teststand wesentlich vom Benetzungsverhalten des CMAS beeinflusst werden. Trotz desoffensichtlichen Angriffs von CMAS auf die Korngrenzen hat die Wechselwirkung von Yttriumdioxid-stabilisiertem Zirkoniumdioxid (YSZ) mit intrudiertem CMAS keinen unmittelbaren Einfluss auf die Struktur und Dichte der innen Oberflächen(Risse, Poren). In einem späteren Stadium wird die Bildung von Rissen senkrecht zur äußeren Oberfläche in einer breiteren Zone der TBC-Schicht beobachtet.
While structural ceramics usually display a brittle mechanical behavior, their composites may show nonlinearities, mostly due to microcracking. Herein, the stiffness evolution of a sandwich-like laminate of an Al2O3 15%vol. ZrO2 matrix reinforced with Nextel 610 fibers is studied as a function of number of cycles N in tension. The stiffness of the composite degrades with increasing N, indicating microcracking. However, synchrotron X-ray refraction radiography shows that the internal specific surface of such cracks varies differently. A modeling strategy is developed for the calculation of the equivalent stiffness of mixtures (first the matrix and then the sandwich), based on the Voigt and Reuß schemes. The Bruno–Kachanov model is then used to estimate the initial microcrack density in the matrix (due to the thermal expansion mismatch) and the amount of microcracking increase upon cyclic loading. The stiffness in the composite degrades dramatically already after 20 000 cycles but then remains nearly constant. The combination of mechanical testing, quantitative imaging analysis, and modeling provides insights into the damage mechanisms acting: microcrack propagation is more active than microcrack initiation upon cyclic loading, but the second also occurs. This scenario is similar but not equal to previous results on porous and microcracked ceramics.