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- Neutron radiography (5)
- LIBS (4)
- Hydrogen (3)
- Hydrogen diffusion (3)
- Hydrogen embrittlement (3)
- Welding (3)
- Blister (2)
- Diffusion (2)
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Organisationseinheit der BAM
We investigated hydrogen embrittlement and blistering in electrochemically hydrogen-charged technical iron samples at room temperature. Hydrogen-stimulated cracks and blisters and the corresponding hydrogen distributions were observed by neutron tomography. Cold neutrons were provided by the research reactor BER II to picture the sample with a spatial resolution in the reconstructed three-dimensional model of ~25 µm. We made the unique observation that cracks were filled with molecular hydrogen and that cracks were surrounded by a 50 µm wide zone with a high hydrogen concentration. The zone contains up to ten times more hydrogen than the bulk material. The hydrogen enriched zone can be ascribed to a region of increased local defect density. Hydrogen also accumulated at the sample surface having the highest concentration at blistered areas. The surfaces of the brittle fractured cracks showed micropores visualized by scanning electron microscopy. The micropores were located at grain boundaries and were surrounded by stress fields detected by electron backscattered diffraction. The cracks clearly originated from the micropores.
Neutron radiography (NR) is compared with the commonly used carrier gas hot extraction (CGHE) technique. We performed isothermal hydrogen effusion experiments at 623 K to study the mass transport kinetics. The investigated material was technical iron. The quantification of the hydrogen mass flow is done for NR by using concentration standards. The temporal hydrogen concentration evolution in the sample coincides well for both methods, i.e. NR and CGHE, and is in good agreement with literature. The advantages of the NR method are the non-destructive nature of measuring and the in-situ determination of hydrogen concentrations with high spatial and temporal resolution. Remaining hydrogen inside the sample can be identified directly by the NR method.
The purpose of the present study was to show the feasibility of measuring hydrogen effusion in austenitic stainless steel (1.4301) using neutron radiography at the facility ANTARES of the research reactor FRM II of the Technische Universität München. This method is appropriate to measure in-situ hydrogen effusion for hydrogen concentrations as small as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 533 K. The measurement principle is based on the parallel comparison of electrochemically hydrogen charged specimen with hydrogen-free reference specimen at the same temperature. This allows the determination of the hydrogen concentration in the specimens as a function of time and temperature. Separate hot carrier gas extraction experiments using the same temperature–time profiles as the radiography experiments have been used to calibrate the grey values of the neutron transmission images into hydrogen concentrations. It can be stated that the hydrogen effusion correlates with the specimen temperature.
Duplex stainless steels (DSS) are used in all industries where corrosion problems play a major role. Examples include the chemical industry, the food industry and shipping industries. DSS have a balanced phase ratio of ferrite (α) and austenite (γ). Unlike single-phase stainless steels, DSS combine the advantages of these and can therefore fit many industry requirements, such as weight saving or high mechanical strength. When these steels are welded, alloying elements can burn off and condense as thin layers on cold surface regions. This loss of chemical elements can lead to changes in the microstructure. With the help of Laser-Induced Breakdown Spectroscopy (LIBS), chemical element distributions were visualized. The results were compared with those of conventional measurement methods, such as energy dispersive X-ray analysis (EDS) and X-ray fluorescence analysis (XRF), and the results from LIBS could be validated. LIBS is suitable as a fast, straightforward measurement method for producing line scans along the weld seam and provides spatially resolved information on accumulation phenomena of burned off alloying elements. LIBS is very well suited for the detection of sub-surface elements due to the exclusively superficial ablation of the material. In addition, the measurement method has been calibrated so that quantitative statements about element concentrations can also be made.
In situ crack detection in the mushy zone and the solid weld of a gas tungsten arc (GTA) weld using X-ray imaging during welding is a new research area for NDT inspection. Usually, NDT flaw detection is done after the complete solidification of the weld seam. In this paper, we present the use of real-time radiography with a minifocus X-ray source (YXLON X-ray tube Y.TU 225-D04) and a 75μm pixel size digital detector array (Dexela 1512) for the acquisition of 2D radiographic images by a sequence of exposures with time intervals of 80 ms for hot crack detection during single pass bead-on-plate GTA welding of 3 mm thick plates of aluminium alloy AlMgSi (6060). An analysis of the crack distribution in the weld sample is conducted from the acquired 2D radiographs and its corresponding 3D volumetric reconstruction achieved by linear coplanar digital laminography.
This in situ approach opens new possibilities in the field of hot crack research by having the direct information of both the crack initiation and growth and its correlation to the welding parameters.
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.
The purpose of the present study is to show the feasibility of examining hydrogen desorption in technical iron samples using neutron radiography at the ANTARES facility of the FRM II research reactor, Technische Universität München. It has been shown that this method is appropriate for in situ determination of hydrogen Desorption for concentrations as low as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 260 °C. Measurement was based on direct comparison between electrochemically hydrogen-loaded iron samples and hydrogen-free reference samples at the same temperature.
This enables the determination of hydrogen concentration as a function of time and temperature. Ex situ carrier gas hot extraction experiments using the same temperature–time profiles as the neutron radiography experiments have been used to calibrate the greyscale values of the radiographs to defined hydrogen concentrations. It can be stated that hydrogen desorption correlates with sample temperature.
Neutron radiography and tomography have been used for a time resolved in situ analysis and a 3D mapping of hydrogen diffusion in iron and steel. Samples were electrochemically charged with hydrogen and afterwards neutron transmission images were taken. Hydrogen diffusion coefficients in duplex stainless steel were determined at 623 K by measuring and comparing the sample's mean intensity with a hydrogen-free reference sample and subsequent normalisation to standards with known hydrogen content. In technical iron and in supermartensitic stainless steel the hydrogen distributions have been investigated. The radiographic images in iron show blisters, cracks and the distribution of molecular hydrogen inside cracks. The analysis of the diffusion behaviour of hydrogen out of a blister illustrates the capabilities of the method with respect to time and spatial resolution. The neutron tomography of supermartensitic tensile stressed samples illustrates the capability to visualise hydrogen distributions three-dimensionally. -------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
On a utilisé la radiographie neutronique et la tomographie pour une analyse in situ à résolution temporelle et une cartographie 3D de la diffusion de l'hydrogène dans le fer et l'acier. On a chargé des échantillons par électrochimie avec de l'hydrogène et ensuite on a pris des images par émission de neutrons. On a déterminé les coefficients de diffusion de lhydrogène dans l'acier inoxydable duplex à 623 K en mesurant et en comparant l'intensité moyenne de l'échantillon avec un échantillon de référence sans hydrogène et une normalisation subséquente à des échantillons références à teneur connue en hydrogène. On a examiné la distribution d'hydrogène dans le fer technique et dans l'acier inoxydable supermartensitique. Les images radiographiques du fer montrent des soufflures, des fissures, et la distribution de l'hydrogène moléculaire à l'intérieur des fissures. L'analyse du comportement de diffusion de l'hydrogène hors d'une soufflure illustre les possibilités de la méthode par rapport à la résolution temporelle et spatiale. La tomographie neutronique des échantillons supermartensitiques chargés en traction illustre la capacité de visualiser les distributions d'hydrogène en trois dimensions.
Neutron tomography has been applied to investigate the mechanism of hydrogen assisted cracking in technical iron and supermartensitic steel. Rectangular technical iron block samples showed blistering due to intense hydrogen charging and the tomographic method revealed in situ the spatial distribution of hydrogen and cracks. Hydrogen accumulated in a small region around cracks and the cracks are filled with hydrogen gas. Cracks close to the surface contained no hydrogen. Hydrogenous tensile test samples of supermartensitic steel were pulled until rupture and showed hydrogen accumulations at the notch base and in the plastically deformed region around the fracture surface.