TY - GEN A1 - Griesche, Axel A1 - Beyer, Katrin A1 - Kannengießer, Thomas A1 - Calzada, E. T1 - Hydrogen diffusion measurements in steels using neutron imaging N2 - Revealing hydrogen embrittlement mechanisms in steels is of great interest to scientists and engineers. Neutron radiography makes it possible to measure in-situ hydrogen diffusion with high spatial and temporal resolution at concentrations as low as 20 ppm. We compare hydrogen-charged specimens with hydrogen-free reference specimens and use calibration standards to normalize the hydrogen concentrations. This allows quantitative tracking of the hydrogen concentration evolution as a function of time, space and temperature. Furthermore, a view into the material with 'neutron eyes' facilitates the detection of cavities that contain molecular hydrogen. KW - Hydrogen KW - Diffusion KW - Steel KW - Neutron radiography PY - 2012 UR - http://cdn.frm2.tum.de/fileadmin/stuff/information/documents/annualReports/Annual_Report_2011_online_version.pdf SP - 50 EP - 51 AN - OPUS4-25981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, Katrin A1 - Kannengießer, Thomas A1 - Griesche, Axel A1 - Schillinger, B. T1 - Neutron radiography study of hydrogen desorption in technical iron N2 - 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. KW - Neutron radiography KW - Hydrogen PY - 2011 U6 - https://doi.org/10.1007/s10853-011-5450-7 SN - 0022-2461 SN - 1573-4803 VL - 46 IS - 15 SP - 5171 EP - 5175 PB - Springer Science + Business Media B.V. CY - Norwell, Mass. AN - OPUS4-25150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel A1 - Dabah, Eitan A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Kannengießer, Thomas T1 - Neutron imaging of hydrogen in steels T2 - Materials Science & Technology (MS&T) 2013 CY - Montreal, Quebec, Canada DA - 2013-10-27 KW - Neutron radiography KW - Hydrogen KW - Diffusion KW - Steel PY - 2013 SP - 945 EP - 950 PB - Curran CY - Red Hook, NY AN - OPUS4-29506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Solórzano, E. A1 - Beyer, Katrin A1 - Kannengießer, Thomas T1 - The advantage of using in-situ methods for studying hydrogen mass transport: Neutron radiography vs. carrier gas hot extraction N2 - 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. KW - Hydrogen diffusion KW - In-situ KW - Neutron radiography KW - Carrier gas hot extraction KW - Imaging PY - 2013 U6 - https://doi.org/10.1016/j.ijhydene.2013.08.145 SN - 0360-3199 VL - 38 IS - 34 SP - 14725 EP - 14729 PB - Elsevier CY - Oxford AN - OPUS4-29413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas T1 - Spatially resolved EDS, XRF and LIBS measurements of the chemical composition of duplex stainless steel welds: A comparison of methods N2 - 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. T2 - EMSLIBS 2021 CY - Online Meeting DA - 25.11.2021 KW - LIBS KW - TIG welding KW - Duplex stainless steel KW - XRF KW - EDS PY - 2022 U6 - https://doi.org/10.1016/j.sab.2022.106439 SN - 0584-8547 VL - 193 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-54837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas T1 - In situ investigation of chemical composition during TIG welding in duplex stainless steels using Laser-Induced Breakdown Spectroscopy (LIBS) N2 - Many applications in industry require a material-to-material joining process of Duplex Stainless Steels (DSS). Therefore, it is essential to investigate the material’s properties during a welding process to control the weld quality. With the help of Laser-Induced Breakdown Spectroscopy (LIBS), the chemical composition during the Tungsten Inert Gas (TIG) welding process of DSS could be monitored in situ. The chemical composition could be quantitatively measured using pre-established calibration curves. Although the surface temperature and the welding plasma have a high influence on the spectral intensities, reliable composition measurements were possible. The concentration of alloying elements could be mapped during the TIG welding process. T2 - 2nd International Conference on Advanced Joining Processes CY - Sintra, Portugal DA - 21.10.2021 KW - LIBS KW - In situ measurement KW - WRC 1992 diagram KW - TIG welding KW - Duplex stainless steels PY - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-542026 SN - 2666-3597 VL - 6 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-54202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Schaupp, Thomas A1 - Griesche, Axel A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Hannemann, Andreas A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - Quantitative analysis of hydrogen-assisted microcracking in duplex stainless steel through X-ray refraction 3D imaging N2 - 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. KW - 2101 duplex stainless steel KW - Hydrogen embrittlement KW - Synchrotron radiation KW - X-ray refraction KW - Computed tomography KW - Microcracking PY - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-542811 SN - 1438-1656 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas T1 - Rapid solidification during welding of duplex stainless steels – in situ measurement of the chemical concentration by Laser-Induced Breakdown Spectroscopy (LIBS) N2 - Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process. T2 - ICASP-6 CY - Le Bischenberg, France DA - 20.06.2022 KW - LIBS KW - In situ measurement KW - Duplex stainless steel KW - TIG welding KW - Evaporation PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-571308 VL - 1274 SP - 1 EP - 8 PB - IOP Publishing CY - Bristol AN - OPUS4-57130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boateng, Francis Twumasi A1 - Ewert, Uwe A1 - Kannengießer, Thomas A1 - Zscherpel, Uwe A1 - Griesche, Axel A1 - Kromm, Arne A1 - Hohendorf, Stephan A1 - Redmer, Bernard T1 - Real-time radiography for observation of crack growth during GTA (Gas Tungsten Arc) welding N2 - 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. KW - Hot cracking KW - Radiography KW - GTA welding KW - Aluminium alloys KW - Real-time operation PY - 2016 U6 - https://doi.org/10.1007/s40194-016-0351-7 SN - 0043-2288 SN - 1878-6669 VL - 60 IS - 5 SP - 931 EP - 937 AN - OPUS4-37128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gollnow, C. A1 - Griesche, Axel A1 - Weidemann, Jens A1 - Kannengießer, Thomas T1 - Influence of external loads on a characteristic angle between grains and solidus line as an indicator for hot cracking susceptibility during GTA welding N2 - A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion. KW - Hot cracking KW - External load test KW - Component design KW - Crack criterion KW - Grain growth PY - 2017 U6 - https://doi.org/10.1016/j.jmatprotec.2016.08.013 VL - 239 SP - 172 EP - 177 PB - Elsevier AN - OPUS4-37278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dabah, Eitan A1 - Griesche, Axel A1 - Beyer, Katrin A1 - Solórzano, E. A1 - Kannengießer, Thomas ED - Kannengießer, Thomas ED - Babu, S. S. ED - Komizo, Y. ED - Ramirez, A.J. T1 - In situ measurements of hydrogen diffusion in duplex stainless steels by neutron radiography N2 - Hydrogen embrittlement (HE) is a widely known phenomenon and under investigation already for more than a century. This phenomenon, though thoroughly studied, is not yet completely understood, and so far, there are several suggested mechanisms that try to explain the occurrence of HE. One important factor of understanding the HE phenomenon and predicting hydrogen-assisted failure is the descent knowledge about the hydrogen transport behaviour in the material. Neutron radiography is a proven method for tracking hydrogen diffusion and it was applied successfully in various research studies. In the presented study, we examined the hydrogen effusion behaviour in duplex stainless steel by means of neutron radiography and calculated the effective diffusion coefficient from the obtained transmission images. KW - Neutron radiography KW - Hydrogen diffusion KW - Duplex stainless steels KW - Hydrogen embrittlement PY - 2014 SN - 978-3-319-06144-3 SN - 978-3-319-06145-0 U6 - https://doi.org/10.1007/978-3-319-06145-0_9 SP - 155 EP - 163 PB - Springer AN - OPUS4-31357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Dabah, Eitan A1 - Kardjilov, N. A1 - Hilger, A. A1 - Manke, I. A1 - Kannengießer, Thomas T1 - Imaging of hydrogen in steels using neutrons N2 - We investigated the hydrogen distribution spatially and temporally in technical iron at room temperature. Samples were charged electrochemically and subsequently analysed by means of neutron radiography and tomography. The radiographic images allowed for a time-resolved analysis of hydrogen fluxes. The three-dimensional distribution of hydrogen measured by neutron tomography delivered valuable information for the damage analysis of hydrogen-induced cracks. For the first time hydrogen concentration gradients inside the material could be detect directly together with the cracks. The neutron radiography and tomography results were gained at the Research Reactor BER II of the HZB in Berlin. KW - Hydrogen embrittlement KW - Hydrogen diffusion KW - Neutron tomography KW - Blister PY - 2014 U6 - https://doi.org/10.3139/146.111043 SN - 1862-5282 VL - 105 IS - 7 SP - 640 EP - 644 PB - Carl Hanser CY - München AN - OPUS4-31084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Dabah, Eitan A1 - Kannengießer, Thomas A1 - Kardjilov, N. A1 - Hilger, A. A1 - Manke, I. T1 - Three-dimensional imaging of hydrogen blister in iron with neutron tomography N2 - 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. KW - Hydrogen embrittlement KW - Hydrogen diffusion KW - In situ KW - Neutron tomography KW - Iron PY - 2014 U6 - https://doi.org/10.1016/j.actamat.2014.06.034 SN - 1359-6454 SN - 1873-2453 VL - 78 SP - 14 EP - 22 PB - Elsevier Science CY - Kidlington AN - OPUS4-31068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, Katrin A1 - Kannengießer, Thomas A1 - Griesche, Axel A1 - Schillinger, B. T1 - Study of hydrogen effusion in austenitic stainless steel by time-resolved in-situ measurements using neutron radiography N2 - 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. KW - Hydrogen effusion KW - Austenitic stainless steels KW - Neutron radiography PY - 2011 U6 - https://doi.org/10.1016/j.nima.2011.02.010 SN - 0168-9002 SN - 0167-5087 VL - 651 IS - 1 SP - 211 EP - 215 PB - North-Holland CY - Amsterdam AN - OPUS4-23401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - 3D imaging of hydrogen assisted cracking using analyser-based imaging N2 - To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution. However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample. To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld. T2 - BESSY User Meeting 2015 CY - Berlin, Germany DA - 09.12.2015 KW - X-ray refraction KW - Synchrotron KW - Analyser-based imaging KW - Hydrogen assisted cracking KW - Welding PY - 2015 AN - OPUS4-38278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - 3D imaging of hydrogen assisted cracking in metals using refraction enhanced synchrotron CT N2 - Hydrogen in metals can cause a degradation of the mechanical properties with possible subsequent hydrogen assisted cracking (HAC). Though, the mechanism of HAC is not completely understood yet and thus suitable methods for in situ investigations to characterise the crack formation are needed. X-ray computed tomography (CT) is a well-known tool for analysing these properties. However, the effective resolution of the detector system limits the detection of small defects by CT. Analyser based imaging (ABI) takes advantage of x-ray refraction at interfaces between volumes of different density, i.e. of cracks, pores, inclusions, etc., within the sample to detect defects smaller than the resolution of the detector system. In this study, measurements on an aluminium alloy weld showed that ABI allows us to resolve the 3D structure of cracks undetected by absorption based CT. Prospective investigations will analyse HAC in steels. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 2015-09-15 KW - Wasserstoffversprödung KW - Wasserstoffunterstützte Rissbildung KW - Röntgenrefraktion KW - CT KW - Hydrogen embrittlement (HE) KW - Hydrogen assisted cracking (HAC) KW - Aluminium alloy KW - X-ray refraction KW - Analyser based imaging KW - Computed tomography (CT) KW - Synchrotron radiation PY - 2015 SN - 1435-4934 SP - 1217 EP - 1224 AN - OPUS4-34287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Dabah, Eitan A1 - Kannengießer, Thomas A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Schillinger, B. T1 - Measuring hydrogen distributions in iron and steel using neutrons N2 - 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. T2 - 10th World Conference on Neutron Radiography (WCNR) CY - Grindelwald, Switzerland DA - 05.10.2014 PY - 2015 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-348022 SN - 1875-3892 VL - 69 SP - 445 EP - 450 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-34802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Dabah, Eitan A1 - Kannengießer, Thomas T1 - Neutron imaging of hydrogen in iron and steel N2 - 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 l’hydrogène 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. KW - Neutron radiography KW - Hydrogen KW - Diffusion KW - Iron KW - Steel KW - Blister KW - Hydrogen assisted cracking PY - 2015 U6 - https://doi.org/10.1179/1879139514Y.0000000162 SN - 0008-4433 VL - 54 IS - 1 SP - 38 EP - 42 PB - Canadian Institute of Mining and Metallurgy CY - Montreal AN - OPUS4-32809 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - 3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT N2 - Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network. T2 - WCNDT 2016 CY - München, Germany DA - 13.06.2016 KW - X-ray refraction KW - Computed tomography KW - Hydrogen assisted cracking KW - Duplex stainless steel PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-366481 SN - 978-3-940283-78-8 VL - BB 158 SP - Tu.4.B.3, 1 EP - 9 AN - OPUS4-36648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taparli, Ugur Alp A1 - Kannengießer, Thomas A1 - Griesche, Axel T1 - Tungsten inert gas bead-on-plate weld chemical composition analysis by laser-induced breakdown spectroscopy N2 - Chemical compositions of a weld can be varying locally as a result of the welding process. These local variations can be due to the vaporization of individual alloying elements. In this work, tungsten inert gas (TIG) bead-on-plate stainless steel welds of EN grade 1.4404 and 1.4435 were investigated using laser-induced breakdown spectroscopy (LIBS) on the completed welds. This study aims to reveal the welding parameters’ influence on the resulting local chemical compositions of the stainless steel welds. We demonstrated Mn vaporize before Cr due to its lower latent enthalpy of vaporization. Hence, Mn accumulates on the heat-affected zone (HAZ) both sides across the weld bead by being swept away through the circulation flow of the welding plasma. Additionally, increasing the heat input tends to enhance the accumulated Mn content on the HAZ as well as increasing the shielding gas flow rate. The results are in good agreement with the literature and proved that LIBS is an effective method to inspect completed welds. T2 - Symposium on Materials and Joining Technology CY - Magdeburg, Germany DA - 07.09.2020 KW - LIBS TIG welding KW - Austenitic stainless steels KW - Chemical composition KW - In situ measurement PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-511595 SN - 1757-8981 SN - 1757-899X VL - 882 IS - 012023 SP - 1 EP - 8 PB - IOP Publishing CY - Bristol AN - OPUS4-51159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taparli, Ugur Alp A1 - Kannengießer, Thomas A1 - Cieslik, K. A1 - Mory, D. A1 - Griesche, Axel T1 - In situ chemical composition analysis of a tungsten-inert-gas austenitic stainless steel weld measured by laser-induced breakdown spectroscopy N2 - The chemical composition of a weld metal determines the resulting solidification mode of stainless steel and the consequent weld metal quality. In this work tungsten inert gas (TIG) welding of EN grade 1.4435 austenitic stainless steel was monitored using laser-induced breakdown spectroscopy (LIBS) for the in situ measurement of chemical composition changes. This research aims to prototype a real-time chemical composition analysis system for welding applications and prove the feasibility of such quality control loop. LIBS was used to investigate in situ the monitoring of metal vaporization during TIG welding. We found Mn vapor formation above the weld pool and subsequent condensation of Mn on the weld metal surface using LIBS. Post-weld line scans were conducted by LIBS on various welds produced with different welding currents. Local changes of Ni and Mn were observed at higher welding currents. The results are in good agreement with the literature and proved that LIBS can be used in situ to inspect the TIG welding process. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brünn, Czechia DA - 08.09.2019 KW - LIBS KW - Welding KW - Austenitic stainless steel KW - Metal vapor KW - In situ measurement PY - 2020 U6 - https://doi.org/10.1016/j.sab.2020.105826 SN - 0584-8547 VL - 167 SP - 105826 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-50582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taparli, Ugur Alp A1 - Jacobsen, Lars A1 - Griesche, Axel A1 - Michalik, Katarzyna A1 - Mory, David A1 - Kannengießer, Thomas T1 - In situ laser-induced breakdown spectroscopy measurements of chemical compositions in stainless steels during tungsten inert gas welding N2 - A laser-induced breakdown spectroscopy (LIBS) system was combined with a bead-on-plate Tungsten Inert Gas (TIG) welding process for the in situ measurement of chemical compositions in austenitic stainless steels during welding.Monitoring the weld pool's chemical composition allows governing the weld pool solidification behavior, and thus enables the reduction of susceptibility to weld defects. Conventional inspection methods for weld seams (e.g. ultrasonic inspection) cannot be performed during the welding process. The analysis system also allows in situ study of the correlation between the occurrence ofweld defects and changes in the chemical composition in theweld pool or in the two-phase regionwhere solid and liquid phase coexist. First experiments showed that both the shielding Ar gas and the welding arc plasma have a significant effect on the selected Cr II, Ni II and MnII characteristicemissions, namely an artificial increase of intensity values via unspecific emission in the spectra. In situ investigations showed that this artificial intensity increase reached a maximum in presence of weld plume. Moreover, an explicit decay has been observedwith the termination of thewelding plumedue to infrared radiation during sample cooling. Furthermore, LIBS can be used after welding to map element distribution. For austenitic stainless steels,Mnaccumulations on both sides of theweld could be detected between the heat affected zone (HAZ) and the base material. T2 - th International Conference on Laser-Induced Breakdown Spectroscopy (LIBS) CY - Chamonix-Mont-Blanc, France DA - 12.09.2016 KW - LIBS KW - TIG KW - Welding KW - Austenitic KW - Stainless steels KW - Chemical composition KW - In situ KW - Measurement PY - 2018 UR - http://www.sciencedirect.com/science/article/pii/S0584854717301064 U6 - https://doi.org/10.1016/j.sab.2017.11.012 SN - 0584-8547 VL - 139 SP - 50 EP - 56 PB - Elsevier CY - Amsterdam, Niederlande AN - OPUS4-43122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel A1 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Kannengießer, Thomas A1 - Kardjilov, N. ED - Somerday, B. P. ED - Sofronis, P. T1 - Measurement of hydrogen distributions in metals by neutron radiography and tomography N2 - Neutron imaging has become a valuable tool for measuring hydrogen distributions qualitatively and quantitatively in metals. Hydrogen mass flow can be measured inside cm thick Steel samples with 10 s temporal resolution. Hydrogen accumulations around craclcs in embrittled iron samples can be visualized three-dimensionally. The gas pressure of hydrogen in crack cavities has been measured to be in the ränge of 5 MPa to 15 MPa. This quality of information allows new insights for the analysis of damage mechanisms on a micrometer scale, e.g., of hydrogen blistering. Further, this method is nondestructive and provides local information in situ and in three dimensions with a spatial resolution of 20 µm - 30 µm. T2 - International Hydrogen Conference 2016 CY - Jackson Lake Lodge, Wyoming, USA DA - 11.09.2017 KW - Hydrogen KW - Neutron imaging KW - Neutron radiography KW - Neutron tomography PY - 2017 SN - 978-0-7918-6138-7 U6 - https://doi.org/10.1115/1.861387_ch46 SP - 416 EP - 422 AN - OPUS4-42505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas A1 - Treutler, K. A1 - Gehling, T. A1 - Eissel, A. A1 - Wesling, V. T1 - In situ Messung der chemischen Konzentration in der Schmelze während des WIG-Schweißens von Duplexstählen N2 - Duplexstähle besitzen ein zweiphasiges Gefüge und werden aufgrund ihrer verbesserten Schweißeignung gegenüber den Vollausteniten häufig im Anlagen- bzw. Apparatebau eingesetzt. Aufgrund der hohen Abkühlgeschwindigkeit und dem Abbrand von Legierungselementen kommt es zu einer Ferritisierung des Schweißguts und damit zu einer Degradation der mechanischen Eigenschaften. Zur Vorhersage des Phasenverhältnisses im Schweißgut wird das WRC1992-Diagramm genutzt. Dieses Diagramm zeigt einige Ungenauigkeiten und benötigt zur genaueren Vorhersage der Phasenverhältnisse eine Überarbeitung. Um den Einfluss einzelner Elemente auf das Schweißnahtmikrogefüge besser zu verstehen, wurden drahtförmige Schweißzusatzwerkstoffe mit dem Ferrit-Bildner Nb und dem Austenit-Bildner Cu beschichtet und für Schweißungen verwendet. Die Messmethode der Laser-induzierten Plasmaspektroskopie (LIBS) bietet hier eine gute Möglichkeit der in situ Überwachung der chemischen Konzentrationen, während des WIG-Schweißens von Duplexstählen. Die LIBS-Messergebnisse, konnten mit der Ferritnummer und der Schweißnahtmikrostruktur korreliert werden. T2 - Symposium Materialtechnik der TU Clausthal CY - Clausthal-Zellerfeld, Germany DA - 23.02.2023 KW - LIBS KW - In situ measurement KW - WRC 1992 diagram KW - Dduplex stainless steel KW - TIG welding PY - 2023 VL - 12 SP - 612 EP - 627 PB - Shaker CY - Aachen AN - OPUS4-57991 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Gornushkin, Igor A1 - Griesche, Axel A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker T1 - In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy N2 - The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, Gas tungsten arc welding (GTAW) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which lead to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), requiring ongoing monitoring of this accumulation. A suitable method for such monitoring is laser-induced breakdown spectroscopy (LIBS), which can be used in two operating modes: calibration using standard reference samples and calibration-free. Unlike conventional quantitative LIBS measurements, which require reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) allows chemical compositions to be determined solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for the quantitative analysis of metal samples. In this work, CF-LIBS is applied to spectra obtained during GTAW DSS welding and the result is compared with those obtained by PLS analysis. A good correlation was found between both types of analysis, demonstrating the suitability of the CF-LIBS method for this application. The CF-LIBS method has a significant advantage over conventional LIBS due to the rapid in situ measurement of concentrations of major alloying elements without calibration procedure. This, combined with fast feedback and appropriate adjustment of welding parameters, helps prevent welding defects. T2 - EMSLIBS 2023 CY - Porto, Portugal KW - LIBS KW - In situ measurement KW - Welding KW - Duplex stainless steel PY - 2024 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-597776 VL - 214 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-59777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Nietzke, Jonathan A1 - Kannengießer, Thomas T1 - In situ measurement of hydrogen concentration in steel using laser‑induced breakdown spectroscopy (LIBS) N2 - The ISO 3690 standard “Determination of hydrogen content in arc weld metal” requires a thermal activation of the diffusible hydrogen in a piece of weld metal for the subsequent ex situ concentration measurement by carrier gas hot extraction CGHE or thermal desorption spectroscopy (TCD). Laser-induced breakdown spectroscopy (LIBS) offers a time and spatially resolved, almost non-destructive, in situ measurement of hydrogen at surfaces without sample preparation. We measured hydrogen in steels, which were charged either electrochemically or by high-pressure hydrogen gas, and compared the results. Further, the feasibility of quantitative hydrogen line scan measurements with LIBS was demonstrated by measuring hydrogen at water jet cut surfaces. The hydrogen concentrations measured with the help of LIBS were compared with CGHE measurements. It was observed that hydrogen can be reliably measured with LIBS for concentrations larger than 2 wt.-ppm. The maximum hydrogen concentration achieved using electrochemical charging was 85.1 ppm. The results show that LIBS is a promising technique for time- and spatially resolved measurements of hydrogen in steels. T2 - IIW Annual Assembly 2023 CY - Singapore KW - LIBS KW - Hydrogen measurement KW - Welding KW - Stainless steel KW - Diffusible hydrogen PY - 2024 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-593664 SP - 1 EP - 9 PB - Springer AN - OPUS4-59366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -