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 - TY - JOUR A1 - Serrano Munoz, Itziar A1 - Pfretzschner, Beate A1 - Kromm, Arne A1 - Nadammal, Naresh A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Neuwirth, T. A1 - Schulz, M. A1 - Griesche, Axel T1 - High-resolution Bragg-edge neutron radiography detects grain morphology in PBF-LB/M IN718 N2 - One of the main advantages of metal additive manufacturing (MAM) techniques is their ability to produce components with site-specific microstructural features. Nevertheless, microstructural defects and lack of repeatability are still major concerns in MAM. In this study, a laser powder bed fusion (PBF-LB/M) IN718 material, produced using two different scan length vectors, is investigated using Bragg-edge neutron 2D imaging (BENI) combined with electron backscatter diffraction (EBSD) analysis. BENI is able to detect, on a macroscopic scale, process-induced changes in texture in a large field of view covering the entire sample (20×80 mm2). In addition, high-resolution BENI (HR-BENI), with a pixel size of 12.8 µm, provides a micro-scale examination of the local variations of texture and grain morphology, otherwise undistinguishable using the standard resolution. As such, HR-BENI offers a straightforward and detailed way of screening the integrity of MAM parts at cm-length scales. KW - Bragg-edge neutron 2D imaging (BENI) KW - Metal additive manufacturing (MAM) KW - IN718 PBF-LB/M KW - Crystallographic texture control KW - Electron backscatter diffraction (EBSD) PY - 2023 U6 - https://doi.org/10.1016/j.mtla.2023.101827 SN - 2589-1529 VL - 30 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-57819 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 - 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 - Griesche, Axel A1 - Pfretzschner, B. A1 - Taparli, Ugur Alp A1 - Kardjilov, N. T1 - Time-Resolved Neutron Bragg-Edge Imaging: A Case Study by Observing Martensitic Phase Formation in Low Temperature Transformation (LTT) Steel during GTAW N2 - Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam). The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature Ms since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging. KW - Austenite-to-martensite transformation KW - Neutron radiography KW - Bragg-edge imaging KW - Gas tungsten arc welding (GTAW) KW - Debye–Waller factor KW - Low transformation temperature (LTT) steel PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-538016 VL - 11 IS - 22 SP - 10886 PB - MDPI CY - Basel AN - OPUS4-53801 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 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Griesche, Axel T1 - Hydrogen in Metals Visualized by Neutron Imaging N2 - Neutron cameras allow visualizing hydrogen distributions with radiographic or tomographic imaging methods in iron (and steel) and many other metals. The necessary contrast between hydrogen and these metals stems from the high difference in the total neutron cross section of both elements. This allows, e.g., the in situ measurement of hydrogen mass flow inside cm thick metal samples with a temporal resolution of at best 10 s using neutron radiography as well as the quantitative measurement of hydrogen accumulations, e.g., at the crack’s inner surfaces in hydrogen embrittled iron samples with neutron tomography. This new quality of the information on a micrometer scale allows new insights for the analysis of hydrogen-assisted damage mechanisms. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20 μm - 30 μm. In this contribution, we give a short historical overview of neutron imaging and show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography methods in order to visualize and quantify hydrogen accumulations, absorption processes, and diffusion. The examples are taken from the works of researchers dealing with titanium, palladium, zirconium, and iron or steel. More detailed descriptions of the experimental and analytic procedures are given for hydrogen detection using radiography and tomography on iron and steel samples. KW - Hydrogen assisted cracking KW - Neutron imaging PY - 2019 U6 - https://doi.org/10.5006/3104 SN - 0010-9312 VL - 75 IS - 8 SP - 903 EP - 910 PB - NACE International AN - OPUS4-48775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konadu, D. S. A1 - Pistorius, P. G. H. A1 - Du Toit, M. A1 - Griesche, Axel T1 - Solidification cracking susceptibility of ferritic stainless steels using Modified Varestraint Transvarestraint (MVT) method N2 - The Modified Varestraint Transvarestraint (MVT) test was used to investigate the solidification cracking susceptibility of an unstabilised, a Nb-stabilised and two (Ti + Nb) dual-stabilised ferritic stainless steels. Two different welding speeds of 6 and 3 mm/s using autogenous gas tungsten arc welding were employed. At the welding speed of 6 mm/s, the high-content (Ti + Nb) steel was resistant and the Nb-stabilised steel was marginally susceptible to solidification cracking. At the welding speed of 3 mm/s, the Nb and the high (Ti + Nb) steels were found to be marginally susceptible to solidification cracking while the unstabilised and low-content (Ti + Nb) grades were resistant to solidification cracking. The weld metal microstructures transverse to the welding direction revealed columnar grains in all the samples for both welding speeds. The ferritic stainless steels were generally resistant to solidification cracking, except the Nb-stabilised steel, which was marginally susceptible to solidification cracking. KW - Susceptibility KW - Modified Varestraint Transvarestraint KW - Solidification cracking KW - Ferritic stainless steel KW - Microstructure KW - Welding PY - 2019 U6 - https://doi.org/10.1007/s12046-019-1175-0 SN - 0973-7677 VL - 44 IS - 9 SP - Article Number: UNSP 194 PB - Springer AN - OPUS4-48938 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 - 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 -