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 DO - 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 - 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 - 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 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593664 DO - https://doi.org/10.1007/s40194-023-01677-2 SP - 1 EP - 9 PB - Springer AN - OPUS4-59366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Gornushkin, Igor B. 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. KW - Duplex stainless steels KW - In situ measurement KW - LIBS KW - GMAW PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597940 DO - https://doi.org/10.1016/j.sab.2024.106899 SN - 0584-8547 VL - 214 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Westin, Elin Marianne A1 - Griesche, Axel A1 - Kromm, Arne A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker A1 - Wessman, Sten T1 - Assessing ferrite content in duplex stainless weld metal: WRC ‘92 predictions vs. practical measurements N2 - AbstractThe weldability of stainless steels is largely controlled by the chemical composition, and alloys with ferritic or ferritic-austenitic solidification show the highest resistance to hot cracking. As the resulting phase balance also affects the final properties, it may be beneficial to both foresee and measure the weld metal ferrite content. The WRC ‘92 constitution diagram is currently the most accurate prediction tool available, but it does not take the cooling rate into consideration and the precision may be less accurate for stainless steels with high ferrite numbers (FNs). This study aims to assess the reliability of the WRC ‘92 diagram for weld metals with FN  50. The chemical composition was altered through gas tungsten arc welding (GTAW) of UNS S32205 with ER347 filler wire that had been coated using physical vapor deposition (PVD) with either niobium (Nb), copper (Cu), nickel (Ni), manganese (Mn), carbon (C), or silicon (Si). The actual ferrite content was evaluated using image analysis, FeriteScope and X-ray diffraction (XRD). While predictions from the WRC ‘92 diagram were deemed acceptable for Ni, Si, and Mn, notable deviations were observed for Nb, Cu, and C. The FeriteScope exhibited a consistent trend with image analysis, albeit with slightly higher FN values, wider scatter, and the conversion factor from FN to vol% is open for discussion. The lowest accuracy and largest spread were obtained using non-contact XRD, rendering it unsuitable for ferrite measurements of welds. These findings underscore the need for improved prediction tools and appropriate measurement methods for assessing ferrite content in duplex weld metals. KW - Duplex stainless steel KW - Welding KW - Phase balance KW - Microscopy KW - Microstructure PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618777 DO - https://doi.org/10.1007/s40194-024-01878-3 SN - 1878-6669 VL - 69 IS - 1 SP - 31 EP - 45 PB - Springer CY - Berlin AN - OPUS4-61877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Westin, Elin Marianne A1 - Griesche, Axel A1 - Kromm, Arne A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker A1 - Wessman, Sten T1 - Assessing ferrite content in duplex stainless weld metal: WRC ‘92 predictions vs. practical measurements N2 - AbstractThe weldability of stainless steels is largely controlled by the chemical composition, and alloys with ferritic or ferritic-austenitic solidification show the highest resistance to hot cracking. As the resulting phase balance also affects the final properties, it may be beneficial to both foresee and measure the weld metal ferrite content. The WRC ‘92 constitution diagram is currently the most accurate prediction tool available, but it does not take the cooling rate into consideration and the precision may be less accurate for stainless steels with high ferrite numbers (FNs). This study aims to assess the reliability of the WRC ‘92 diagram for weld metals with FN  50. The chemical composition was altered through gas tungsten arc welding (GTAW) of UNS S32205 with ER347 filler wire that had been coated using physical vapor deposition (PVD) with either niobium (Nb), copper (Cu), nickel (Ni), manganese (Mn), carbon (C), or silicon (Si). The actual ferrite content was evaluated using image analysis, FeriteScope and X-ray diffraction (XRD). While predictions from the WRC ‘92 diagram were deemed acceptable for Ni, Si, and Mn, notable deviations were observed for Nb, Cu, and C. The FeriteScope exhibited a consistent trend with image analysis, albeit with slightly higher FN values, wider scatter, and the conversion factor from FN to vol% is open for discussion. The lowest accuracy and largest spread were obtained using non-contact XRD, rendering it unsuitable for ferrite measurements of welds. These findings underscore the need for improved prediction tools and appropriate measurement methods for assessing ferrite content in duplex weld metals. KW - Duplex stainless steel KW - Phase fraction prediction KW - WRC diagram PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623682 DO - https://doi.org/10.1007/s40194-024-01878-3 VL - 69 SP - 31 EP - 45 PB - Springer Science and Business Media LLC AN - OPUS4-62368 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 DO - 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 - 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 DO - 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 - Dabah, Eitan A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Kannengießer, Thomas T1 - Neutron imaging of hydrogen in steels N2 - Transmission images with neutrons show a high contrast between hydrogen and iron when using state-of-the-art scintillator materials and digital Cameras. Monitoring the 2D hydrogen distribution evolution with good temporal resolution is possible if a high flux of neutrons is provided. The mass transport of hydrogen can be quantified by Converting the intensity distribution of the images in a hydrogen concentration distribution by using Standards with known composition and similar thickness. Then neutron radiography can be used quantitatively as a non-destructive measurement technique to determine diffusion coefficients e.g. for hydrogen in Steel. We report about measurements at Research Reactors in Germany. The capabilities and limitations, s well as perspectives of this method will be discussed and illustrated with selected examples. T2 - Materials Science & Technology (MS&T) 2013 CY - Montreal, Quebec, Canada DA - 27.10.2013 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 DO - https://doi.org/10.1016/j.ijhydene.2013.08.145 SN - 0360-3199 VL - 38 IS - 34 SP - 14725 EP - 14729 PB - Elsevier Ltd. CY - Oxford AN - OPUS4-29413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -