TY - CONF A1 - Griesche, Axel T1 - Laser-Induced Breakdown Spectroscopy (LIBS) for Hydrogen Measurements in Steel N2 - Laser-induced breakdown spectroscopy (LIBS) allows for a time and spatially resolved almost non-destructive in situ measurement of hydrogen in metals. A surface pretreatment is not necessarily needed. We measured quantitatively hydrogen in steel samples, which were charged either electrochemically or by high-pressure hydrogen gas and compared the results. Further, the feasibility of quantitative hydrogen line scan measurements 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 results show that LIBS is a promising technique for time- and spatially resolved measurements of hydrogen in steel and steel weldments. Results of time-dependant hydrogen permeation experiments will also be presented. T2 - H2MSE 2025 CY - Siegburg, Germany DA - 11.02.2025 KW - LIBS KW - Hydrogen Measurements KW - Steel PY - 2025 AN - OPUS4-62561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - In situ Measurement of Hydrogen 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 - 2025 European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - Hydrogen measurement KW - LIBS KW - Spatial resolution KW - Temporal resolution PY - 2025 AN - OPUS4-62699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - In situ Measurement of Hydrogen in Steel using Laser-induced Breakdown Spectroscopy (LIBS) N2 - Laser-induced breakdown spectroscopy (LIBS) is an analysis technique that allows contactless and fast in situ measurements of hydrogen in welded steels. The surface does not need necessarily be prepared as the laser can ablate material before the measurement. Depth profiling, point measurements as well as scanning of areas (mapping) can be utilized and automated. The method can be used for quantitative measurements, which requires a calibration with standards of similar material containing known hydrogen concentrations. LIBS is a candidate for ISO 3690, determination of diffusible hydrogen in martensitic, bainitic, and ferritic steel weld metal using arc welding processes with filler material. The capability of the method is shown in a hydrogen diffusion experiment. T2 - Tagung Steel & Hydrogen 2025 CY - Genth, Belgium DA - 14.10.2025 KW - LIBS KW - Hydrogen measurement KW - Laser spectroscopy KW - Steel PY - 2025 AN - OPUS4-64451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - Crystallographic phase transformations and corresponding temperature distributions during gtaw of supermartensitic stainless steel visualized by nbei N2 - We investigated the phase transformations during butt-welding of supermartensitic steel plates with help of Neutron-Bragg-Edge Imaging (NBEI). Gas tungsten arc welding (GTAW) was used with a motorized torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. The re-transformation into the martensitic phase during cooling was clearly detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm, a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS [3]. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature. T2 - WCNR-12 CY - Idaho Falls, Id, USA DA - 02.06.2024 KW - Neutron KW - Radiography KW - Welding PY - 2024 AN - OPUS4-60242 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 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 T1 - In situ bragg edge imaging with neutrons for crystallographic phase and temperature field mapping during tig welding N2 - In Neutron-Bragg-Edge Imaging (NBEI) experiments, we studied the phase transition during butt-welding of martensitic Low Temperature Transformation (LTT) Steel [1]. Tungsten inert gas (TIG) welding was used with a moveable torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) underneath the welding head could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. Also, the re-transformation upon cooling from austenite into martensitic phase was detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm that is a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice [2]. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS [3]. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel sample plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature. T2 - MSE 2024 CY - Darmstadt, Germany DA - 24.09.2024 KW - In situ neutron Bragg edge imaging KW - Temperature field mapping KW - Crystallographic phase mapping KW - TIG welding PY - 2024 AN - OPUS4-61268 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 -