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3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT
(2016)
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.
Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic
stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial
resolution of 100 µm.
Neutron cameras allow visualizing hydrogen distributions with radiographic or tomographic imaging methods in iron and steel. The necessary contrast between hydrogen and iron 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 steel samples with a temporal resolution of 20 s using neutron radiography as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples with neutron tomography. We could detect directly gaseous hydrogen in the crack cavities and we measured the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of hydrogen-induced damage mechanisms. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm. In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography methods in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of the HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching.
Neutron cameras allow visualizing hydrogen distributions with radiographic or tomographic imaging methods in iron and steel.
The necessary contrast between hydrogen and iron 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 steel samples with a temporal resolution of 20 s using neutron radiography as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples with neutron tomography. We could detect directly gaseous hydrogen in the crack cavities and we measured the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of hydrogen-induced damage mechanisms. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 μm.
In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography methods in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed
at the research reactor BER II of the HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in
Garching.
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.
Die dehnungsinduzierte Martensitbildung wurde mittels Röntgen-Diffraktion und -Radiographie mit dem EDDI-Instrument am BESSY II in supermartensitischem Stahl mit Anlassaustenit untersucht. Die Bildung wird durch Wasserstoff im Gefüge unterdrückt. Die Duktilität von wasserstofffreiem SMSS korreliert mit dem Anteil an dehnungs-induziertem Martensit
Hydrogen-charged supermartensitic steel samples were used to systematically investigate imaging artifacts in neutron radiography. Cadmium stencils were placed around the samples to shield the scintillator from excessive neutron radiation and to investigate the influence of the backlight effect. The contribution of scattered neutrons to the total detected intensity was investigated by additionally varying the sample-detector distance and applying a functional correlation between distance and intensity. Furthermore, the influence of the surface roughness on the edge effect due to refraction was investigated.
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.
Neutron imaging is a valuable tool for measuring hydrogen distributions qualitatively and quantitatively in metals. Time-resolved neutron radiography allows to measure hydrogen mass flow inside cm thick steel samples with ~10 s temporal resolution. Hydrogen accumulations around cracks in embrittled iron samples can be visualized three-dimensionally by neutron tomography. This quality of information allows new insights for the analysis of damage mechanisms on a micrometer scale, e.g. of hydrogen blistering. Even the gas pressure of molecular hydrogen in crack cavities has been measured from tomographic reconstructions to be in the range of 5 MPa to 15 MPa for technical iron. Further, this method is non-destructive and provides local information in situ and in all three dimensions with a spatial resolution of 20 - 30 µm. The combination with other methods gives a new quality of information, e.g. of the hydrogen allocation on fractured surfaces.
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.
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.
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.
Gravity has significant effects on alloy solidification, primarily due to thermosolutal convection and solid phase buoyancy. Since 2004, the European Space Agency has been supporting investigation of these effects by promoting in situ X-ray monitoring of the solidification of aluminium alloys on microgravity platforms, on earth, and in periodically varying g conditions. The first microgravity experiment-investigating foaming of liquid metals - was performed on board a sounding rocket, in 2008. In 2012 the first ever X-ray-monitored solidification of a fully dense metallic alloy in space was achieved: the focus was columnar solidification of an Al-Cu alloy. This was followed in 2015 by a similar experiment, investigating equiaxed solidification. Ground reference experiments were completed in all cases. In addition, experiments have been performed on board parabolic flights-where the effects of varying gravity have been studied. We review here the technical and scientific progress to date, and outline future perspectives.
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.
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.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
In Neutron-Bragg-Edge Imaging (NBEI) experiments, we studied the phase transition during butt-welding of supermartensitic steel plates. Gas tungsten arc welding (GTAW) was used with a motorized 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 into the martensitic phase upon cooling 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. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS. 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.
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.
In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy
(2024)
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.
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.
In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy
(2024)
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.