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Organisationseinheit der BAM
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.