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The purpose of the present study is to show the feasibility of examining hydrogen desorption in technical iron samples using neutron radiography at the ANTARES facility of the FRM II research reactor, Technische Universität München. It has been shown that this method is appropriate for in situ determination of hydrogen Desorption for concentrations as low as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 260 °C. Measurement was based on direct comparison between electrochemically hydrogen-loaded iron samples and hydrogen-free reference samples at the same temperature.
This enables the determination of hydrogen concentration as a function of time and temperature. Ex situ carrier gas hot extraction experiments using the same temperature–time profiles as the neutron radiography experiments have been used to calibrate the greyscale values of the radiographs to defined hydrogen concentrations. It can be stated that hydrogen desorption correlates with sample temperature.
The purpose of the present study was to show the feasibility of measuring hydrogen effusion in austenitic stainless steel (1.4301) using neutron radiography at the facility ANTARES of the research reactor FRM II of the Technische Universität München. This method is appropriate to measure in-situ hydrogen effusion for hydrogen concentrations as small as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 533 K. The measurement principle is based on the parallel comparison of electrochemically hydrogen charged specimen with hydrogen-free reference specimen at the same temperature. This allows the determination of the hydrogen concentration in the specimens as a function of time and temperature. Separate hot carrier gas extraction experiments using the same temperature–time profiles as the radiography experiments have been used to calibrate the grey values of the neutron transmission images into hydrogen concentrations. It can be stated that the hydrogen effusion correlates with the specimen temperature.
In situ crack detection in the mushy zone and the solid weld of a gas tungsten arc (GTA) weld using X-ray imaging during welding is a new research area for NDT inspection. Usually, NDT flaw detection is done after the complete solidification of the weld seam. In this paper, we present the use of real-time radiography with a minifocus X-ray source (YXLON X-ray tube Y.TU 225-D04) and a 75μm pixel size digital detector array (Dexela 1512) for the acquisition of 2D radiographic images by a sequence of exposures with time intervals of 80 ms for hot crack detection during single pass bead-on-plate GTA welding of 3 mm thick plates of aluminium alloy AlMgSi (6060). An analysis of the crack distribution in the weld sample is conducted from the acquired 2D radiographs and its corresponding 3D volumetric reconstruction achieved by linear coplanar digital laminography.
This in situ approach opens new possibilities in the field of hot crack research by having the direct information of both the crack initiation and growth and its correlation to the welding parameters.
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.
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.
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.
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.
We report about investigations of typical material problems in steels. First, residual stresses in and around weld seams with low martensite transition temperature filler material were analyzed w/ and w/o additional transverse tensile load. The investigation was accompanied by x-ray diffraction measurements to track stress-induced phase transitions. Martensite formation during welding under external load yield strain gradients near the surface that improve the integrity of the weld. Further, the residual stress distribution close to laser-treated steel surfaces was analyzed. The method could be improved to reduce analysis artifacts. Finally, hydrogen diffusion in different steels was measured using neutron radiography and subsequent image analysis. Diffusion coefficients were derived by analyzing the time-dependent mass flux. In an outlook we describe the optimal ESS instrumentation from a metallurgists point of view.
Hydrogen assisted cracking of metals limits the durability of welds and constructions. Still
the failure mechanisms are not fully understood, for instance the role of hydrogen mass
transport during crack initiation. Measuring the hydrogen concentration as a function of
time (and space) would allow to determine diffusion coefficients helping to enlighten this
lack of understanding. Therefore, neutron radiography is a valuable tool for measuring in
situ hydrogen transport in iron and steels [1].
The influence of grain boundaries on the hydrogen diffusion behaviour can be determined
by comparing the diffusion behaviour of samples with e.g. different microstructure. In a
first study we investigated in situ the simplest case, the hydrogen effusion out of pure iron
(ARMCO) using neutron radiography at ANTARES [2]. Samples were charged electrochemically
ex situ with a well defined amount of hydrogen, stored in liquid nitrogen and were then
heat treated during a neutron radiography measurement whilst the change of neutron transmission
was recorded. For analysis the gray values in the pictures were transformed into
concentrations with help of an ex post calibration. Therefore, the experimental temperaturetime
profile of the heat treatment has been repeated with identical samples in the home lab
and the amount of effusing hydrogen was measured by carrier gas hot extraction. In a first
approximation the concentration of hydrogen in the sample can be calculated by subtracting
the hydrogen concentration in the atmosphere from the initial one in the sample. We
were able to measure hydrogen concentrations as low as 65 wt.ppm.
Simultaneously monitoring of hydrogenous
sample and hydrogen-free reference allowed
for in situ measurement of hydrogen effusion.
Sample heating was done by infrared radiation.
Diffusion coefficients for hydrogen effusion
from iron have been calculated. They coincide
fairly with literature data.
We could show in GTAW experiments with steel samples that the attenuation of neutron transmission underneath the welding torch due to the Debye-Waller-effect correlates well with sample temperatures obtained by FE numerical simulations. This would allow principally to determine sample temperatures by measuring the neutron beam attenuation.
Die Ergebnisse von in-situ Experimenten am Berliner Elektronenspeicherring (BESSY II) werden vorgestellt. Es wurden Zugversuche an wasserstoffbeladenen und wasserstofffreien supermartensitischen Proben durchgeführt und Diffraktionsspektren und radiographische Bilder aufgenommen. Die energiedispersive Röntgendiffraktion ermöglichte dabei in-situ die dehnungsinduzierte Phasenumwandlung von Restaustenit zu Martensit zu beobachten. Die Radiographiebilder der zerreisenden Probe gaben Einblicke in das Bruchverhalten in Abhängigkeit vom Wasserstoffgehalt.
In Neutron-Bragg-Edge Imaging (NBEI) in situ experiments, we studied the phase transitions in martensitic steel sheets during butt-welding. Gas tungsten arc welding was used with a motorized torch allowing automated weldments. The austenitization in the heat affected zone underneath the welding head could be clearly visualized. Also, the retransformation into the martensitic phase upon cooling. However, we observed an unexpected additional change in transmission at λ = 0.44 nm that is at 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. With help of temperature field simulations that were calibrated by the reading of anattached thermo couple during welding, we could show that the Debye-Waller factor can produce an additional image contrast.
We report about diffusion measurements and molecular dynamic simulations
in Al-Ni and Al-Cu melts. Capillary methods were used to measure Ni and
Cu self diffusion and to measure interdiffusion. The combination of the
capillary set-up with X-ray radiography allowed in-situ detecting of
convective contributions to the interdiffusion transport by tracking the
time dependence of diffusion. Thus, the determination of the
interdiffusion coefficient can
be restricted to convection-free experiment times resulting in an
increased accuracy of the measured interdiffusion coefficient.
Additionally, quasielastic neutron scattering was used to measure
convection-free Ni and Cu self diffusion. Molecular dynamics simulations
were used to determine all diffusion coefficients and the thermodynamic
factor. The comparison between experiment and simulation shows an
excellent agreement of the interdiffusion coefficients as a function of
temperature. It was found that interdiffusion is enhanced by
thermodynamic forces with a maximum around the stoichiometric composition.