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Eingeladener Vortrag
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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.
Solid-state phase transformations and the evolution of thermal and elastic strains in novel low temperature transformation (LTT) weld filler materials in the near surface region are monitored in real time by means of an innovative experimental set-up at the PDIFF (powder diffraction) beamline at the synchrotron light source ANKA (Angströmquelle Karlsruhe) at the KIT (Karlsruhe Institute for Technology). The key components of the diffraction set-up are two fast microstrip line detectors, which enables the strain evolution to be followed as a function of time and temperature for a 0.5?s counting time. During controlled heating and cooling cycles, as well as during near welding cycles, the martensite–austenite–martensite phase transitions are analysed. The transformation kinetics are monitored during resistance heating of small chips of the pure LTT alloys and during gas tungsten arc welding of simplified LTT welds using a specially designed welding rig for in-situ studies on the diffraction instruments. Under the mechanically unconstrained condition allowing free thermal expansion and shrinkage, the LTT alloys are found to exhibit decreasing transformation temperatures Ac and MS and increasing phase fraction of retained austenite for increasing Ni content. The strain evolution during welding reveals increased compressive stresses upon welding, which is attributed to the martensite formation upon cooling, which counteracts the thermal contraction strains. Comparison of the transformation temperatures reveals higher values than in the pure LTT alloys, but no variation between the different alloys. On the one hand, this is attributed to preferred grain orientation affecting the diffraction measurements and the determination of the transformation temperatures. On the other hand, it is possible that with the different chemical compositions of the LTT alloys and the mechanical constraints during welding, the evolution of the residual strain and stress may vary and result in counteracting affects with respect to lowered martensite start temperatures.
In-situ analysis of solid state phase transformation in TRIP-aided steels by synchrotron diffraction
(2011)
Energy dispersive synchrotron diffraction (EDXRD) analysis and 3 dimensional digital image correlations were conducted to investigate the stress and strain effected transformation behavior during tensile loading of low alloyed TRansformation Induced Plasticity (TRIP) steel. This technique allowed for phase specific stress measurement during certain tensile load steps in the elastic and also plastic regime. Additionally the simultaneous determination of the load dependent phase content was realized. The results show that the martensite transformation starts only after exceeding the overall yield point and is finished before reaching the uniform elongation, whereas a large portion of the austenite remains unchanged in the structure. Furthermore, the martensite transformation related to the stress in the γ-phase and α-phase was analyzed and quantified.
Energy-dispersive x-ray diffraction offers the possibility for measurement and evaluation of diffraction spectra containing information of various diffraction lines of all contributing crystalline phases of a material. Combined strain imaging and diffraction analysis was conducted during the tensile test of a low alloyed transformation-induced plasticity (TRIP) steel in order to investigate the transformation induced plasticity, strain hardening, and load partitioning effects. Optical strain imaging allowed for determination of localized true strains from three-dimensional deformations measured in situ. High-energy synchrotron radiation has permitted diffraction analysis in transmission mode to gather information from the material interior. Phase-specific stress evolution during loading could be observed applying the sin2ψ technique during certain load steps. The strains of the individual lattice planes were determined in different locations under varying angles between loading and perpendicular direction. Using energy-dispersive methods it was also possible to determine the transformation behaviour during elastic and plastic regime taking into account a large number of diffraction lines. The results show that the approach practised here enables one to pull together macroscopic and phase-specific microscopic material behaviour in order to improve existing models for prediction of complex load situations.
We discuss the stability of weld residual strain under static and quasi cyclic transverse tensile loading in the elastic and elastic–plastic region. The test welds were joined with low transformation temperature weld filler materials with 10 wt% Cr and varying Ni-content from 8 to 12 wt%. Using neutron diffraction the residual lattice strain in the martensitic α'- and austenitic γ-phase in the fusion zone as well as the ferritic α-phase in the heat affected zone and base metal as induced by welding, superimposed by stepwise tensile loading and after unloading was measured. The amount of retained austenite in the fusion zone increases with increasing Ni-content, but it decreases with increasing load level due to stress induced martensite formation. In the as-welded condition the transverse macroscopic residual lattice strain was found to be in low compression in the fusion zone in each weld, while the heat affected zone was in tension. Local plastic deformation of the γ-phase as a result of yielding during tensile loading in combination with the change in phase fraction resulted in increased macroscopic compression in the fusion zone. The reduced yield strength in the heat affected zone resulted in plastic deformation and a considerable shift into compression. Comparison with the cross weld distribution of the hardness and FWHM of the neutron diffraction interference lines supported the assumption of plastic deformation of the γ- and α-phase in the fusion and heat affected zone, respectively, while the α'-phase in the fusion zone was stressed within the elastic regime only. Microstructural observations as well as measurement of the local γ-phase fraction by means of laboratory X-ray diffraction in the fusion zone strengthen these observations.
In situ analysis of hydrogen behaviour in stainless steels by high energy synchrotron radiation
(2011)
Hydrogen generally causes lattice distortions and phase transformations when introduced into a metal matrix. The present contribution provides a report of first in situ investigations of hydrogen effects on the lattice of the austenite and the martensite phase in a supermartensitic stainless steel using hard synchrotron radiation for respective energy dispersion diffraction measurements. Lattice distortions, such as the planar spacing expansion, have been monitored during the complete hydrogen effusion process over 24 h and are directly correlated to the dissolved hydrogen in the metal matrix. Among other results, it turned out that hydrogen at the introduced concentration level causes a reversible lattice expansion and after hydrogen effusion the lattice nearly regained its original dimensions. Hydrogen much more significantly affects the austenite phase with respect to lattice expansion than the martensite phase, but no phase transformations occur during the hydrogen desorption process.
Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration
(2011)
The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS.
Gegenstand dieses Forschungsprojekts waren Untersuchungen zur Qualifikation von Fülldrahtelektroden für das Laserstrahl-MSG-Hybridschweißen hochlegierter Stähle. Dieser Typ Drahtelektrode ermöglicht aufgrund seines ringförmigen Metallmantels und der pulverartigen Füllung insbesondere im oberen Bereich der erzielbaren Abschmelzleistungen einen stabilen, spritzerarmen Werkstoffübergang vergleichbar dem im Sprühlichtbogen. Im Gegensatz dazu wird beim Abschmelzen von Massivdrahtelektroden ein kontrollierter Werkstoffübergang durch die Impulslichtbogentechnik erreicht.
Die Werkstoff- und prozessspezifischen Eigenschaften beim Schweißen dieser Zusatzwerkstoffe haben einen signifikanten Einfluss auf die Schweißnahtmetallurgie sowie die Prozessstabilität. Zur Untersuchung der Übertragbarkeit der erzielbaren Werkstoffeigenschaften vom MSG-Schweißen auf das Laserstrahl-MSG-Hybridschweißen wurden Versuche am hochlegierten Grundwerkstoff AISI403L (X2CrNil911) durchgeführt. Als Zusatzwerkstoffe gemäß DIN EN 12 072 und DIN EN ISO 17 633 kamen vier Drahtelektroden, ein eigens für das Positionsschweißen konzipierter Rutilfülldraht 19 9 L P M1, ein zum Schweißen in Wannenposition geeigneter Rutilfülldraht T 19 9 L R M (C) 3, ein Metallpulverfülldraht T199LMM1 sowie ein Massivdraht G19 9 L Si zum
Einsatz.
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.
Novel martensitic filler materials with specially adjusted martensite start temperatures (Ms) can counteract the cooling specific shrinkage due to expansion effects of the weld metal associated with phase transformations. That can be exploited to create compressive residual stresses in the weld and adjacent areas, i.e. beneficial for increasing fatigue strength. The Ms-temperature is shifted via the chemical composition, mainly by the alloying elements nickel and chromium, resulting as well in different retained austenite contents. Investigations were made using different Low Transformation Temperature (LTT) alloys with varying nickel content. The resulting phase transformation temperatures were — for the first time — detected using high energy synchrotron diffraction and Single Sensor Differential Thermal Analysis (SS-DTA). Compared to angle dispersive diffraction, energy dispersive diffraction offers the possibility to measure residual stresses of the martensite and austenite phase parallel fast in one experiment up to depths of 100 μm. The residual stresses show significant distributions dependent on the Ms-temperature. The effect on the cold cracking behaviour of these alloys was investigated using the Tekken test. Results show that cold cracking can be avoided when appropriate contents of retained austenite are existent.
The development of high-strength structural steels with yield strengths up to 1000 MPa results in the requirement of suitable filler materials for welding. Recently designed low transformation temperature (LTT) alloys offer appropriate strength. The martensitic phase transformation during welding induces compressive residual stress in the weld zone. Therefore, the mechanical properties of welded joints can be improved. The present paper illustrates numerical simulation of the residual stresses in LTT-welds taking into account the effect of varying Ms/Mf-temperatures, and therefore different retained austenite contents, on the residual stresses. Residual stress distributions measured by synchrotron diffraction are taken as evaluation basis. A numerical model for the simulation of transformation affected welds is established and can be used for identification of appropriate Ms-temperatures considering the content of retained austenite.
Low Transformation Temperature (LTT) alloys were developed in order to control the residual stress development by the martensitic phase transformation already during cooling of the weld metal. The positive effect of such LTT alloys on the mitigation of detrimental tensile residual stresses during welding has already been confirmed on the basis of individual laboratory tests. Within the current project it was experimentally investigated whether the phase transformation mechanisms are effective under increased restraint due to multi-pass welding of thicker specimens. The local residual stress depth distribution was analyzed non-destructively for V-type welds processed by arc welding using energy dispersive synchrotron X-ray diffraction (EDXRD). The use of high energy (20 keV to 150 keV) EDXRD allowed for the evaluation of diffraction spectra containing information of all contributing phases. As the investigated LTT alloy contains retained austenite after welding, this phase was also considered for stress analysis. The results show in particular how the constraining effect of increased thickness of the welded plates and additional deposited weld metal influences the level of the residual stresses in near weld surface areas. While the longitudinal residual stresses were reduced in general, in the transition zone from the weld to the heat-affected zone (HAZ) compressive residual stresses were found.
Wasserstoffanalytik und Degradation von Werkstoffeigenschaften von hochfesten Feinkornbaustählen
(2011)
In this study, hydrogen absorption and diffusion were investigated for various high-alloyed ferritic-austenitic duplex steels. On account of the specific transformation and solidification behaviour, respectively, of duplex steels as compared to single-phase ferritic and austenitic steels, special conditions have to be considered concerning hydrogen absorption which may ultimately lead to microstructure-dependent hydrogen-assisted weld metal cracking. Hydrogen absorption during welding may occur via the shielding gas, moisture from the surroundings or via the welding filler material. As a contribution to the interpretation and prediction of hydrogen-induced cracking in welded duplex steels, the actual hydrogen absorption via the arc as well as the weld metal hydrogen diffusion was investigated for the first time in a duplex steel DS (1.4462), a super duplex steel SDS (1.4501) and in a lean duplex steel LDS (1.4162). Isothermal heat treatment using carrier gas hot extraction enabled quantification of the amounts of hydrogen trapped in the respective microstructure areas. The hydrogen diffusion coefficients were determined by analytical and numerical calculation. The total hydrogen concentrations and the diffusion coefficients were found to be nearly identical. Trapped hydrogen was however observed to be dependent on the material and on the microstructure condition. The influence of hydrogen on the mechano-technological properties of the weld metal was characterized with the help of tensile tests. In addition, the hydrogen embrittlement effect was detected in scanning electron microscopic analyses.
Realization and safe operation of modern welded structures are progressively requiring for base and filler materials to cope with continually increasing loads, Analyses with a view to crack prevention therefore need to accommodate particularly the structural design (restraint intensity) and the thermomechanical effects in terms of stresses introduced during welding, Against this background, multi-run welding experiments were carried out in an IRC - (Instrumented Restraint Cracking) Test under defined restraint intensity in order to examine the influence of heat control (preheating and interpass temperatures) on the weldinq-specific forces and stresses, The experiments revealed significant rises in the reaction force and stress after welding with increasing preheating and interpass temperature, Furthermore, various concepts for calculating the preheating temperature are discussed, It is demonstrated that the hitherto existing concepts for high-strength finegrained structural steels can lead to divergent results.
Novel martensitic filler materials with specially adjusted martensite start temperatures (Ms) can counteract the cooling specific shrinkage due to expansion effects of the weld metal associated with phase transformations. That can be exploited to create compressive residual stresses in the weld and adjacent areas, i.e. beneficial for increasing fatigue strength. The Ms temperature is shifted via the chemical composition, mainly by the alloying elements nickel and chromium, resulting as well in different retained austenite contents. Investigations were made using different Low Transformation Temperature (LTT) alloys with varying nickel content. The resulting phase transformation temperatures were – for the first time – detected using high energy synchrotron diffraction and Single Sensor Differential Thermal Analysis (SS-DTA). Compared to angle dispersive diffraction, energy dispersive diffraction offers the possibility to measure residual stresses of the martensite and austenite phase parallel fast in one experiment up to depths of 100 µm. The residual stresses show significant distributions dependent on Ms temperature. The effect on the cold cracking behaviour of these alloys was investigated using the Tekken test. Results show that cold cracking can be avoided when appropriate contents of retained austenite are existent.
Hot crack assessment during production and processing of metallic materials is an essential prerequisite for the safety of welded structures. The hot cracking investigations presented here were carried out as part of a study aimed at the development of Cr/Ni low transformation temperature filler materials. Low transformation temperature alloys open up the possibility for welding high strength steels. The externally loaded Modified Varestraint Transvarestraint hot cracking test was employed in the experiments described. The hot cracking resistance was evaluated with the help of light microscopy applied at the specimen surface. The proportionality between hot cracking susceptibility and Cr/Ni alloy content was explained by the altered solidification kinetics and by the enlarged solidification interval. The internal crack paths and the three-dimensional structure of the crack net in the material volume were examined using X-ray computer tomography. The total crack lengths for different material depths and circumjacent rectangular volumes, respectively, were be determined. An increasing hot cracking susceptibility with increasing Cr/Ni alloy content was also be established for the specimen volume.