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Paper des Monats
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Laser-Metal-Deposition (LMD) and Plasma-Transferred-Arc (PTA) are well known Technologies which can be used for cladding purposes. The prime objective in combining LMD and PTA as a Hybrid Metal Deposition-Technology (HMD) is to achieve high Deposition rates at low thermal Impact. Possible applications are coatings for wear protection or repair welding for components made of steel. The two energy sources (laser and Plasma arc) build a Joint process Zone and are configurated to constitute a stable process at laser powers between 0.4-1 kW (defocused) and Plasma currents between 75-200 A. Stainless steel 316L serves as filler material. For this HMD process, a Plasma Cu-nozzle is designed and produced by powder bed based Selective Laser Melting. The potential of the HMD Technology is investigated and discussed considering existing process. This paper demonstrates how the interaction of the two energy sources effects the following application-relevant properties: Deposition rate, powder Efficiency and energy Input.
This invited plenary lecture is aimed at giving a General overview about the assessment of the fatigue strength of metallic components under constant Amplitude loading based on fracture mechanics. A particular Focus is put on the Evaluation of the fatigue crack driving force and material resistance to fatigue crack Propagation in the Regime of physically/mechanically short cracks. The potential of the methodolody is demonstrated on case studies dealing with the fatigue life prediction of welded joints.
The Topic of the presentationis a discussion on defects which can cause failure in cyclically loaded metallic components. Although also touching Features such as material defects such as pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches (which are not considered in the design process) which origin in manufacturing, and others the presentation concentrates on non-metallic inclusions. It is prefaced by an introduction to the life cycle of a fatigue crack from initiation up to fracture. Special emphasis is put on the fact that only cracks which are not arrested during one of their distinct Propagation stages can grow to a critical size.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing.
The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotron- and the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin.
The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates a dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from both X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
IBESS Methology for the fracture mechanics-based determination of the fatigue strength of weldments
(2018)
The presentation provides a brief overview on the results of a German cluster project on the use of fracture mechanics to the determination of the fatigue strength of weldments with fatigue cracks originating at the weld toes. The approach includes (a) a concept for short crack propagation for which the common K concept is not applicable and the crack closure effects are still being gradually build-up, (b) a method for determining fatigue life relevant initial crack sizes as they are needed in any fracture mechanics analysis and (c) multiple cracking and crack coalescence at load levels higher than the endurance limit. The analyses are stochastically performed. Both, the endurance limit as defined for 107 loading cycles and the finite life branch of the S-N curve are determined.
Dissimilar metal weld overlays of nickel-base alloys on low-alloy steel components are commonly used in the oil and gas, petrochemical, and power generation industries to provide corrosion and oxidation resistance in a wide range of service Environments and temperatures. Traditionally, dissimilar weld overlays are produced using cold or hot wire gas tungsten arc welding.
This study aims to identify and evaluate potential advantages of low heat input gas metal arc welding processes over the conventional gas tungsten arc welding in the production of such overlays. Parts I and II of this publication series described characteristics of the heat-affected zone and the transition zone region of alloy 625 on grade 22 steel overlays. These results indicate a good resistance against hydrogen-assisted cracking, which is being verified within this third part of the publication series. To determine the hydrogen-assisted cracking susceptibility, welded samples are tested using the delayed hydrogen-assisted cracking test. Fractography is performed using scanning electron microscopy along with energy dispersive spectroscopy. The results confirm the suitability and efficiency of low heat input gas metal arc welding for dissimilar weld overlays. Variation of the postweld heat treatment procedure bears potential for improvement in this respect.
This chapter deals with the development of polyetheretherketone (PEEK) and polytetrafluoroethylene (PTFE)-based composites, optimized for low friction and low wear performance under extreme environments. It is demonstrated that the incorporation of a harder polymer component into PTFE (such as PEEK particles), a short fiber reinforcement (e.g. carbon fibers (CFs)) and internal lubricants (e.g. PTFE particles) helps to reduce the friction and to improve the wear resistance over a very wide temperature range.
Residual stresses are crucial when assessing the performance of welded components. The present work deals with the possibilities of transferring the real-life boundary conditions of welding, which influence the residual stress, into the laboratory. The possibilities of a test system specifically developed for this purpose with a maximum capacity of 2 MN are shown. Due to the structural design, global process, geometry and material-dependent stresses are induced, which can be simulated and quantified within the system. Additionally, X-ray diffraction can be applied to determine the resulting local residual stress distribution precisely with high spatial resolution. Two examples are presented how the conditions to be found during production are simulated in the laboratory. It is shown how welding residual stresses in high-strength steels are affected by the heat control. It was possible to clarify why elevated working temperatures significantly increase the bending stresses in the welded joint and therefore the tensile residual stresses in the heat affected zone (HAZ). The effect of a heat treatment applied under mechanical stress resulting from welding is demonstrated by the example of a creep resistant steel. Reheat cracking is significantly increased in this case compared to small scale laboratory based tests.
The development within the offshore wind energy sector towards
more powerful turbines combined with increasing water depth
for new wind parks is challenging both, the designer as well as
the manufacturer of support structures. Besides XL-monopiles
the jacket support structure is a reasonable alternative due to the
high rigidity combined with low material consumption. However,
the effort for manufacturing of the hollow section joints reduces
the economic potential of jacket structures significantly. Therefore,
a changeover from an individual towards a serial production
based on automated manufactured tubular joints combined with
standardized pipes has to be achieved. Hence, this paper addresses
the welding process chain of automated manufactured
tubular joints including digitization of the relevant manufacturing parameters such as laser scanning of the weld seam geometry.
Two-dimensional residual stress mapping of multilayer LTT weld joints using the contour method
(2018)
Low transformation temperature (LTT) weld filler materials offer an attractive alternative to cost intensive postweld treatments as they can mitigate detrimental welding residual stresses during the welding process. Compared to conventional weld filler materials, LTT alloys are characterized by a delayed martensite transformation at low temperatures, which can result in compressive residual stresses in the weld. The high strength of these filler materials makes them potentially applicable to high-strength steels as well as for a large amount of requested repair works in steel structures. The focus of the study is on the confirmation of the LTT idea with regard to the residual stress state for multipass weld lines processed by metal active gas welding. It is demonstrated that the contour method is a well-suited technique for measuring the residual stress in the weld joint as it gives an entire two-dimensional map of the residual stress state in the weld line, heat affected zone (HAZ), and base material. The technique was applied at different LTT alloys with varying chemical compositions. Additionally, the results are compared to residual stress maps that were determined by Neutron diffraction using the Strain Analyzer for Large Scale Engineering Applications, an
instrument referred to as SALSA, at the Institut Laue-Langevin in Grenoble. For all investigated specimens, compressive residual stress distributions were determined in the area of the weld joint and the HAZ. They are balanced by tensile residual stresses in the surrounding base material. However, it is shown that the size of theregion exhibiting compressive residual stresses and the absolute values of the compressive residual stresses depend on the chemical composition of the weld filler material.
A simplified model for numerical simulation of laser metal deposition process with beam oscillation
(2018)
A model of laser metal deposition with beam oscillation has been developed. The proposed model consists of two coupled sub-models calculating the heat transfer in the deposited part and the free surface of the molten pool, respectively. The heat transfer simulation of the deposited part solves a three-dimensional quasi-stationary heat conduction problem. The free surface of the molten pool are determined by solving the Laplace-Young equation. The developed model enables the layer-by-layer prediction of the shape of the deposited part and the resulting temperature field. It is shown that for an oscillation amplitude equal to the beam radius the peak value of the heat flux decreases by about 53% and 73% in the case of lateral oscillation and circular oscillation, respectively. Lateral oscillating laser beam results in a higher penetration depth due to the higher thermal efficiency. The amplitude of the laser beam oscillation effects the shape of the deposited wall and the deposition rate. A good correlation between the numerically calculated and experimentally observed results is obtained.
This paper represents the results for proposed optical flow method based on the Lucas-Kanade (LK) algorithm applied to two different problems. The following observations can be made:
- The estimated strain and displacement for conducted tensile test are generally very close to those measured with conventional DIC-technique.
- The LK technique allows measurement of strain or displacement without special selection of a region of interest.
Using a novel optical measurement technique together with the optical flow algorithm, a twodimensional deformation analysis during welding was conducted. This technique is the first to provide a measurement of the full strain field locally in the immediate vicinity of the solidification front. Additionally, the described procedure of the optical measurement allows the real material-dependent values of critical strain characterizing the transition to hot cracking during laser welding processes to be determined.
In this study, a three-dimensional CFD-simulation model was developed to simulate the fluid flow in the weld pool. The CFD-model showed a bulging region in the middle of the depth, which is separated from the top surface and bottom surface by two narrowing regions. It can be concluded that the interaction of the movement of the laser source with the Marangoni vortex leads to a teardrop shape at the upper and bottom surface of the workpiece. Additionally, it shows that the bulging in the weld is a result of the backflows on the upper and lower sides due to the thermo-capillary-driven flows. The weld pool shape was used as a heat source in a two-dimensional thermomechanical model, which allows a highly accurate transformation of the weld pool dimensions obtained from the CFD model. This developed technique allows the consideration of physical aspects, which cannot be considered when using traditional heat sources. The mechanical model has shown that the chronological order of the solidification of the weld has a significant influence on the nature and distribution of the stresses in the weld. High tensile stress has been observed in the bulging region, i.e. in the susceptible region for solidification cracking, when compared to the other narrowing regions, which show compressive stress.
The residual stress distribution in IN718 elongated prisms produced by Selective Laser Melting was studied by means of neutron (bulk) and laboratory X-ray (surface) diffraction.
Two deposition hatch lengths were considered. A horizontal plane near the top surface (perpendicular to the building direction) and a vertical plane near the lateral surface (parallel to the building direction) were investigated. Samples both in as-built (AB) condition and removed (RE) from the base plate were characterized.
While surface stress fields seem constant for AB condition, X-ray diffraction shows stress gradients along the hatch direction in the RE condition. The stress profiles correlate with the distortion maps obtained by tactile probe measurements.
Neutron diffraction shows bulk stress gradients for all principal components along the main sample directions. We correlate the observed stress patterns with the hatch length, i.e. with its effect on temperature gradients and heat flow. The bulk stress gradients partially disappear after removal from the baseplate.
In this study, a three-dimensional CFD-simulation model was developed to simulate the fluid flow in the weld pool. The CFD-model showed a bulging region in the middle of the depth, which is separated from the top surface and bottom surface by two narrowing regions. It can be concluded that the interaction of the movement of the laser source with the Marangoni vortex leads to a teardrop shape at the upper and bottom surface of the workpiece. Additionally, it shows that the bulging in the weld is a result of the backflows on the upper and lower sides due to the thermo-capillary-driven flows. The weld pool shape was used as a heat source in a two-dimensional thermomechanical model, which allows a highly accurate transformation of the weld pool dimensions obtained from the CFD model. This developed technique allows the consideration of physical aspects, which cannot be considered when using traditional heat sources. The mechanical model has shown that the chronological order of the solidification of the weld has a significant influence on the nature and distribution of the stresses in the weld. High tensile stress has been observed in the bulging region, i.e. in the susceptible region for solidification cracking, when compared to the other narrowing regions, which show compressive stress.
The present research work aims at clarification of the effect of the welding electrode type on the mechanical properties of SMA welded joints of 9%Ni steel plates. Properties of produced SMA welded joints were evaluated using different non-destructive and destructive investigation methods. In comparison with the conventionally used Ni-based welding electrode ENiCrMo-3 (AWS A5.11), an experimentally produced non-conventional ferritic welding electrode with 11%Ni (ENi11-Company specification) has resulted in a better combination of the mechanical properties of SMA welded joints of this steel type for critical cryogenic applications. Besides, a positive economic impact for the experimentally produced non-conventional ferritic welding electrode, due to its lower cost, could be another attractive aspect.
The present research work encloses results of experimental investigations of the interaction between welding process parameters for laser-beam and hybrid-laser-arc as well as type of the filler metal and the achievable mechanical properties of the weld joints on steel grade X8Ni9+QT640 for cryogenic service containing 9% nickel. The results obtained contribute to the development and conversion in the industrial practice a new laser beam-based welding technology for the automated manufacturing of facilities for the liquefaction, storage and the transport of natural gases (LNG facilities). The results show, that the martensitic microstructure of the laser weld metal including low amount of retained austenite not exceeding 3.5% leads to the relatively low V-notch impact energy. The remarkable heterogeneity in the chemical composition of the weld metal through the weld thickness could be recognized in the case of hybrid-laser-arc welding with ERNiCrMo-3 austenitic filler metal, what also led to insufficient impact toughness of the weld metall. The most promising results could be achieved by using 11%Ni filler wire, which is similar to the base metal and provides a homogeneous microstructure with uniform distribution of Ni through the weld seam. It is remarkable, that a correlation between Charpy impact toughness and wire feeding speed and respectively process heat input exists. The highest toughness values were 134±58 J at -196C. The both laser as well as laser-hybrid welds passed the tensile test. The failure stress of 720±3 MPa with a fracture location in the base material was achieved for all samples tested.
Supermartensitic stainless steels (SMSS) are a commonly used material nowadays for building offshore structures, i.e. pipelines in the oil and gas industry. The harsh and corrosive environments in oil and gas applications require the correct combination of alloys to attain the desired properties of steel, including high strength and good corrosion properties, even in severe sour service conditions. Welding is the most commonly used method in joining offshore components, depending on requirements requiring strength or fitting. It has been shown that the heat affected zone (HAZ) is more susceptible to certain types of corrosion, including pitting corrosion, especially during severe sour service where a high pH and lower H2S values in the flow medium can lead to pitting corrosion in the HAZ of welded structures. Subsequent hydrogen uptake in the pits can cause cracks to initiate and propagate, leading to rupture of pipelines or catastrophic failures of structures, even at low mechanical loads. Offshore standards allow a certain amount of corrosion, including pitting, to be present before action is required, however the extent of pitting corrosion is not identified by performing visual inspection alone as the subsurface pit diameter may be vastly greater than the pit diameter at the surface. The critical conditions which lead to crack initiation and propagation from a pit with hydrogen uptake are currently not known. Therefore, pitting corrosion and subsequent crack initiation are a danger to the safety of structures. The interest in this phenomenon has resulted in many experimental studies and numerical simulations.
Several numerical models of pitting corrosion and hydrogen uptake resulting in crack initiation are already in existence, but these two phenomena are regularly modelled individually. Thus, a model enabling simulation of both phenomena simultaneously would be of great benefit. Hence, the goal of this study is to develop a model enabling simulation of pit growth and crack initiation, considering hydrogen uptake in the pit from a corrosive environment.
As a first step, this paper presents an investigation into various parameters, which influence crack initiation at pits. These crack critical parameters include: pit geometry, pit location, mechanical load and hydrogen transport into the microstructure. The results will help to identify critical conditions for crack initiation starting at the pit and developing measures to avoid hydrogen assisted cracking (HAC).
Additive Manufacturing (AM) offers the opportunity to produce easier geometrically complex parts compared to traditional production technologies. An important AM technology for metals is selective laser melting (SLM) where a part is produced by melting and solidifying powder in layers. This technique is known to cause a pronounced texture in the produced AM products due to the specific heat flow and the associated solidification of the material during SLM deposition. In order to evaluate the influence of the deposition hatch length during SLM of nickel based superalloy Inconel 718 samples on the texture and in order to identify any preferred crystallographic direction, we performed monochromatic neutron radiography scans (using wavelength from 1.6 Å to 4.4 Å, step size 0.05 Å) to image the samples while rotating it through 90°. Samples produced with short hatch length showed fine textured columnar grains oriented along the sample building direction in high-resolution radiographs. Whereas processing the sample using a ten-fold longer hatch length reduced the texture. The neutron radiographic experiments were accompanied by scanning electron microscopy including electron back-scattered diffraction to visualize and verify the microstructure and texture.
With the recent rise in the demand for additive manufacturing (AM), the need for reliable simulation tools to support experimental efforts grows steadily. Computational welding mechanics approaches can simulate the AM processes but are generally not validated for AM-specific effects originating from multiple heating and cooling cycles. To increase confidence in the outcomes and to use numerical simulation reliably, the result quality Needs to be validated against experiments for in-situ and post-process cases. In this article, a validation is demonstrated
for a structural thermomechanical simulation model on an arbitrarily curved Directed Energy Deposition (DED)part: at first, the validity of the heat input is ensured and subsequently, the model’s predictive quality for in-situ
deformation and the bulging behaviour is investigated. For the in-situ deformations, 3D-Digital Image Correlation measurements are conducted that quantify periodic expansion and shrinkage as they occur. The results show a strong dependency of the local stiffness of the surrounding geometry. The numerical Simulation model is set up in accordance with the experiment and can reproduce the measured 3-dimensional in-situ displacements. Furthermore, the deformations due to removal from the substrate are quantified via 3D-scanning, exhibiting considerable distortions due to stress relaxation. Finally, the prediction of the deformed shape is discussed in regards to bulging simulation: to improve the accuracy of the calculated final shape, a novel Extension of the model relying on the modified stiffness of inactive upper layers is proposed and the experimentally observed bulging could be reproduced in the finite element model.
Foreword
(2018)
The subject of this Special Issue is the fracture mechanics-based determination of the fatigue strength of weldments. Except for one, all papers were written in closer or wider relation to a methodology developed within the framework of the German Project cluster IBESS. Some of them provide background or supplementary information needed in that context but which is also relevant in a wider frame of research activities. The acronym IBESS stands for the topic of this Special Issue (in German: „Integrale Methode zu Bruchmechanischen Ermittlung der Schwingfestigkeit von Schweißverbindungen). Eight partners were involved. The cluster was cooperatively founded by the German Research Foundation (Deutsche Forschungsgemeinschaft) and by the German AiF Network (Arbeitsgemeinschaft industrieller Forschungsvereinigungen) for industrial research.
During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments.
Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear.
Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield.
In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation.
The reduction of harmful emissions to the environment is one of the most urgent challenges of our time. To achieve this goal, it is inevitable to shift from using fossil fuels to renewable energy sources. Within this transition, hydrogen can play a key role serving as fuel in transportation and as means for energy storage.
The storage and transport of hydrogen using austenitic stainless steels as the infrastructure, as well as the use of these grades in hydrogen containing aggressive environments, remains problematic. The degradation of the mechanical properties and the possibility of phase transformation by ingress and accumulation of hydrogen are the main drawbacks. Advanced studies of the behaviour of hydrogen in austenite is necessary to fully understand the occurring damage processes. This knowledge is crucial for the safe use of components in industry and transportation facilities of hydrogen.
A powerful tool for depicting the distribution of hydrogen in steels, with high accuracy and resolution, is time-of-flight secondary ion mass spectrometry (ToF-SIMS). We here present a comprehensive research on the hydrogen degradation processes in AISI 304L based on electrochemical charging and subsequent ToF-SIMS experiments. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed afterwards. All the gathered data was treated employing data fusion, thus creating a thorough portrait of hydrogen diffusion and its damaging effects in AISI 304L.
Specimens were charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and traces existing in the material or adsorbed from the rest gas in the analysis chamber. Similar diffusion and permeation behaviour, as well as solubility, allow nonetheless to draw onclusions from the experiments.
Due to their excellent combination of ductility, strength and corrosive resistance, austenitic stainless steels (ASS) are widely used in many industrial applications. Thus, these steel grades can be found as structural components in the (petro-)chemical industry, in offshore applications and more recent for storage and transport of hydrogen fuel. Steels employed for these applications are exposed to aggressive environments and hydrogen containing media. The ingress and accumulation of hydrogen into the microstructure is commonly observed during service leading to a phenomenon called “hydrogen embrittlement”. A loss in ductility and strength, the formation of cracks and phase transformations are typical features of this hydrogen-induced degradation of mechanical properties.
Although, great efforts are made to understanding hydrogen embrittlement, there is an ongoing debate of the underlying mechanisms. This knowledge is crucial for the safe use and durability of components on the one side and the development of new materials on the other.
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a powerful tool for depicting the distribution of the hydrogen isotope deuterium in the microstructure of austenitic and duplex steels. The combination with imaging techniques such as electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM), delivering structural and morphological information, creates a comprehensive picture of the hydrogen/deuterium-induced effects in the materials. All the gathered data is treated with principal component analysis (PCA) and data fusion to enhance the depth of information.
The mobility of hydrogen and deuterium in a steel microstructure is affected by external mechanical stress. To investigate the behaviour of deuterium in a strained microstructure, a new in situ experimental approach was developed. This gives the possibility of analysing samples in the SIMS instrument simultaneously to four-point-bending-tests.
Specimens made from ASS AISI 304L were electrochemically charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and hydrogen existing in the pristine material or adsorbed from the rest gas in the analysis chamber. Nonetheless, similar diffusion, permeation and solubility data allow to draw qualitative conclusions from the experiments, which are relevant for the application addressed.
Additive manufacturing (AM) opens the route to a range of novel applications.However, the complexity of the manufacturing process poses a challenge for the production of defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields, thermography is a valuable tool for process surveillance. The high process temperatures in metal AM processes allow one to use cameras usually operating in the visible spectral range to detect the thermally emitted radiation from the process. In our work, we compare the results of first measurements during the manufacturing processes of a commercial laser metal deposition (LMD) setup and a laser beam melting (LBM) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.
For almost 150 years it is known that hydrogen has a deleterious effect on the mechanical properties of metallic components. Nowadays, the problem of hydrogen assisted degradation is highly relevant in energy related fields due to the massive use of steel as a structural component in these applications and its sensitivity to hydrogen. Since the discovery of hydrogen assisted cracking (HAC), researchers studied intensively and suggested possible explanations and mechanisms in order to define how hydrogen is affecting the material. In general, it is considered that hydrogen changes the mechanical properties more in terms of ductility (deformation capacities) than in strength (load capacities). Hydrogen concentration is one of three crucial factors in the degradation process, together with the microstructure of the material and the internal/external mechanical load. The relatively high concentration of hydrogen resulting in this loss of ductility can originate during production or before service (e.g. welding processes) and during service (i.e. catholically protected systems to eliminate corrosion processes in sour environments).
In parallel to the theoretical work, tremendous efforts were, and are still, invested in searching for a proper method to elucidate, map and quantify the hydrogen in the microstructure, which is the basis for this work. For steels, the focus is mainly on the observations of diffusion processes and the interaction of hydrogen with the microstructure
in regions with high local stresses/strains (for example around evolving cracks). The challenge for reaching this goal arises from the fact that accurate indication of hydrogen by means of position, unlike heavier atoms, can be made only by mass spectrometry or by interaction with another element (e.g. silver decoration, special coating and resonant nuclear reaction by nitrogen). In addition to this, the difficulty recording the hydrogen behavior while it rapidly diffuses through the material, leaving only the unpredicted failure, should be taken into account.
Although using powerful characterization methods, models and computational simulations, the key to defining the mechanisms behind HAC is still under debate and not fully understood. The relationship between material and hydrogen is determined by three factors, i.e., the material structure and microstructure – determining the physical properties, the mechanical load applied on the material and the hydrogen concentration. It is well known that in order to have a complete definition of HAC these three factors must be examined locally with the minimal scale and the maximal resolution reachable. The major gap is the lack in such a characterization method or a technique by which one has the ability to detect and observe the hydrogen in the metallic microstructure. The commonly used techniques nowadays are capable of characterization of the microstructure without the ability to observe the hydrogen distribution. Global hydrogen concentration and localized hydrogen observation are possible by some techniques which are incapable of indicating a change in the structure or microstructure therefore a comprehensive overview can be gained only by combining several methods.
In the presented research, secondary ion mass spectrometry (SIMS) was adopted as the main tool to detect and locally map the hydrogen distribution in two types of duplex stainless steel grades: EN 1.4462 (standard 2205 duplex stainless steel) and EN 1.4162 (2101 lean duplex stainless steel). The term duplex stainless steel (DSS) refers to the austenitic-ferritic microstructure of the steel where the combination of physical and mechanical properties of the two phases is achieved. The DSS was selected as a case study for this work due to the wide use of this grade in many energy and the lack of knowledge on hydrogen behavior in two-phase containing microstructures. ToFSIMS was exploited in-situ and ex-situ in three experimental approaches during or following
an electrochemical charging procedure. This type of hydrogen charging was selected as it simulated a procedure of cathodic protection of most sub-water oil and gas extraction and delivery systems. The experimental procedures were:
1. Ex-situ charging followed by ToF-SIMS imaging for basic understanding of hydrogen distribution.
2. Ex-situ charging followed by in-situ mechanical loading to obtain information on hydrogen behavior around a propagating crack.
3. In-situ permeation of hydrogen through a steel membrane inside the ToF-SIMS to obtain information on diffusion behavior of hydrogen in a two-phase microstructure.
The comprehensive view of the effect of hydrogen on steel was gained by using supplementary methods, such as high resolution scanning electron microscopy (HR-SEM), focused ion beam (FIB) and electron back-scattered diffraction (EBSD). The state of the art in this work lies in applying both: in-situ experimental approaches and data treatment of the ToF-SIMS raw data. The data treatment includes the combination of data from several sources (data fusion).
The results for the ex-situ charging followed by static sample imaging and data fusion showed that when the analyzed surface is directly exposed to the electrolyte the degradation is pronounced differently in the ferrite, austenite and interface. The degradation mechanisms in the ferrite and austenite were reflected by the formation of cracks on the surface of both, where a high concentration of hydrogen was obtained. This result supports the assumption that hydrogen is attracted to highly deformed regions. The advantage of using in-situ charging/permeation in comparison to ex-situ charging is that the effect of hydrogen on the ferrite and austenite phases when the hydrogen is evolving from within the microstructure is realized, in comparison to when the analyzed surface is initially exposed directly to the electrolyte. In both experiments the ferrite was observed as a fast diffusion path for the hydrogen. The faster diffusion of hydrogen through the ferrite is expected due to the higher diffusion coefficient, however, a direct proof for the diffusion sequence in this scale was never shown. Most significant results were achieved by the ‘core’ experiments of this research. These experiments included the design of a novel dynamic mechanical loading device to apply an external load during SIMS imaging of a hydrogen precharged-notched sample. For the first time it was shown that plastic deformation induced by applying a mechanical load is resulting in a redistribution of hydrogen locally around the notch.