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- 2016 (13) (entfernen)
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- Englisch (13)
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- Hydrogen assisted cracking (3)
- Hydrogen embrittlement (3)
- ToF-SIMS (3)
- hydrogen assisted cracking (3)
- Data fusion (2)
- Duplex stainless steel (2)
- Hydrogen (2)
- SEM (2)
- numerical simulation (2)
- supermartensitic stainless steel (2)
In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution.
Real Time Imaging of Deuterium in a Duplex Stainless Steel Microstructure by Time-of-Flight SIMS
(2016)
For more than one century, hydrogen assisted degradation of metallic microstructures has been identified as origin for severe technical component failures but the mechanisms behind have not yet been completely understood so far. Any in-situ observation of hydrogen transport phenomena in microstructures will provide more details for further elucidation of these degradation mechanisms. A novel experiment is presented which is designed to elucidate the permeation behaviour of deuterium in a microstructure of duplex stainless steel (DSS). A hydrogen permeation cell within a TOF-SIMS instrument enables electrochemical charging with deuterium through the inner surface of the cell made from DSS. The outer surface of the DSS permeation cell exposed to the vacuum has been imaged by TOF-SIMS vs. increasing time of charging with subsequent chemometric treatment of image data. This in-situ experiment showed evidently that deuterium is permeating much faster through the ferrite phase than through the austenite phase. Moreover, a direct proof for deuterium enrichment at the austenite-ferrite interface has been found.
Hydrogen assisted stress corrosion and cold cracking represent still a major topic regarding the safety of welded steel components against failure in many industrial branches. Hydrogen might be introduced during fabrication welding or might be taken up from an environment during sour service or at cathodic protection. Additionally, understanding and avoidance of hydrogen entry into weld microstructures from gaseous pressurized environments becomes increasingly important for renewable energy components. There are two types of metallurgical mechanisms associated with hydrogen assisted cracking, i.e. the cracking as well as hydrogen transport and trapping mechanisms. For numerical modelling, it has to be considered that both types are not independent of each other, that the mechanisms are not yet completely clarified and that validation of such models strongly depends on implementation of the correct hydrogen related materials properties. However, quite significant achievements have been made in modelling of hydrogen assisted cracking by indirect coupling of thermal, stress-strain as well as hydrogen uptake and diffusion analyses. After a brief introduction into the subject and by revisiting various proposed cracking mechanisms, the present contribution focuses on recent developments of a numerical model based on a comparison of actual hydrogen concentrations and mechanical loads with respective hydrogen dependent material properties as crack initiation and propagation criteria. The basic procedure for numerical simulation of crack initiation and propagation is outlined and it is shown how such numerical simulations can be validated experimentally. Furthermore, it is highlighted how such a procedure has been extended to a comprehensive model for life time prediction of welded steel pipeline components and experimentally verified. Finally, it is outlined how the model can be extended to simulate cracking in heterogeneous steel microstructures on the different scales.
Numerical investigations on hydrogen-assisted cracking in duplex stainless steel microstructures
(2016)
Duplex stainless steels (DSS) are used in various industrial applications, e.g. in offshore constructions as well as in chemical industry. DSS reach higher strength than commercial austenitic stainless steels at still acceptable ductility. Additionally, they exhibit an improved corrosion resistance against pitting corrosion and corrosion cracking in harsh environments. Nevertheless, at specific conditions, as for instance arc welding, cathodic protection or exposure to sour service environments, such materials can take up hydrogen which may cause significant property degradation particularly in terms of ductility losses which, in turn, may entail hydrogen-assisted cracking (HAC). The cracking mechanism in DSS is different from steels having only a single phase, because hydrogen diffusion, stress-strain distribution and crack propagation are different in the austenite or ferrite phase. Therefore, the mechanism of HAC initiation and propagation as well as hydrogen trapping in DSS have not been fully clarified up to the present, as for most of the two-phase microstructures. At this point the numerical simulation can bridge the gap to a better insight in the cracking mechanism regarding the stress-strain distribution as well as hydrogen distribution between the phases, both austenite and ferrite, of the DSS. For that purpose, a two dimensional numerical mesoscale model was created representing the microstructure of the duplex stainless steel 1.4462, consisting of approximately equal portions of austenite and ferrite. Hydrogen assisted cracking was simulated considering stresses and strains as well as hydrogen concentration in both phases. Regarding the mechanical properties of austenite and ferrite different statements can be found in the literature, dependent on chemical composition and thermal treatment. Thus, various stress-strain curves were applied for austenite and ferrite simulating the HAC process in the DSS microstructure. By using the element elimination technique crack critical areas can be identified in both phases of the DSS regarding the local hydrogen concentration and the local mechanical load. The results clearly show different cracking behavior with varying mechanical properties of austenite and ferrite. Comparison of the results of the numerical simulation to those of experimental investigations on DSS will improve understanding of the HAC process in two phase microstructures.
Duplex stainless steels have been used for a long time in the offshore industry, since they have higher strength than conventional austenitic stainless steels and they exhibit a better ductility as well as an improved corrosion resistance in harsh environments compared to ferritic stainless steels. However, despite these good properties the literature shows some failure cases of duplex stainless steels in which hydrogen plays a crucial role for the cause of the damage. Numerical simulations can give a significant contribution in clarifying the damage mechanisms. Therefore, a numerical model of a duplex stainless steel microstructure was developed enabling simulation of crack initiation and propagation in both phases. The phase specific stress strain analysis revealed that local plastic deformation occurs in both austenite and δ-ferrite already in the macroscopically elastic range. Altogether, phase specific hydrogen-assisted material damage was simulated for the first time taking into account all main factors influencing hydrogen assisted cracking process. The results agree well with experimental observations and thus allow a better insight in the mechanism of hydrogen-assisted material damage.
In the field of modelling hydrogen assisted cracking (HAC) phenomenon, hydrogen diffusivity is an important input parameter for numerical simulation. In terms of hydrogen diffusion coefficients, they have great impact on realistic assessment of the evolution of possible crack critical hydrogen concentrations. In addition, the chemical compositions of steels can have a strong effect on hydrogen diffusion. Unfortunately, literature provides a wide range of available hydrogen diffusion coefficients even for similar microstructures and equal temperatures. The scattering of the data can lead to significant deviations in the results of simulating the evolving hydrogen concentrations due to hydrogen uptake (by fabrication or service). Thus, the application of such data to crack-models or for component life tie predictions can be realized up to the present only by considering envelope curves of such value, corresponding to a work or bench case scenario, respectively. For improved reliability of numerical simulaitons, it is necessary to minimize the mentioned deviation of these data. Hence, this work focuses on the validation of hydrogen diffusion coefficients obtained from permeation experiments at room temperature. Two baintic steels with different alloying concepts were investigated, the creep-resistant 7CrMoVTiB10-10 and the reactor pressure vessel grade 20MnMoNi4-5. A numerical model is presented for simulation of the corresponding hydrogen diffusion during permeation experiments using the finite element software ANSYS. Three different diffusion coefficients (obtained from different common calculation methods) are considered and compared to numerical results. The vases of thes calculation methods are permeation transients which are a direct measure for hydrogen. The results of the simulated hydrogen diffusion coefficients show that only one procedure for calculation of diffusion coefficitnes is suitable in comparision to the experimental values. Thus, it is suggested to use this method for analysis of experimental results in case of hydrogen diffusion during permeation experiments. Furthermore, this work supplies validated values for the hydrogen diffusion coefficients of both steel grades.
Modeling of Hydrogen-Assisted Cracking (HAC) in Duplex Stainless Steels (DSS):
- Hydrogen causes significant degradation in DSS and consequently HAC
- Mechanisms of HAC have not been fully understood in two-phase microstructures
- Mesoscale numerical modeling for HAC in DSS was created, coupled to the macroscale, enabling simulation of HAC in both phases independent from predefined crack paths
As a chemical metrology tool time-of-flight secondary ion mass spectrometry (ToF-SIMS) has become a very popular technique to monitor the elemental, isotopic and molecular distribution in two or three dimensions. Its reduced sampling depth, high sensitivity, great structural specificity and the direct detection of hydrogen thereby increase the emergence of ToF-SIMS for material and analytical surface science, particularly due to recent instrumental developments improving mass, depth and lateral resolution. For basic surface science, adsorption processes and surface reactivity thus can be investigated in high detail on organic as well as inorganic samples. The use of multivariate data analysis in addition can effectively assist to identify trends in the complex SIMS raw data set and define key co-variances between certain samples or mass spectra. In this contribution the essence of ToF-SIMS is illustrated by discussing two highly relevant energy applications. First, for piezoelectric electroceramics oxygen exchange active zones have been visualized to determine the impact of external field-load to the oxygen vacancy distribution between anode and cathode. As a second case study the interaction of hydrogen species with the microstructure of a duplex stainless steel was investigated. It was concluded that ToF-SIMS has a valuable essence for detailing hydrogen related degradation mechanisms.
Spectacular failure cases of fossil power stations in the recent years exhibited severe cracking in T24 welds. The results show that hydrogen-assisted cracking up to 200 °C cannot be excluded. Hence, it is important to gain a basic understanding on how hydrogen might affect the basic material properties in the respective weld microstructures. The present study focuses on hydrogen degradation of the respective weld microstructures, i.e., the weld metal and the coarse grained heat affected zone, where actually cracking appeared in practice. Tensile tests were carried out for coarse grain heataffected zone (CGHAZ) and the weld metal in uncharged and electrochemically hydrogen-charged condition. It turned out that both microstructures show distinct tendency for gradual degradation of mechanical properties in the presence of increasing hydrogen concentration. Already for a hydrogen concentration about and above 2 ml/100 g Fe, a significant ductility reduction has been observed. SEM investigations revealed that the fracture topography changes from ductile topography in uncharged condition to intergranular topography for the CGHAZ and to ductile-brittle mix for the weld metal (WM) in hydrogen charged condition. Ti-rich inclusions were identified as central regions of quasi-cleavage fracture areas in the WM. An approximation procedure is applied to quantify the degradation intensity.
Since the mid-nineties, supermartensitic stainless steels (SMSS) have increasingly been applied to welded subsea-pipeline systems in the North Sea oil and gas fields, especially to flowlines at mild sour service conditions. However, in 2001 cracking and leaks occurred during installation and service start-up of two SMSS flowlines in the Norwegian Tune gas condensate field, welded with a new developed matching filler wire. Brittle transgranular cracking started especially at inter-run lack of fusion and propagated brittle, predominantly through the weld metal. The present paper provides a brief overview of the original failure case and respective sequence of events leading to complete replacement of the SMSS by carbon steel flowlines in 2002. Then, detailed investigations of a circumferential weld sample of the failed Tune flowline are highlighted, targeted at comparison of the failure appearance to previous investigations of this filler material type and to search for possible explanations for the brittle fracture at the crack initiation area. SEM investigations of the fracture surface revealed brittle areas only in the direction towards the top side of the weld while the major part of the investigated surface exhibited ductile fracture. As an approach to clarify, if the fracture was a consequence of hydrogen assisted cracking, five small sized specimens have been cut out of the original sample. Cracking has been introduced parallel to the original fracture surface in these specimens at respective saw cuts and bending. The results show that brittle transgranular cracking appeared only in the specimen cooled down to very low temperatures by liquid nitrogen and in the sample charged with hydrogen to an average concentration of about 15 ml/100 g. However, a fracture similar to the original surface was observed only in the hydrogenized specimen. As a further result, very similar fracture surfaces of supermartensitic stainless steel weld metals had been observed on specimens subjected to hydrogen assisted cold cracking (HACC) as well as to hydrogen assisted stress corrosion cracking (HASCC). In total, the results indicate that brittle fracture starting at the inter-run lack of fusion were not initiated by high notch tip deformation rates, but rather influenced by hydrogen, probably taken up during welding.