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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.
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.
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.
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.
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.
Short Term Metallurgy and Hot Cracking During Laser Beam Welding of Austenitic Stainless Steels
(2011)
Industrial application of high alloyed austenitic stainless steel laser welding has grown significantly in the recent time due to the continuous improvement of compact and high power density lasers systems. The application of such processes meanwhile ranges from pipeline or railway car body manufacturing to the production of household wares. The largest advantages of the laser application to welding production are much higher welding speeds, reduction or complete exclusion of welding consumables, easy design of the weld joints, decrease of thermal distortions and thus, costs saving. In contrast to arc welding, laser beam welding might particularly be associated with metallurgical defects, like the formation of hot cracks. Such phenomena are related to an order of magnitude higher temperature gradients and cooling rates in the solidification zone, providing rapid solidification kinetics which may cause significant segregation of alloying elements such as Ni and Cr and respective undercooling of the solute at the solidification front. In specific metastable austenitic stainless steels alloys in vicinity of the so called eutectic rim of the Fe-Cr-Ni constitutional diagram, such effects might entail a change of solidification mode from primary ferrite to austenite, providing an increased risk of solidification cracking. Previous studies has shown that the primary solidification mode change during laser beam welding of Cr-Ni austenitic stainless steels such alloys could be effectively influenced by nitrogen absorption as well as by the laser plasma type and also proved the occurrence of metastable primary ferritic solidification. In the present contribution, such results are compared to recent investigations of laser welding newer austenitic Fe-Cr-Mn-Ni steel grades by identification of respective hot cracking critical welding parameter intervals and strain rates in the Controlled Thermal Weldability (CTW) Test.
Up to the present, the thermomechanical loads during welding and subsequent cooling under design-specific shrinkage restraint resulting from the interaction between the materials and the structure have often not been taken into consideration approperiately for weldability assessment of components. As compared to previous investigations using small specimens this report presents component weld tests under varying intensities of restraint. Online records of the reaction forces and moments demonstrate in which way the intensity of restraint affects the reaction stresses and moments and their meaning for the evaluation of the load level in welded components.
Eine Reihe nichtrostender austenitischer Cr-Ni-Stähle in der Nähe der eutektischen Rinne können beim Laserschweißen sowohl primär ferritisch als auch primär austenitisch erstarren. Speziell konzipierte Heißrißprüfungen zeigen eine Rißanfälligkeit der im Unterschied zum WIG-Schweißen mit großen Streckenenergien beim Laserschweißen mit kleinen Streckenenergien primär austenitisch erstarrenden Gefügebereiche. Die Ursache dafür ist, daß im Unterschied zu einer langsamen primär ferritischen Erstarrung bei einer schnellen Erstarrung über metastabile primär austenitische Zustände Restschmelzen entstehen können, die gegenüber dem Grundwerkstoff erhebliche temperaturabhängige Zähigkeitsverluste aufweisen. Es wird gezeigt, wie sich durch die Wahl auf den Werkstoff gezielt abgestimmter Schweißparameter die Heißrißsicherheit beim Laserschweißen weitestgehend sicherstellen läßt. Darüber hinaus werden Perspektiven vorgestellt, wie die Heißrißsicherheit bei Hybridschweißen durch die Auswahl vom Zusatzwerkstoffen und durch eine geeignete Prozeßführung zu erreichen ist.