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The wear rates of self-mated alumina couples show that friction as well as wear is largely determined by the above-mentioned hydro-thermal conditions. The presence of water and its amount available in the surrounding system either in liquid or in gaseous form plays a key role for friction and wear behavior and can be beneficial for the tribological profile of steam degradation resistant materials. Hot steam enhances the tribo-chemical formations of oxides and hydroxides on MgO-ZrO2 alumina and antimony impregnated carbon.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
In a first test series, the friction and wear properties of 6 polymeric candidate materials for application in LNG tribosystems were tested. The most favorable properties showed PTFE composite, filled with carbon fibers and PEEK, which showed low and stable friction and a wear coefficient in the order of 10-7 mm3N-1m-1. PTFE containing PEEK composites seem to be also appropriate for LNG applications. Admixtures of graphite as solid lubricant result in lower wear. Contrary, a lubricating mechanism of MoS2 was not observed. The PI-materials showed comparatively high friction and medium wear.
The tribological characteristics of pure and graphite filled polymers were investigated in gaseous hydrogen at ambient temperatures and in LH2 at -253°C. It could be shown that the tribological properties of PI and PEEK materials is related to the formation of a transfer film. The influence of both hydrogen and cryogenic temperatures will be discussed in the presentation.
The tribological characteristics of pure and graphite filled polymers were investigated in gaseous hydrogen at ambient temperatures and in LH2 at -253°C. It could be shown that the tribological properties of PI and PEEK materials is related to the formation of a transfer film. The influence of both hydrogen and cryogenic temperatures will be discussed in the presentation.
In situ laser-induced breakdown spectroscopy measurements in stainless steels during TIG welding
(2018)
Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects. A prototype of a LIBS controlled welding process is presented.
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.
In an increasing number of modern steel applications, high-strength structural steel grades are demanded to meet specifications regarding a high load-bearing capacity and a low operating weight. Lightweight design rules enhance the safety requirements, especially for welded joints. Besides a higher cracking risk for high-strength steel welds, the formation of tensile residual stresses might lead to fracture due to overloading or premature failure if not adequately considered. In this study, a stress-strain analysis was conducted at component-related structures from S960QL using digital image correlation while preheating, welding and cooling adjacent to the weld seam. X-ray diffraction analysis of the local residual stresses in the weld seam showed a good comparability with global analyses using either a DIC system or a special testing facility, which allowed in situ measurements of welding loads. By analysing two different seam geometries, it could be shown that lower multi-axial stresses arise if a narrower weld groove is used. Comparative analyses revealed a direct correlation of the local residual stresses in the weld with transverse shrinkage restraint, whereas the residual stress level in the HAZ is significantly affected by the bending restraint of the weld construction and the occurring bending stresses, respectively.
A three-dimensional multi-physics numerical model was developed for the calculation of an appropriate equivalent volumetric heat source and the prediction of the transient thermal cycle during and after fusion welding. Thus the modelling process was separated into two studies. First, the stationary process simulation of full-penetration keyhole laser beam welding of a 15 mm low-alloyed steel thick plate in flat position at a welding speed of 2 m/min and a laser power of 18 kW was performed. A fixed keyhole with a right circular cone shape was used to consider the energy absorbed by the workpiece and to calibrate the model. In the calculation of the weld pool geometry and the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature were taken into account. The obtained local temperature field was then used in a subsequent study as an equivalent heat source for the computation of the transient thermal field during the laser welding process and the cooling stage of the part. The system of partial differential equations, describing the stationary heat transfer and the fluid dynamics, were strongly coupled and solved with the commercial finite element software COMSOL Multiphysics 5.0. The energy input in the transient heat transfer simulation was realised by prescription of the nodes temperature. The prescribed nodes reproduced the calculated local temperature field defining the equivalent volumetric heat source. Their translational motion through the part was modelled by a moving mesh approach. An additional remeshing condition and helper lines were used to avoid highly distorted elements. The positions of the elements of the polygonal mesh were calculated with the Laplace’s smoothing approach. Good correlation between the numerically calculated and the experimentally observed weld bead shapes and transient temperature distributions was found.
The monitoring of oil and gas pipelines by means of distributed fibre optic sensors is becoming common. The most recent development in the field of fibre optic sensing is the distributed acoustic sensing (DAS), which allows to detect and to localize third party threats to pipelines. For this purpose, fibre optic telecommunication cables located close to the pipelines are usually used. However, DAS carries a far greater potential for continuous condition monitoring of pipelines.
The interdisciplinary research project AGIFAMOR (Ageing Infrastructures – Fibre Optic Monitoring of Pipes) at BAM investigates a new technical approach to extend the application field of DAS towards the detection and localization of acoustic signals that indicate critical alterations and certain damage scenarios originated from within the pipeline or the pipe wall. Therefore, the optical fibre sensors are applied onto the pipe itself and the application procedure towards an optimal acoustic signal transduction is optimized.
A number of laboratory scale experiments were performed focusing on the signal transmission of acoustic signals as well as the detection of damage in the pipe wall by means of DAS. Furthermore, real-scale tests on a pipeline DN100 of 38 m length have been carried out at the BAM test site for technical safety (BAM-TTS) to study the detection and localization of leaks and of changing flow profiles due to corrosion or sedimentation processes.
The monitoring of oil and gas pipelines by means of distributed fibre optic sensors is becoming common. The most recent development in the field of fibre optic sensing is the distributed acoustic sensing (DAS), which allows to detect and to localize third party threats to pipelines. For this purpose, fibre optic telecommunication cables located close to the pipelines are usually used. However, DAS carries a far greater potential for continuous condition monitoring of pipelines.
The interdisciplinary research project AGIFAMOR (Ageing Infrastructures – Fibre Optic Monitoring of Pipes) at BAM investigates a new technical approach to extend the application field of DAS towards the detection and localization of acoustic signals that indicate critical alterations and certain damage scenarios originated from within the pipeline or the pipe wall. Therefore, the optical fibre sensors are applied onto the pipe itself and the application procedure towards an optimal acoustic signal transduction is optimized.
A number of laboratory scale experiments were performed focusing on the signal transmission of acoustic signals as well as the detection of damages in the pipe wall by means of DAS. Furthermore, real-scale tests on a pipeline DN100 of 38m length have been carried out at the BAM test site for technical safety (BAM-TTS) to study the detection and localization of leaks and of changing flow profiles due to corrosion or sedimentation processes.
In the present work an approach is presented which combines various aspects of the former models with probability considerations. It is used to simulate the impact of more than one billion Alumina particles onto a steel substrate. This approach permits the simulation of an entire erosion experiment on an average PC within about six hours.
Hydrogen-assisted cracking is a critical combination of local microstructure, mechanical load and hydrogen concentration. Welded microstructures of low-alloyed creep-resistant Cr-Mo-V steels show different hydrogen trapping kinetics. This influences the adsorbed hydrogen concentration as well as the diffusion by moderate or strong trapping. A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens
were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. Finally, realistic temperature assessment is mandatory for calculation of activation energy via TDA.
Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The residual stress distribution in the bulk of IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-build condition (on a build plate) and after removal from the build plate.
The absolute values of all stress components decreased after removal from the build plate. Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component depending on the thermal gradient in the respective direction.
Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects.
High-strength low-alloyed (HSLA) steels with yield strength ≥ 690 MPa have increasing importance in steel construction and civil engineering. However, weld processing of those steels is a major challenge. The susceptibility for degradation of mechanical properties of weld joints significantly increases in presence of hydrogen and can result in hydrogen assisted cracking (HAC). Generally, risk for HAC increases with increasing yield strength of HSLA steels. To minimize the incidence of HAC, it is essential to gain knowledge about both the (1) absorbed hydrogen amount and its distribution in the weld seam and (2) options to lower
the amount of introduced hydrogen. Existing standards recommend heat treatment procedures (interpass temperature or post weld heat treatment) to reduce the diffusible hydrogen concentration in weldments. In this context, different weld seam geometries should be considered. For HSLA steel fabrication weld processing with seam opening angles of 45° to 60° is typical. Modern weld technologies allow welding with seam opening angles of 30° - reduced welding time and costs. In the present study, the hydrogen distribution in multi-layer welds of a 960 MPa HSLA steel was analysed. Influence of different seam opening angles as well as heat input, interpass temperature and post weld heat treatments were investigated. The welded samples were quenched in ice water immediately after welding and subsequently stored in liquid nitrogen. After defined warming up, small specimens were machined from the weld seam by water jet cutting. The diffusible hydrogen concentration was measured by carrier gas hot extraction with coupled mass spectrometer. The results showed, that low heat input and post weld heat treatment procedures can lower hydrogen concentrations in welds. Furthermore, a gradient of the hydrogen concentration was
identified with increasing weld pool depth. By varying the seam opening angles different hydrogen concentrations were
measured.
Neutron cameras allow visualizing hydrogen distributions with radiographic or tomographic imaging methods in iron and steel. The necessary contrast between hydrogen and iron stems from the high difference in the total neutron cross section of both elements. This allows e.g. the in situ measurement of hydrogen mass flow inside cm thick steel samples with a temporal resolution of 20 s using neutron radiography as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples with neutron tomography. We could detect directly gaseous hydrogen in the crack cavities and we measured the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of hydrogen-induced damage mechanisms. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm. In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography methods in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of the HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching.
High-strength steels are increasingly applied in modern steel constructions to meet today’s lightweight requirements. Welding of these steels demands a profound knowledge of the interactions between the welding process, cooling conditions, heat input and the resulting metallurgical occurrences in the weld and its vicinity. Additionally, welding stresses may be detrimental for the safety and performance of high-strength steel component welds during fabrication and service, especially due to the high yield ratio. For a development of strategies to adjust welding heat control, all these effects should be considered, to reach a complete exploitation of the high-strength steel potential. In recent researches at BAM, multilayer GMAW experiments were performed with high-strength steels, in which cooling conditions and resulting microstructure were analysed for varied heat control parameters. The application of a unique 3d-operating testing facility and X-ray diffraction measurements allowed the analysis of local stresses in the weld while welding and cooling under component relevant shrinkage restraints. As a result, correlations between material behaviour, welding and cooling condition and the arising multi-axial stresses and forces were found. Based on this study, statements for the development of adapted heat control concepts were derived, which are presented by means of specific analysis examples.