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In diesem Beitrag wird der Einfluss der Umgebung auf das Reibungs- und Verschleißverhalten von Polymerwerkstoffen präsentiert. Dabei wurden reine und mit Graphit gefüllte Polymere an Luft, im Vakuum und in einer Wasserstoffumgebung bei Raumtemperatur sowie in flüssigem Wasserstoff bei – 253°C untersucht.
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.
Low heat input gas metal arc welding for dissimilar metal weld overlays part II: the transition zone
(2018)
Dissimilar metal weld overlays (DMWOL) 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 dissimilar weld overlays. In order to evaluate the quality of these overlays regarding resistance against hydrogen-assisted cracking, their transition zone region is investigated in this part of the publication series. Metallurgical characterization, including energy-dispersive x-ray spectroscopy, is performed on Alloy 625/grade 22 steel overlays. The transition zone is characterized by a narrow planar growth zone and steep compositional gradients from the fusion boundary towards the weld metal. Evidence of low carbon contents in the planar growth zone, as well as for carbide precipitation in the cellular growth zone was found. The microstructure in the transition zone region of the fusion zone shows characteristics known to be suitable for good resistance against hydrogen embrittlement.
Laser Metal Deposition (LMD) as a technology for additive manufacturing allows the production of large components outside of closed working chambers. Industrial applications require a stable process as well as a constant deposition of the filler material in order to ensure uniform volume growth and reproducible mechanical properties. This paper deals with the influence of travel path strategies on temperature profile and material deposition. Meandering and spiral hatching strategies are used in the center as well as in the edge of a specimen. The temperature is measured with thermocouples attatched to the backside of the specimen. The tests are carried out on the materials S235JR and 316L. The results show a strong dependence of the maximum temperatures on the travel path strategy and the welding position on the component.
The phase transformation under various cooling rates and in different HAZ regions for high-strength armour steel was analysed by dilatometry. To develop a continuous cooling transformation (CCT) diagram, the samples were heated up to a peak temperature of 1250 °C to achieve a coarse-grained microstructure and then cooled down with a cooling time t 8/5 varying from 3 to 240 s. Analysis of dilatation curves revealed the austenite decomposition process, during which transformation temperatures were determined. The results showed martensitic transformations for all welding-relevant cooling times. Furthermore, to analyse different heat-affected subzones of the weld, the peak temperature was varied between 550 and 1250 °C at a constant cooling time t 8/5 of 6 s. The simulated coarse-grained heat-affected zone (CGHAZ) and fine-grained-heat affected zone (FGHAZ) showed only martensitic transformations with transformation temperatures below 400 °C. The steel exhibited an inhomogeneous hardness with hardening in the CGHAZ and FGHAZ and softening in the intercritical and subcritical HAZ. The physically simulated microstructure was validated by a real hybrid laser-arc weld microstructure.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2018)
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
Laser metal deposition (LMD) has been applied as a coating technology for many years. Today, the technologies capacity to produce 3D depositions leads to a new field of application as additive manufacturing method. In this paper, 3D laser metal deposition of titanium alloy Ti-6Al-4V is studied with special regard to the demands of additive manufacturing. Therefore, only the coaxial LMD powder nozzle is used to create the shielding gas atmosphere, which ensures high geometric flexibility. Furthermore, specimen with high aspect ratio and hundreds of layers are manufactured, which represent typical features in additive manufacturing. The presented study contains the following steps: First, cylindrical specimens are manufactured with a standard shell-core build-up strategy and mechanical properties as well as fracture mechanisms are determined. Based on the results, experiments are conducted to improve the build-up strategy and new tensile test specimens are built with the improved strategy. The improved strategy incorporates variable track overlap ratios to achieve a constant growth in the shell and core area. As blanks, lean cylinders comprising more than 240 layers and a height of more than 120mm are manufactured. The specimens are analyzed by X-ray inspection for material defects. Fractured surfaces are observed via scanning electron microscopy and the composition of the surfaces is determined using energy dispersive X-ray spectroscopy. The tensile test results prove mechanical properties close to ASTM F1108 specification for wrought material.
The accurate EDS microanalysis of light elements such as boron and carbon by spectrum imaging will be demonstrated using a sintered hard ceramic material composed of the three major phases titanium boride (TiB2), titanium carbide (TiC), silicon carbide (SiC) and minor phases, sub-μm in size.
The combination of these three materials leads to improved mechanical and tribological properties. Silicon carbide is a material used for mechanical seals. It has the disadvantage of reduced failsafe running functions, causing increased wear when running dry. The added titanium components (TiC and TiB2) improve the failsafe running functions. This technology has already been transferred to industrial applications.
Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms.