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Eingeladener Vortrag
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Severe mechanical fatigue conditions for worldwide proliferating windfarms are a Major challenge for high-performance concrete in towers, connecting joints and foundations of wind turbines. High-performance concrete offers potential for the application in offshore windfarms, not only regarding its good mechanical, but also chemical resistivity due to low diffusivity in the highly densified microstructure. For a more reliable fatigue assessment, monitoring based on nondestructive testing can be a valuable complement to design rules. Both approaches demand reliable experimental data, information about scalability and the development of standardized testing methods. This article presents results of an ongoing research program of BAM (Bundesanstalt für Materialforschung und -prüfung), which is a part of a joint national project (WinConFat) funded by the German Federal Ministry for Economic Affairs and Energy. The subproject implemented by BAM examines the fatigue behavior in dependence of size and slenderness for varying concrete strength at different stress levels. Besides fatigue strength, nondestructive testing is carried out additionally.
Methods used are strain measurement and ultrasonic testing. The change of strain, stiffness and ultrasonic pulse velocity in the fatigue process is discussed. Results disclose a deeper insight into the damage process under cyclic loading of high-performance concrete and contribute to improve nondestructive monitoring.
Applications on Surface Functionalization by Laser-Induced Periodic Surface Structures (LIPSS)
(2019)
In recent years, the understanding on the formation of laser-induced periodic surface structures (LIPSS) has led to an emerging variety of applications that modify the optical, mechanical and chemical properties of many materials. Such structures strongly depend on the used polarization and are formed usually after irradiation with ultrashort linearly polarized laser pulses. Some specific formation mechanisms to explain every situation are still to be uncovered, but the most accepted explanation relies on the interference of the incident laser beam with electromagnetic surface waves that propagate or scatter at the surface of the irradiated materials. This leads to an intensity modulation that is finally responsible for the selective ablation in the form of parallel structures with periodicities ranging from hundreds of nanometers up to some micrometers. The versatility when forming such structures is based on the high reproducibility with different wavelength, pulse duration and repetition rate laser sources, customized micro- and nanometric spatial resolutions and compatibility with industrially relevant processing speeds when combined with fast scanning devices. In this contribution, we review the latest applications in the rapidly emerging field of surface functionalization through LIPSS, including biomimetic functionalities on fluid transport, control of the wetting properties, specific optical responses in technical materials, improvement of tribological performance on metallic surfaces and bacterial and cell growth for medical devices among many others.
Ultra high performance concrete (UHPC) is characterised by its high compressive strength of more than 150 MPa and its high durability. Due to thermal treatment at 90°C a strength comparable to the 28-days-strength can be achieved immediately after the treatment and in some cases can be even further increased up to 30 %. The explanations for the increase in strength are the accelerated hydration of the clinker minerals and the intensified pozzolanic reaction contributing to a denser microstructure and hence, a high performance in compressive strength.
Former research shows that thermal treatment can lead to inhomogeneities in form of a visible zonation within the cross-section. The width of the margin increases with shorter pre-storage time before the thermal treatment and with omitting protective measures against desiccation during the treatment. Specimens exhibiting a zonation typically show a lower compressive strength compared to the undisturbed reference whereas changes in chemistry, mineral content and microstructure were not reported in detail.
In this study the zonation of thermally treated UHPC is investigated with respect to its chemistry, mineral composition and microstructure to allow predictions on durability and strength development. Measurements show a change in pore sizes, minerals phase composition and element distribution leading to the visible zonation and weaker bending tensile strength compared to the reference.
The life time of mechanical components in high temperature applications is basically determined by their workings. Corrosion determines the loss of material corresponding to the loss of the effective load-bearing section and consequently increasing stress levels. To improve the material selection for such applications a numerical life prediction corrosion model for different alloys and environments is needed. Based on the ferritic alloys FeCr and FeCrCo a first quantitative model is to be developed. For this purpose, the alloys are aged at 600 °C, 650 °C and 700 °C in synthetic air under normal pressure for between 10 and 240 hours. The first objective is to establish a quantitative relationship between the oxidation rate as a function of composition and microstructure of the alloys. The influence of the inner interface as an essential parameter for transport by diffusion on the oxidation kinetics is discussed in this paper.
Boehmite nanoparticles has been successfully functionalized with APTES. After APTES functionalization further modification with tailored molecules e.g. via carboxylic acids is possible. The tailored surface functionalization is strongly enhanced by improved coupling protocols. Arbitrary variation of the functionalization degree is possible. Thereby the temperature stable APTES functionalization enables a wide range of functional groups.
By TGA-MS analysis strong evidence for the bonding situation of the APTES on the boehmite surface has been found. Additionally first experiments has been performed to predict the polymer-particle compatibility enhancement via reverse wetting angle measurements with AFM.
Semiconductor nanocrystals (quantum dots, QDs) are well known for their superior photophysical properties and enabled advancements in several key technologies of the 21st century and numerous technological applications. However, the most studied II-VI semiconductor nanocrystals contain the toxic heavy metal element cadmium, which is limiting their utilization in commercial applications. This has drawn the interest to alternative materials with less toxicity but having similar photophysical features.
The newest generation of TV screens based on QDs have shown that there is a promising environmentally friendly alternative with similar optoelectronic properties, namely indium phosphide (InP) QDs. InP QDs possess a bulk band gap of 1.35 eV with an exciton Bohr radius of ca. 10 nm and thus allow to tune their photoluminescence (PL) from the visible to the near-infrared. Tuning the size and shape of InP QDs and thus tailor their optoelectronic properties can be achieved by different strategies, which range from different types and concentrations of precursors, synthesis temperature or post-synthetic manipulations like etching. The incorporation of other elements like Gallium within the InP core synthesis is another possibility. Using a GaP intermediate layer before growing a ZnS shell has been shown to increase the PL quantum yield, which has been attributed to reduced lattice strain and the removal of phosphor vacancies. Different Ga precursors were investigated but a thorough investigation in terms of their reactivity, localization in the QD and influence on the photophysical properties is lacking to date.
In this contribution we will present the detailed investigation of the presence of two different Ga precursors within the InP core synthesis. Photophysical characterizations (steady-state and PL life-time measurements), transmission electron microscopy, XRD and EDX gave insights into the reactivity of the Ga precursors, the Ga localization in the InP core and influences on the photophysical properties. The variation of the precursor and surfactant concentration and the utilization of different ligands for the Ga precursor allowed tuning the PL emission towards the blue or the red. Depending on the used precursor type we observed the formation of larger-sized InP/GaP core/shell nanocrystals or the formation of InGaP alloy structures enabling to assess the blue range of emission (475 nm).
Residual stresses count among the most limiting factors in the application of additively manufactured materials in safety relevant components subject to cyclic loading. The source of such stresses is inherent in the manufacturing Laser Beam Melted (LBM) process due to rapid cooling and solidification and their distribution in the specimen or component is not homogeneous, but it is usually characterized by high gradients. Moreover, the magnitude of the residual stress field depends very much on the orientation, being higher in the build direction.
Many works in the literature advise to carry out a post-LBM treatment to relieve residual stresses, even though particular attention should be paid in choosing the parameters for the thermal treatment in order to avoid microstructural/phase transformations, which would affect greatly the mechanical properties of the material.
Particularly in the case of the austenitic stainless steel 316L, it has been shown that annealing at high temperatures (above 900°C), besides relieving the residual stresses, may cause recrystallization, grain growth and even phase transformation. In contrast, if a too low annealing temperature is chosen in order to preserve the microstructure, the residual stresses cannot be completely relieved.
This work aims to address the effect of residual stresses on short and long crack propagation for SEN(B) specimens made of 316L fabricated by LBM, in which notches have been machined by electro-discharge machining (EDM) on the mid-plane, perpendicular to the build direction. The specimens underwent different annealing treatments in inert atmosphere, in which the maximum temperature has been varied up to 900°C. The amount of residual stresses and their distribution has been measured by X-ray and neutron diffraction and the specimens have been subject to cyclic loading in a resonant testing machine. The tests show a massive influence of the residual stresses in the build direction on the resistance to fatigue crack propagation of additively manufactured 316L. Finally, a comparison with conventionally manufactured 316L is presented.
The present study deals with the experimental characterization of short crack propagation in SLM (selective-laser-melting) manufactured stainless steel. More specifically, the determination of cyclic R-curves is discussed. This describes the dependency of the crack propagation threshold on crack growth during the short crack propagation stage. For metals, the threshold, starting at a material-intrinsic value, increases until it reaches a value independent of the crack length due to crack closure phenomena which build up at that stage. The cyclic R-curve, when used in the frame of a cyclic R curve analysis, characterizes the resistance of a material to fatigue crack growth and the ability to arrest a physically short crack. Thus, it is the link between classical fatigue and fracture mechanics. In the high-cycle-fatigue range, the short crack propagation stage dominates the overall lifetime, i.e., the number of cycles until failure. Below the fatigue limit crack arrest of hitherto propagable micro-cracks will occur. The effort for the experimental characterization of the short fatigue crack propagation behavior and the cyclic R-curve is very high compared to experiments on long crack propagation. A very exact measurement of crack extension is required, since small increments need to be depicted. Pre-cracking must leave a closure free initial crack, since closure must be build up only by the cyclic R-curve. The closure-free status is achieved by compression pre-cracking. The aim of the present study is an insight into the influence of an AM process on the short crack propagation threshold. Cyclic R-curves are experimentally determined at different load-ratios for 316L austenitic steel specimens produced by SLM and conventional manufacturing. Residual stresses are measured in the crack plane and their influence on the cyclic R-curve is discussed.
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) in offshore industries, such as the oil and gas pipelines, due to the high concentrations of sulfate in the seawater. SRM act upon the metal by the reactiveness of hydrogen sulfide (HS-), and by withdrawal of the available electrons (Fe --> Fe2+ + 2e-; E° = -0.47 V) in electrical contact with the metal (EMIC). However, methanogenic archaea can also cause MIC. Because they do not produce HS-, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood.
To investigate the corrosion potential of methanogens, we studied the EMIC methanogenic strains isolated from marine sediments (Methanobacterium-affiliated strain IM1) and crude oil tanks (Methanococcus maripaludis Mic1c10), in an in-house developed flow-through cell to simulate a fluctuating environment. A co-culture of M. maripaludis and D. alaskensis was also established to study the effect of syntrophic growth on metal corrosion that may occur in industrial pipelines. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.4 mm/yr) are higher to that caused by the marine SRM Desulfovibrio alaskensis (0.15 mm/yr). Surface analyses of the metal showed severe pitting with high methane production. Genomic analysis of the EMIC methanogen M. maripaludis Mic1c10 will provide an insight on the mechanisms of MIC. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) in offshore industries, such as the oil and gas pipelines, due to the high concentrations of sulfate in the seawater. SRM act upon the metal by the reactiveness of hydrogen sulfide (HS-), and by withdrawal of the available electrons (Fe --> Fe2+ + 2e-; E° = -0.47 V) in electrical contact with the metal (EMIC). However, methanogenic archaea can also cause MIC. Because they do not produce HS-, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood.
To investigate the corrosion potential of methanogens, we studied the EMIC methanogenic strains isolated from marine sediments (Methanobacterium-affiliated strain IM1) and crude oil tanks (Methanococcus maripaludis Mic1c10), in an in-house developed flow-through cell to simulate a fluctuating environment. A co-culture of M. maripaludis and D. alaskensis was also established to study the effect of syntrophic growth on metal corrosion that may occur in industrial pipelines. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.4 mm/yr) are higher to that caused by the marine SRM Desulfovibrio alaskensis (0.15 mm/yr). Surface analyses of the metal showed severe pitting with high methane production. Genomic analysis of the EMIC methanogen M. maripaludis Mic1c10 will provide an insight on the mechanisms of MIC. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC
Spectral encoding of cells or particles and the discrimination of multiple spectral codes are a critical process in flow cytometry (FCM). Typical issues in spectral encoding are, e.g., the spectral overlap of codes, or the increasing complexity of instruments . The exploitation of the photoluminescence lifetime (LT) as an encoding parameter could be used to circumvent both of these issues, as it adds another dimension to the parameter space, or, when used as a stand-alone parameter, requiring only one excitation light source and one detector. While LT encoding was considered already decades ago it is still not implemented as a routine technique in FCM yet, mainly due to the challenge of very few photons being available within the limited transition time of a cell or particle through the laser spot.
Recently, we demonstrated LT-FCM based on luminophores with ns LTs in a compact and low-cost flow cytometer. Measurements on polymer microbeads containing luminophores with distinctly different excited state LTs enabled the complete discrimination of three LT codes and five codes in total could be identified.
Now, we have extended our approach towards considerably longer LTs by custom-made polymer microbeads loaded with different ratios of InP/ZnS and AgInS2 quantum dots. The use of these materials significantly expands the usable time range for LT encoding to up to several hundred ns. Our studies demonstrate the possibility to further increase the number of viable LT codes for multiplexing in LT-FCM without the need for extensive hardware modifications.
Laser Powder Bed Fusion (L-PBF) is a promising additive manufacturing (AM) technology for metal part production especially for complex and lightweight structures or functional designs. In L PBF processes several by-products including welding plume and its condensates, spatter and ejected powder are generated during laser exposure. Investigations of micro- and nano-sized by-products have received little attention in literature. This study focuses on the analysis of particle emissions in L PBF of 316L stainless steel using a scattered light aerosol spectrometer and a fast mobility particle sizer spectrometer during the process which allows for in-situ analysis of particle sizes in the range of 6 nm to 100 µm. A distinct correlation of emission signals to part position can be revealed. In addition, a significant influence of laser scanning vector directions on emission signals is presented. Furthermore, differing powder layer thicknesses can be recognised by deviations in emission signals.
Laser powder bed fusion (L-PBF) is one of the most promising additive manufacturing (AM) technologies for the production of complex metallic real part components. Due to the multitude of factors influencing process conditions and part quality and due to the layer-wise characteristic of the process, monitoring of process signatures seems to be mandatory in case of the production of safety critical components. Here, the iterative process nature enables unique access for in-situ monitoring during part manufacture. In this talk, the successful test of the synchronous use of a high-frequency infrared camera and a camera for long time exposure, working in the visible spectrum (VIS) and equipped with a near infrared filter (NIR), will be introduced as a machine manufacturer independent thermal detection monitoring set-up. Thereby, the synchronous use of an infrared camera and a VIS NIR camera combines the advantages of high framerate and high spatial resolution. The manufacture of a 316L stainless steel specimen, containing purposely seeded defects and volumes with forced changes of energy inputs, was monitored during the build. The measured thermal responses are analysed and compared with a defect mapping obtained by micro X-ray computed tomography (CT).
The first results regarding methods for data analysis, derived correlations between measured signals and detected defects as well as sources of possible data misinterpretation are presented in this talk.
WelDX is a newly started research project at BAM publicly funded by the German Federal Ministry of Education and Research. Over the course of three years the project aims to build the foundation for a publicly accessible file format and to foster research collaboration in arc welding on a national and international level.
The talk will motivate benefits and discuss challenges of using a common file format designed to describe, store and share arc welding research data in the scope of "Open Science". By using common open source software and tools, welding data will be made more accessible and reusable so that new scientific practices may emerge.
The proposed file format aims to be easy to use for common welding applications while also offering the possibility to describe complex experiments for state of the art welding research.
In addition the talk will illustrate how in the future other facilities and researchers will be able to use experimental arc welding data generated at BAM for their own research, for example to conduct their own data analysis or welding process and thermo-mechanical simulations.
The talk will give an overview of past, ongoing and future activities at BAM welding divisions, specifically those regarding prospects and challenges of the ongoing digital transformation and the move to more accessible research data (open science) with concerns to welding research. We will discuss current ways to publish and share research results inside the welding community and highlight approaches and advancements from other scientific fields to improve accessibility and reproducibility. We would also like to discuss the feasibility of integrating open science principles into the current IIW landscape of meetings, publications and education. In Addition we will introduce our upcoming series of workshops organized by BAM focusing on defining and implementing an open source file format specifically designed to publish and exchange high quality welding research data.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2019)
This work aims for an yield function description of additively manufactured (AM) parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures.
EBSD/CT-Scans from in-house additively manufactured specimen extract the unique microstructural topology which is converted to a representative volume element (RVE) with grain structure and crystal orientations.
Crystal plasticity model parameters on this RVE are calibrated and validated by means of mechanical testing under different texture angles. From virtual experiments on this RVE, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation.
Residual stresses in Laser Beam Melting (LBM) – Critical Review and outlook of activities at BAM
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, which is coupled with the knowledge about the resulting material properties and performance. In particular, residual stress (RS) was soon recognized as an important issue in AM parts, such that parts are usually subjected to a post build-heat-treated. Significant effort has been spent on simulations of RS in AM, especially using finite element methods. As a consequence, the experimental determination of RS has thereby become increasingly important as a validation tool for simulations, as well as a method for assessing the influence of process parameters. In particular, diffraction methods, which are fundamentally non-destructive, offer enormous possibilities to gain knowledge on the residual stress state in real components, since synchrotron radiation and neutrons can penetrate even heavy metals up to several millimeters or centimeters, respectively. Indeed, significant progress has been achieved, in the understanding of the origins of the RS fields as a function of process parameters, as well as their stability under thermal and/or mechanical exposure.
In this paper, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with the focus on those produced by laser powder bed fusion) has even revealed that process parameters that were previously considered unimportant (e.g. the position and orientation on the base plate) play a major role in the onset of residual stress accumulation.
However, while RS characterization is starting to be considered in the component design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigates about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even those which to date are unclear, will also be discussed. These include the determination of the stress-free reference and of the principal axes of stress. All of these aspects will lead towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Because of its excellent corrosion resistance, a high tensile strength together with a high ductility, duplex stainless steel 2205 offers many areas of application in the chemical and the offshore industry, to name just two. Though welding, especially laser beam welding accompanied by high cooling rates, duplex steels tend to perform higher ferrite contents in weld metal upon cooling down from melting temperature as the base metal. This trend leads to a reduction of the ductility as well as the corrosion resistance of the weld joint. To overcome this problem a solution, based on buffering the plate edges by laser metal deposition with material containing higher Ni concentrations prior to the laser welding was suggested. This method offers more benefits in comparison to conventional usage of higher Ni-alloyed filler wire due to the better control over Ni-distribution in the weld seam, resulting in balanced austenite- ferrite ratio everywhere in the weld metal.
In this context different mixtures of duplex and nickel powder were investigated as well as different process parameters, that enable a smooth surface structure with slightly reduced ferrite contents. In a second step the possibility of welding those edges defect free with standard parameters while achieving balanced austenite- ferrite ratio was verified with metallographic analysis of the microstructure, Electron Backscatter Diffraction (EBSD) and impact testing according to Charpy. The improved corrosion resistance of the welds in comparison to unbuffered ones was observed with the ASTM G48 standard test method.
Because of its excellent corrosion resistance, high tensile strength and high ductility, duplex stainless steel 2205 offers many areas of application. Though laser beam welding accompanied by high cooling rates, duplex steels tend to perform higher ferrite contents in weld metal as the base metal, which leads to a reduction of ductility and corrosion resistance of the weld joint. To overcome this problem, a solution, based on buttering the plate edges by laser metal deposition (LMD) with material containing higher Ni concentrations prior to laser welding was suggested.
In this context different process parameters for LMD and different mixtures of duplex and nickel powder, were investigated. In a second step the possibility of welding those edges defect free while achieving balanced austenite-ferrite ratio was verified with metallographic analysis, Electron Backscatter Diffraction (EBSD) and impact testing according to Charpy. The improved corrosion resistance was observed with ASTM G48 standard test method.
The comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters require accurate and quantitative photo-luminescence measurements. This is of special importance for all photoluminescence applications in the life and material sciences and nanobiophotonics. In the following, procedures for the determination of the spectroscopic key parameter photoluminescence quantum yield, i.e., the number of emitted per absorbed photons, in the UV/vis/NIR/SWIR are presented including pitfalls and achievable uncertainties and material-specific effects related to certain emitter classes are addressed.
Photoluminescence applications in the life and material sciences require bright molecular and nanocrystalline emitters, stimuli-responsive optical probes, signal enhancement, multiplexing, and barcoding strategies and traceable methods to quantify the signal-relevant optical properties of luminescent materials at the ensemble and single molecule/particle level. In this context, current research at Division Biophotonics of BAM is presented ranging from dye and nanocrystal photophysics, absolute measurements of photoluminescence quantum yields in the UV/vis/NIR/SWIR, lifetime multiplexing, and the development of different types of fluorescence standards for validating optical-spectroscopic measurements.
The geometrical characteristics of the weld end crater are commonly used for the validation of numerical results in welding simulation. A semi-analytical model calculating the cooling stage of the welding process after the moving energy source is turned off has been developed. A solution for various combinations of heat sources and workpieces has been found. The theoretical limits for the heat transfer of the absorbed energy during cooling in a thin plate and a semi-infinite body were studied. It is shown that after turning off the energy source, an additional melting of the base material in longitudinal direction may occur. The developed technique is applied to complete-penetration keyhole laser beam welding of a 2 mm thick austenitic chromium-nickel 316L steel plate at a welding speed of 20 mm/s and a laser power of 2.3 kW. The results show a theoretical increase of the weld end crater length in comparison to the length of the steady-state weld pool of up to 19 %. A shift of the centre of the end crater, in which the solidification of the liquid metal ends, towards the tail of the end crater relative to the axis of the heat source at the time of its termination, was computed. The speed and the direction of crystallization of the molten material in the weld pool and the end crater were found to be different. A good agreement between the computational results and the welding experiments was achieved.
The weld pool dynamics and shape play a fundamental role in keyhole mode welding. The presented work aims the experimental and numerical investigation of the influence of the weld pool characteristics on the formation of hot cracking. The experimental procedure allows recording the molten pool in the longitudinal section of a butt joint configuration of 15 mm thick structural steel and transparent quartz glass by using a high-speed video camera and two thermal imaging cameras. The observations show that the dimensions of the weld pool vary depending on the depth. The regions close to the surface form a teardrop-shaped weld pool. A bulge-region and its temporal evolution are observed approximately in the middle of the depth of the weld pool, where hot cracking appears. A numerical framework including models for the weld pool dynamics, global temperature field, transient stress state, crystal growth, diffusion and macro-segregation and subroutines for their one-way couplings is developed. The numerically obtained and experimentally observed results are in a good agreement. It is shown that the bulge-region leads to a delay in the solidification behavior, increased temporal tensile stresses and accumulation of impurities in the defect region and hence enhance the probability of hot cracking formation.
The control of friction and wear is a major concern in many industrial applications. A promising method for a tailored surface modification is the so-called laser implantation technique. This method combines surface texturing and material optimization in one processing step by a localized dispersing of hard ceramic particles using pulsed laser radiation. Wear resistant, protruding micrometric features (implants) with defined geometry can be created in deterministic pattern where needed on highly stressed surfaces, i.e. on forming or cutting tools. However, in order to maintain the implants over the tool’s lifetime, a suitable selection of hard ceramic particles is a prerequisite. They must provide a defect-free Metal Matrix Composite with a high share of homogeneously distributed particles and especially a high implant hardness.
In this study TiN, TiC and TiB2 hard particles were compared as implant materials for the first time. By a systematic variation of the pulse power and pulse duration, their dispersing behavior and influence on the material properties of AISI D2 tool steel was investigated. Although all powder materials had grain sizes smaller than 10 µm, it was possible to disperse them by pulsed laser radiation and to obtain defect-free protruding implants. The highest share of dispersed particles (~64 %) was observed for TiB2. By scanning electron microscopy and energy dispersive X-ray spectroscopy, it was also shown that a significant share of the pre-placed particles was dissolved by the laser beam and precipitated as nanometer sized particles within the matrix during solidification. These in-situ formed particles have a decisive influence on the material properties. While the TiN and TiC implants have shown maximum hardness values of 750 HV1 and 850 HV1, the TiB2 implants have shown the highest hardness values with more than 1600 HV1. By X-ray diffraction, it was possible to ascribe the lower hardness values of TiC and TiN implants to high amounts of retained austenite in the metal matrix. By implanting TiB2, the formation of retained austenite was successfully suppressed due to the in-situ formation of TiC particles, which was proven by electron backscatter diffraction. In conclusion, all the implant materials are basically suitable for laser implantation on AISI D2 tool steel. However, TiB2 has shown the most promising results.
A novel approach for the reconstruction of an equivalent volumetric heat source from a known weld pool shape is proposed. It is based on previously obtained weld pool geometries from a steady-state thermo-fluid dynamics simulation. Hereby the weld pool dimensions are obtained under consideration of the most crucial physical phenomena, such as phase transformations, thermo-capillary convection, natural convection and temperature-dependent material properties. The algorithm provides a time and calibration efficient way for the reproduction of the weld pool shape by local Lamé curves. By adjusting their parameters, the identification of the finite elements located within the weld pool is enabled. The heat input due to the equivalent heat source is assured by replacing the detected nodes’ temperature by the melting temperature.
The model offers variable parameters making it flexible and adaptable for a wide range of workpiece thicknesses and materials and allows for the investigation of transient thermal effects, e.g. the cooling stage of the workpiece. The calculation times remain acceptably short especially when compared to a fully coupled process simulation. The computational results are in good agreement with performed complete-penetration laser beam welding experiments.
Biodiesel is subject to degradation processes like oil and grease. The oxidative degradation products of vegetable oil esters in biodiesel particularly lead to enhanced sedimentation in blended fuels.
The polarity of biodiesel increases its solvency and facilitates permeation and extraction. Solvation, swelling and/or extraction lead to changes in the physical properties and chemical changes of polymeric materials. It also accelerates the degradation (hydrolysis and oxidation) of these materials with the loss of additives and stabilizers.
The objective of this research was to determine the resistance of frequently used polymeric materials such as ACM, EPDM, FKM, FVMQ, CR, CSM, IIR, HNBR, NBR, PA, PE; POM, PUR, PVC and VMQ in biodiesel and heating oil with 10 %/20 % biodiesel (B10/B20) at 40°C and 70°C.
Mass, tensile strength and breaking elongation of the test specimens were determined before and after the exposure for 84 days in the biodiesel heating oil blends. The visual examination of some elastomer test specimens clearly showed the great volume increase until break or partial dissolution. Shore hardness A and D were determined before and after exposure of the test specimens in the biofuels for 42 days.
The elastomers CR, CSM, EPDM, IIR, NBR and VMQ were generally not resistant to biodiesel and B10 at 40°C and 70°C. FKM, ACM, HNBR, PA, PE, POM, and PVC showed high compatibility in B10/B20 at 40°C. A lower compatibility was determined for ACM in biodiesel. ACM and HNBR were not resistant in B20 at 70°C.
This contribution provides current findings regarding materials susceptibility for carbon capture, utilization and storage (CCUS) applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2-stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide material recommendations for certain parts.
The additional element from the filler wire in the laser beam welding is usually distributed inhomogeneously in the final weld due to the high solidification rate of weld pool. It has been found that the electromagnetic stirring produced by an external oscillating magnetic field can enhance the material mixing in the weld pool to achieve a more uniform element distribution. However, the magnetic field has a highly non-linear and multi-coupled interaction with the weld pool behavior, which makes the quantitative explanation of the physical mechanism difficult. In this study, the effect of electromagnetic stirring on the transport phenomena in the wire feed laser beam welding is investigated by a numerical modelling. A 3D transient multi-physical model considering the magnetohydrodynamics, heat transfer, fluid flow, keyhole dynamics and element transport is developed. The multiple reflections and the Fresnel absorption of the laser on the keyhole wall are calculated using the ray tracing method. The numerical results show that a Lorentz force produced by the oscillating magnetic field and its induced eddy current gives significant influence on the transport phenomena in the molten pool. The forward and downward flow is enhanced by the electromagnetic stirring, which homogenizes the distribution of the additional elements from a nickel-based filler wire in a steel weld pool. The numerical results show a good agreement with the high-speed images of the molten pool, the fusion line from the optical micrograph and the element distribution from the energy dispersive X-ray spectroscopy. This work provides a physical base for the electromagnetic-controlled laser beam welding and some guidance for the selection of electromagnetic parameters.
Two epoxy-based nanocomposites with different nanofillers (layered double hydroxide and boehmite) were investigated employing temperature modulated DSC, flash DSC and broadband dielectric spectroscopy. Detailed investigation on the molecular mobility of the two systems showed the effect of the fillers on the structure of the bulk epoxy matrix and the interface formed at the polymer/particle interface
New reference material candidates for traceable size measurement of non-spherical nanoparticles
(2019)
New model nanoparticles with well-controlled shape were synthesized within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. Their systematic characterization takes place by the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following reference nanoparticle candidates are under investigation with respect to their homogeneity and stability: titania nanoplatelets (10-15 nm x 50-100 nm), titania bipyramides (~60 nm x 40 nm), titania acicular particles (100 nm x 15-20 nm; aspect ratio 5.5/6), gold nanorods (~10 nm x 30 nm), and gold nanocubes (~55 nm x 55 nm x 55 nm).
Susceptibility of 304 stainless steel to crevice corrosion in electrochemically active fluids
(2019)
The susceptibility of AISI 304 stainless steel to crevice corrosion on the effect of contact with electrochemically active fluids was investigated using exposure and stepwise potentiostatic polarisation. Crevice materials made up of 304 SS and Polyether ether ketone (PEEK) forming two kinds of crevices including 304 SS-to-PEEK and 304 SS-to-304 SS were tested.
Susceptibility of 304 stainless steel to crevice corrosion in electrochemically active fluids
(2019)
The susceptibility of AISI 304 stainless steel to crevice corrosion on the effect of contact with electrochemically active fluids was investigated using exposure and stepwise potentiostatic polarisation. Crevice materials made up of 304 SS and Polyether ether ketone (PEEK) forming two kinds of crevices including 304 SS-to-PEEK and 304 SS-to-304 SS were tested.
Plasma-Transferred-Arc (PTA) welding is a process that enables high deposition rates, but also causes increased thermal 9 load on the component. Laser based Direct Energy Deposition (DED) welding, on the other hand, achieves a high level of 10 precision and thus comparatively low deposition rates, which can lead to high processing costs. Combining laser and arc 11 energy aims to exploit the respective advantages of both technologies. 12 In this study, different possibilities of this process combination are presented using a PTA system and a 2 kW disk laser. 13 This includes the combination in a common process zone as a highspeed plasma laser cladding technology (HPLC), which 14 achieves process speeds of 10 m/min. Besides that it is being examined whether a pre-running plasma arc can be used to 15 coat difficult-to-weld rail steel with a carbon content of 0.8 % due to a preheating effect. Furthermore, a smoothing of the 16 coating by a plasma arc following the laser is investigated.
Some zinc coated advanced high strength steels (AHSS), under certain manufacturing conditions, are known to be prone to liquid metal embrittlement (LME) during resistance spot welding. LME is an undesired phenomenon, which can cause both surface and internal cracks in a spot weld, potentially influencing its strength. An effort is made to understand influencing factors of LME better, and evaluate geometry-material combinations regarding their LME susceptibility. Manufacturers benefit from such knowledge because it improves the processing security of the materials. The experimental procedure of welding under external load is performed with samples of multiple AHSS classes with strengths up to 1200 MPa, including dual phase, complex phase and TRIP steels. This way, externally applied tensile load values are determined, which cause liquid metal embrittlement in the samples to occur. In the future, finite element simulation of this procedure gives access to in-situ stress and strain values present during LME formation. The visualization improves the process understanding, while a quantification of local stresses and strains allows an assessment of specific welded geometries.
New reference material candidates for traceable size measurement of nonspherical nanoparticles
(2019)
Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary.
The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering.
Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.
3D images such as those produces by X-ray tomography can provide a wealth of information on the internal structure of materials, but quantification of specific geometrical or topological characteristics linked to some bulk physical property is far from being straightforward. This study focuses on methods to quantify the differences in physical properties as a function of direction, i.e. their anisotropy, and how it can be linked to measures of anisotropy of the internal structure of the material. The auto-correlation function gives a similarity measure in the volume as a function of distance and direction. This is a cross-correlation of the image with itself fast to compute and relatively insensitive to noise. It is why we focus on this method to compare with the physical property of our DPF material. Diesel Particulate Filter (DPF) materials are porous ceramics that; a) can be used at very high temperatures; b) have very good thermal shock resistance; c) are inert; d) can be manufactured with tailored porosity. Their usual way of production consists of the extrusion of a slurry into the desired filter shape, with successive ceramming at high temperature. This process causes anisotropy at both microscopic and macroscopic levels.
Sulfur and water have a fundamental impact on the corrosion rate and potential failure of materials. It is therefore necessary to understand the mechanisms, rates, and potential means of transport, as well as the reactions of these elements with an alloy. This work investigates the effect of water vapor in the initial stages of SO2 corrosion of an ferritic model alloy containing 9 wt% Cr and 0.5 wt% Mn.
The exposure experiments were studied at 650°C in situ under laboratory conditions using energy-dispersive x-ray diffraction analysis. Two separate experiments were run, one with a 99.5% Ar + 0.5% SO2 atmosphere and one with a 69.5% Ar + 0.5% SO2 + 30% H2O atmosphere. With a wet atmosphere, the alloy formed a scale with decreasing oxygen content towards the scale–alloy interface. Sulfides were identified above and below a (Fe, Cr)3O4 layer in the inner corrosion zone. In contrast to this, the overall scale growth was slower in a dry SO2 atmosphere.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles.
The layerwise slurry deposition (LSD) has been established in the recent years as a method for the deposition of ceramic powder layers. The LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade; each layer is sequentially deposited and dried to achieve a highly packed powder layer.
The combination of binder jetting and LSD was introduced as a novel technology named LSD-print. The LSD-print takes advantage of the speed of binder jetting to print large areas, parallel to the flexibility of the LSD, which allows the deposition of highly packed powder layers with a variety of ceramic materials.
The working principle and history of the LSD technology will be shortly discussed. A theoretical background will be also discussed, highlighting advantages and drawbacks of the LSD compared to the deposition of a dry powder.
The last part of the talk will be dedicated to highlight recent results on the LSD-print of SiSiC of geometrically complex components, in collaboration between BAM and HC Starck Ceramics GmbH. Density, microstructure and mechanical properties of LSD-printed and isostatic pressed samples will be discussed and compared.
Explosive spalling is caused by, among others, the thermohydraulic spalling mechanism. During this process, vaporization, dehydration, moisture-transport and condensation processes interact. As a result, a drying and dehydration zone as well as a saturated zone, known as a moisture clog, are observed inside the unilaterally-heated concrete. The presented research is focused on the experimental investigation of the underlying thermohydraulic processes.
To investigate these, a test methodology based on X-ray computed tomography (CT) and nuclear magnetic resonance (NMR) was developed. Thereby, the X-ray CT scans are carried out simultaneously during the application of a defined unilateral-heating regime on a specially-constructed specimen. This miniaturized specimen, equipped with a double-layer casing, reproduces the condition within a planar, unilaterally-heated building component.
A preliminary test methodology and the first experimental results were presented at the 5th International Workshop on Concrete Spalling in Borås, Sweden (2017). The contribution for the upcoming workshop presents an improved version of this test methodology and new results for a high-performance concrete (HPC) mixture exposed to temperatures up to 500 °C. Regarding the CT measurements, a higher time-resolution of 15 min was achieved and a quantification of the moisture changes was implemented. Due to an increase in signal quality of the NMR measurements, a pore-size specific moisture distribution can now be resolved. This allows to conclude about the moisture reconfiguration between small gel pores and larger interhydrate pores. Additionally, the NMR measurement are no longer limited to first 2.5 cm below the heated surface but a one-dimensional moisture distribution can now be estimated over the whole 10 cm long specimen.
The presented results demonstrate that the combination of X-ray CT and NMR measurements enables to image and quantify the thermally-induced moisture transport and reconfiguration from small gel pores up to macro pores. This provides important insights into the thermohydraulic damage mechanism and leads to a better understanding of spalling avoidance strategies, like the addition of polypropylene fibres.
Renowned institutions in the field of tribology combine their testing and analytical capabilities with experts in materials/process information management technology to provide the respective services in Europe (i-TRIBOMAT). This requires a centralized materials information management system or the standardised capture, consolidation and harmonization of tribological information.
In Europe biodiesel gained from rapeseeds are considered as an alternative to common fossil fuels due to its environmental performance and its independence from import of raw materials. Biodiesel is also suitable to serve as blending component to heating oil. In that case, it must be considered that changes of fuel composition might cause material degradation.
The objective of this research was to investigate the resistance of metallic materials exposed to heating oil, heating oil blend B20 with 20 % biodiesel and pure biodiesel. Furthermore, the resistance of metals to eight-year aged B10 and six-year aged pure biodiesel was evaluated. Ageing of biodiesel forms acids and water which might propagate metal corrosion. The investigated metals (aluminium, unalloyed steel, austenitic CrNi-steel, copper, die cast zinc and brass) are commonly used for components in middle distillate facilities.
According to DIN 50905-4 the immersed metals were exposed in a climate chamber at 50°C for 4 weeks. The metallic materials were evaluated as resistant if the annual corrosion rate due to uniform corrosion remained under 0.1 mm/year and no localized corrosion in the form of pitting occurred.
The corrosion rates of the exposed materials stayed far below the limit of 0.1 mm/year for all tested fuels. An exception was die cast zinc ZP0410 in eight-year aged B10; a corrosion rate up to 0.3 mm/year due to uniform corrosion was measured. In no case localized corrosion occurred. Copper and brass caused discolouration of biodiesel from yellow to green.
In conclusion, the tested metallic materials were resistant in heating oil, heating oil blend B20 and pure biodiesel at 50 °C. Even the metals exposed to six-year aged biodiesel and eight-year aged B10 showed no uniform or localized corrosion; except for zinc, which was not resistant in eight-year aged B10.
The applicability of 1D-quadrupole-model on the depth estimation of overload-induced delaminations is tested in this contribution. While classical 1D-methods like Pulsed Phase Transformation and Thermographic Signal Reconstruction determine the depth of a defect by one parameter, a two-layer quadrupole model provides two parameters: depth and thermal resistance. In addition, the convectional losses at the surfaces may be considered. The defect investigated is a large-scale delamination in glass fibre reinforced polymer generated by tension overload.
Zinc materials are of high importance in the field of corrosion protection. For example, almost half of the annual production of zinc is used as anti-corrosive layer for steel components, particularly under atmospheric conditions. The corrosion protection is frequently ascribed to zinc carbonate species with low solubility which form on the metal surface under atmospheric conditions. Due to the technological importance and wide use of zinc materials, its corrosion behavior and the formation of reaction products has been intensively investigated over decades.
Assuming atmospheric corrosion conditions, an initial native passive film of few nanometers thickness forms spontaneously. It consists of zinc oxide and hydroxide, transforming into various species in dependence of the surrounding atmospheric conditions.
This study focusses on the investigation of corrosion product layers on massive titanium-zinc sheets, formed during short- and mid-term exposure experiments by Fourier-transformed infrared spectroscopy. This method enables the investigation of extremely thin native passive films which form during the initial hours of exposure. Furthermore, aged surface layers are analyzed which were formed by transformation of initial passive layers over the time of several weeks. The spectroscopic investigations are complemented by scanning electron microscopy (SEM/EDX) in order to obtain information on the chemical composition and morphology of the corrosion products. The combination of both methods offers a comprehensive view on the processes occurring in the early stages of zinc corrosion.
A look inside nanoparticles
(2019)
Small-angle scattering is the method of choice when it comes to obtaining information about the interior of nanoparticles. The aim is to make nanotechnology safer. While the use of small-angle neutron scattering (SANS) is limited to a few instruments in the world, small-angle X-ray scattering (SAXS) is widely accessible, with an upward trend. The example of core-shell particles shows how simple their analysis is with data from an Anton Paar laboratory system. Here, SAXS is a central tool for the development of new reference materials based on poly(methyl) acrylate-PVDF core-shell particles. The dimensions of the cores and shells can be precisely determined. A detailed analysis makes it possible to show that the cores contain fluorinated and nonfluorinated polymers, whereas the shell consist only of PVDF. This core-shell particles with a diameter around 40 nm show a significantly higher PVDF beta phase content than the PVDF homopolymer when using an emulsion polymerization technique. This finding is of importance with respect to applications in electroactive devices.