Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
- nein (287)
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.
Im Vortrag wird die Problematik Mikroplastik eingeführt und ein Probenset aus dem Mittelmeer mit ersten Ergebnissen besprochen. Die Alterung von Polymeren im Umweltkontext sowie Möglichkeiten der Analyse von Polymeralterungsfortschritten werden diskutiert. Die thermoanalytische Methode mit Zersetzungsgasanalytik (TED-GC-MS) wird eingeführt und deren Einsatzmöglichkeiten in der Thematik umrissen.
Several decades have passed since the initial drafting of the European standards for explosives subject to European Directive 2014/28/EU, and this field as experienced some substantial technical innovations. While at the turn of the millenium the concept of electronic detonators had just been conceived, and it is mentioned in a Technical Specification, today electronic detonators exist in many variants, also regarding communication means between shotfirer and the detonating cap. Questions regarding safe functioning and prevention of inadvertent ignition have to be asked in a quite different way, where delicate electronic circuits are used, and where information is transmitted by radio waves. In addition, the safety of functioning is partly found in software components and the corresponding standards need to be reviewed thoroughly on these grounds.
A different but in recent times more and more popular technology, is the on-site production of explosives, being mostly emulsion explosives, ANFO, or combined products. Also here software in the machinery is starting to play an important role. The on-site produced explosive must fulfil safety requirements and has to be, in addition, quality controlled. This cannot solely be left to the hopefully proper design of the software and machinery, but needs to be made accessible to verification. Since this area seems broader in approach, it is not going to be addressed by a new standard. The state of the art technology shall be described in a Technical Specification with a perspective from requirements of the above mentioned European Directive.
Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost-effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells, the corrosion resistance of the materials used needs to be determined.
In this study, representative low-cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were investigated in simulated pore water at 333 K and under CO2 saturation condition to represent the worst-case scenario: CO2 diffusion and aquifer fluid penetration. These simulated pore waters were made from relevant cement powder to mimic the realistic casing-cement interface. Electrochemical studies were carried out using the pore water made of cement powder dissolved in water in comparison with those dissolved in synthetic aquifer fluid, to reveal the effect of cement as well as formation water on the steel performance. Two commercially available types of cement were investigated: Dyckerhoff Variodur® and Wollastonite. Variodur® is a cement containing high performance binder with ultra-fine blast furnace slag which can be used to produce high acid resistance concrete. On the other hand, Wollastonite is an emerging natural material mainly made of CaSiO3 which can be hardened by converting to CaCO3 during CO2 injection.
The results showed the pH-reducing effect of CO2 on the simulated pore water/aquifer (from more than 10 to less than 5) leading to the active corrosion process that happened on both 1.8977 and 1.7225. Electrochemical characterization showed negative free corrosion potential and polarisation curves without passive behaviors. The tested coupons suffered from pitting corrosion, which was confirmed by surface analysis. Interestingly, basing on the pit depth measurements from the tested coupons and the hardness of cement powder, it is suggested that Variodur® performed better than Wollastonite in both aspects. The electrochemical data was compared to that resulted from exposure tests to give a recommendation on material selection for bore-hole construction.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has enormous influence on the early hydration of cement. C3A as the most reactive phase of Portland cement plays a significant role in early hydration reactions and affects the rheological performance. Therefore, this talk presents experimental results about the influence of delayed addition of PCEs on the Hydration of alite and C3A-gypsum pastes investigated by isothermal heat flow calorimetry. Complementary in-situ XRD was carried out on C3S and C3A-gypsum pastes to analyze hydration and phase changes related to the addition of PCE. Cement pastes with a delayed addition of PCE showed less retardation compared to simultaneous addition. The alteration caused by PCE is much more pronounced for C3A-gypsum mixes. With a delayed addition of SP, the hydration of C3A is less retarded or even accelerated. It is obvious that there is less retardation the later the addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and Hydration rates. XRD results showed that more C3A is dissolved in the presence of PCE. Also, the gypsum depletion occurs earlier in the presence of PCE and even faster with delayed addition. Without PCE AFm starts to form just after the gypsum depletion. However, in the presence of PCE AFm already starts to form at the beginning of the hydration. Due to the faster gypsum depletion in the presence of PCE, also the transformation from ettringite into AFm begins earlier, but takes longer as without SP.
Femtosecond laser-induced periodic surface structures: from light localization to applications
(2019)
This presentation reviews the current state in the field of Laser-induced Periodic Surface Structures (LIPSS). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized laser radiation. LIPSS are formed in a “self-ordered” way and are often accompanying material processing applications. They can be produced following a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their structural sizes typically range from several micrometers down to less than 100 nanometers exhibiting a clear correlation with the polarization direction of the laser radiation. Various types of surface structures are classified, relevant control parameters are identified, and their material specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics, through time-resolved optical experiments and theoretical simulations. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
By allowing economic on demand manufacturing of highly customized and complex workpieces, metal based additive manufacturing (AM) has the prospect to revolutionize many industrial areas. Since AM is prone to the formation of defects during the building process, a fundamental requirement for AM to become applicable in most fields is the ability to guarantee the adherence to strict quality and safety standards. A possible solution for this problem lies in the deployment of various in-situ monitoring techniques. For most of these techniques, the application to AM is still very poorly understood. Therefore, the BAM in its mission to provide safety in technology has initiated the project “Process Monitoring of AM” (ProMoAM). In this project, a wide range of in-situ process monitoring techniques, including active and passive thermography, optical tomography, optical emission and absorption spectroscopy, eddy current testing, laminography, X-ray backscattering and photoacoustic methods, are applied to laser metal deposition (LMD), laser powder bed fusion and wire arc AM. Since it is still unclear which measured quantities are relevant for the detection of defects, these measurements are performed very thoroughly. In successive steps, the data acquired by all these methods is fused and compared to the results of reference methods such as computer tomography and ultrasonic immersion testing. The goal is to find reliable methods to detect the formation of defects during the building process. The detailed acquired data sets may also be used for comparison with simulations.
Here, we show first results of high speed (> 300 Hz) thermographic measurements of the LMD process in the SWIR range using 316L as building material. For these experiments, the camera was mounted fixed to the welding arm of the LMD machine to keep the molten pool in focus, regardless of the shape of the specimen. As the thermograms do not contain any information about the current spatial position during the building process, we use an acceleration sensor to track the movement and synchronize the measured data with the predefined welding path. This allows us to reconstruct the geometry of the workpieces and assign the thermographic data to spatial positions. Furthermore, we investigate the influence of the acquisition wavelength on the thermographic data by comparing measurements acquired with different narrow bandpass filters (50 nm FWHM) in a spectral range from 1150 nm to 1550 nm.
This research was funded by BAM within the Focus Area Materials.
Bioanalytical, diagnostic, and security applications require the fast and sensitive determination of a steadily increasing number of analytes or events in parallel in a broad variety of detection formats.[1,2] Ideal candidates for spectral encoding and multiplexing schemes are luminescent nanocrystals like semiconductor quantum dots (QDs), particularly Cd-containing II/VI QDs with their narrow and symmetric emission bands. With the availability of relatively simple and inexpensive instrumentation for time-resolved fluorescence measurements, similar strategies utilizing the compound-specific parameter fluorescence lifetime or fluorescence decay kinetics become increasingly attractive.[3-5] The potential of different types of QDs like II/VI, III/V and Cd-free ternary QDs such as AgInS (AIS) QDs for lifetime-based encoding and multiplexing has been, however, barely utilized, although the lifetimes of these nanocrystals cover a time windows which is barely accessible with other fluorophores. Here we present a brief insight into the photophysics of AIS QDs and show the potential of dye- and QD-encoded beads for lifetime-based encoding and detection schemes in conjunction with flow cytometry and fluorescence lifetime imaging microscopy
Biodiesel is viewed as a major source of energy. In areas such as the European Union, where 80 % of the oil-based fuel is imported, there is also the desire to reduce dependence on external oil supplies.
Materials compatibility is a major concern whenever the fuel composition is changed. The question arises of whether polymeric materials are resistant to heating oil with 20 % biodiesel (B20) in comparison to pure heating oil.
The polarity of biodiesel increases its solvency and facilitates permeation and extraction. Solvation, swelling and/or extraction lead to changes in the physical properties. Extraction alters the fuel chemistry. These chemical changes could also accelerate the degradation (hydrolysis and oxidation) of the polymeric material with the loss of additives and stabilizers.
The objective of this research was to determine the resistance of frequently used materials for components in middle distillate facilities such as ACM, FKM, HNBR, PA, PE, POM, PUR and PVC in heating oil and heating oil blend B20 for 84 days at 40 °C, and FKM, HNBR, PA, POM, PUR and PVC at 70 °C.
Mass, tensile strength, breaking elongation and Shore hardness A (D) of the test specimens were determined before and after exposure for 84 (42) days in the test fuels under static conditions.
For the investigations under compressed conditions, the mass and the compression set of FKM test specimens were determined before and after exposure for 3, 7, 14, 28, 56 and 90 days in B20 at 40 °C and 70 °C according to ISO 815-1 “Rubber, vul-canized or thermoplastic - determination of compression set – Part 1: At ambient or elevated temperatures”.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore, a threshold of 15 % was determined for the evaluation of the compatibility.
The change of tensile strength and breaking elongation of test specimens made of ACM, FKM, HNBR, PA, PE, POM, PUR and PVC exposed to heating oil and the blend B20 was less than 15 % at 40 °C. A maximum reduction in Shore hardness A of 14 % was determined for ACM at 40 °C and for HNBR of 15 % at 70 °C.
It can be concluded that ACM, FKM, HNBR, PA, PE, POM, PVC and PUR were resistant in B20 at 40°C. FKM, PA, POM and PVC were evaluated as resistant in heat-ing oil and B20 at 70 °C, HNBR and PUR were not resistant in these fuels at 70°C.
Based on the mass increase and compression set values of FKM test specimens it can be stated that FKM is resistant in B20 under compressed conditions at 40 °C and 70 °C.
The presented study deals with the performing and mechanical testing of single pass hybrid laser-arc welds (HLAW) on 25 mm thick plates made of steel grade S355J2. One of the challenges have to be solved at full penetration HLAW of thick plates is the drop formation occurring due to the disbalances of the forces acting in the keyhole and on the melt pool surface. Such irregularities mostly limit the use of high-power laser beam welding or HLAW of thick-walled constructions. To overcome this problem, an innovative concept of melt pool support based on generating Lorentz forces in the weld pool is used in this work. This method allows to perform high quality welds without sagging even for welding of 25 mm thick plates in flat position at a welding speed of 0.9 m min-1. For the obtain of full penetrated welds a laser beam power of 19 kW was needed. A high V-impact energy of up to 160 J could be achieved at the test temperature of 0 °C. Even at the most critical part in the weld root an impact energy of 60 J in average could be reached. The tensile strength of the weld reaches that of the base material. An introduce of the HLAW process with electromagnetic support of the melt pool in the industrial practice is an efficient alternative to the time- and cost-intensive arc-based multi-layer welding techniques which are established nowadays for joining of thick-walled constructions.