Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
- nein (287)
During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained.
The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution.
Formation of interphases between inorganic nanofillers and thermoplastic matrices are usually correlated to short-range interactions which does not exceed more than tens of nanometers away from the surface of the filler. Nevertheless, in nanocomposites with thermosetting matrices, the effect of nanofillers on the properties of the matrix is not limited to the immediate vicinities, but a long-range property alteration of the bulk polymer may be observed. The interaction between nanofillers and the polymer can disturb the curing reaction and alters the chemical, physical and mechanical properties of the polymer network in the matrix phase. In our studies, we aim to investigate short and long-range interphases of a nanocomposite system consisting of a thermosetting matrix (DGEBA) filled with an inorganic nanoparticle (boehmite). For this purpose, a combination of atomic force microscopy (AFM)-based approaches is implemented. Scanning kelvin probe microscopy (SKPM) was used to map the compositional contrast and the interphase with different electrical properties than the bulk. The mechanical properties of the interphase were probed by high resolution intermodulation AFM. (ImAFM). Furthermore, infrared spectroscopy AFM (AFM-IR) is used to investigate the chemical structure of the matrix at different distances from the nanoparticle. SKPM and (AFM-IR) measurements both show a long-range (to 10 µm) effect of boehmite on the chemical structure and surface potential of the bulk epoxy, respectively, whereas ImAFM force measurements reveals a short-range mechanical interphase between the filler and the matrix. The AFM-IR demonstrated the existence of unreacted anhydride hardener at the interphase. This indicates the preferential absorption of anhydride on the surface of boehmite. The consequence of such a selective interaction between the inorganic filler and the epoxy components is disturbance of the epoxy-hardener stoichiometric ratio, the curing mechanism. and the alteration of bulk properties of the matrix.
A new dual purpose cask design was developed for the safe transport and interim storage of spent fuel elements of German research reactors. In the framework of the safety assessment within the licensing procedure the Bundesanstalt für Materialforschung und –prüfung (BAM) as competent authority performed a series of drop tests according to the IAEA-Regulations. The package consists of a cylindrical thick-walled ductile cast iron cask body closed by a double lid system with metallic seals. A lid and bottom sided impact limiter consisting of a wood/steel construction limit the mechanical impact loading. The full-scale test specimen was equipped with a basket and assembled with dummy-fuel elements. The package and test specimen, respectively have a total mass of approximately 24 metric tons.
The mechanical test program included three 9m free drop tests, in horizontal, vertical and oblique cask orientation onto the lid system. Additionally, a 1m-puncture drop test followed the horizontal drop test to consider an IAEA-test sequence. The horizontal and vertical drop tests were performed at a temperature of minus 40°C. During the oblique drop test the upper impact limiter was heated to +80°C. The tests were conducted onto an unyielding target, fulfilling the requirements of the IAEA regulations.
The test specimen was considerably instrumented with strain gauges and accelerometers. Transient strains at selected locations of the inner and outer container walls, of the primary and secondary lid, as well as of the corresponding lid bolts were measured during the drop tests. Furthermore, decelerations in different locations at the cask body and the lids were measured. The complex geometrical deformation of the impact limiters due to the impact were determined by optical 3d- measurements using the projected fringe method in combination with multi-image photogrammetry. Before and after the drop tests the leakage rate of the lid system was determined by helium leakage testing.
The experimental results contribute to the evaluation of the package response to mechanical tests, demonstrating safety under normal and accident conditions of transport. Especially to the verification of the dynamic finiteelement model of the package used in the package design safety report. The paper describes the performance of the drop tests, selected test results focusing on the lid screws and the cask body and the deformation of the impact limiters as well as impact kinematics, respectively.
Glass
(2019)
Overview about the key activities of division 5.6 glass and the diversity of the material glass. For the vacuum hot extraction method (VHE-MS) some examples are presented e. g. for the measurement of water content or the determination of diffusion coefficient of hydrogen in glasses. Finally, an outlook is shown on the robot controlled glass screening device which will be available next year.
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered ¬glass-ceramics, glass matrix composites or glass bonded ceramics with tailored mechanical, thermal, electrical and optical properties and complex shape. Its wide and precise adjustability makes this class of materials a key component for advanced technologies. Processing of glass or composite powders often allow even more flexibility in materials design. At the same time, however, processing can have substantial effects on the glass powder surface and sinterability. Thus, mechanical damage and surface contamination can strongly enhance surface crystallization, which may retard or even fully prevent densification. Whereas sintering and concurrent crystallization have been widely studied, partially as cooperative effort of the TC7 of the ICG, and although glass powder sintering is predominantly applied for glasses of low crystallization tendency, sintering is also limited by gas bubble formation or foaming. The latter phenomenon is much less understood and can occur even for slow crystallizing glass powders. The lecture illustrates possible consequences of glass powder processing on glass sintering, crystallization and foaming.
In service, most materials are operated under simultaneous corrosive and mechanical load and there are very few methods capable for testing material degradation under these conditions, especially when it comes to high resolution analysis. For this purpose, in this work, a tensile module capable of uniaxial stretching and compression with up to 5 kN force was integrated into an AFM stage. The elimination of the need for sample unmounting and remounting and the resulting possibility of keeping the sample under constant mechanical load during AFM measurements not only enables a precise positioning of the area of interest but also allows for the analysis of processes in the elastic deformation regime.
This methodology was demonstrated for two case studies. Scanning Kelvin Probe Force Microscopy (SKPFM) was used as the main tool to characterize the deformation behavior. Moreover, a flexible electrochemical measurement cell was used to enable electrochemical analysis by means of electrochemical impedance spectroscopy (EIS) and Linear Sweep Voltammetry (LSV) during AFM measurements at different levels of strain. The in situ AFM results are complemented by microstructure analysis by means of electron backscatter diffraction (EBSD).
In the first case study, the deformation induced delamination of a thin organic coating on AA2024 T3 aluminium alloy was investigated as a function of alloy surface treatment. The formation of cracks in the insulating passive film enabled an early detection of deformation processes by means of SKPFM. The second case study focused on the comparison of corrosion and deformation behavior of conventional and additively manufactured 316 stainless steels. In comparison to the conventional 316 stainless steel, the effect of processing was clearly detectable on the additively manufactured material as zones of inhomogeneous potential, which also affected the initiation of local corrosion processes. The contribution will provide detailed information on the new AFM setup and summarize our results from both case studies.
The performance of functional coatings and adhesively joined hybrid components relies strongly on the stability of the polymer-metal interface. With the increasing utilization of multi-material structures in the automotive and aerospace industry, it is of great scientific and technical interest to understand the processes leading to interface degradation and to develop novel strategies to increase corrosion and delamination resistance.
The aim of this project is to develop thin epoxy-based films and their carbon nanofiller loaded composites on aluminium alloy AA2024-T3 as a model system and to investigate their interfacial stability under corrosive and coupled corrosive-mechanical load. Spin coating was used for the layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Atomic force microscopy (AFM) results indicate a very homogeneous and dense film with low surface roughness. Carbon nanofillers were introduced either by mixing into the coating components or in between individual layers to control the separation between the carbon nanofillers and alloy surface. The film chemistry and barrier properties were characterized by means of spectroscopic and electrochemical methods, respectively. The degradation and delamination behavior of the epoxy-based films was characterized by means of in situ AFM corrosion experiments. The quantitative imaging (QI) mode allowed the observation of hydrogen-generation induced blister formation during exposure to corrosive electrolyte and how the local corrosion processes evolved with exposure time. Complementary energy dispersive X-ray spectroscopy (EDX) analysis was performed to correlate the corrosion behavior with the different intermetallic particle chemistries and distributions. The presentation will summarize our results on the effect of interface chemistry and carbon nanofiller – alloy separation on the initiation of local corrosion processes on thin film covered AA2024-T3 aluminium alloys.
The presentation summarizes our recent results on the coupled electrochemical methods for high resolution corrosion studies. The combination of Scanning Electrochemical Microscopy (SECM) and multielectrode (MMA) based real-time corrosion monitoring was presented as a new method for achieving high time resolution in local electrochemical analysis. Correlative imaging by means of Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) was demonstrated as a tool for the investigation of local corrosion processes initiated by the intermetallic particles (IMPs) on AA2024-T3 aluminium alloy.
The study presented here focusses on a systematic analysis of oxidation mechanisms of the well-known Cr20Mn20Fe20Co20Ni20 alloy and one of its ternary sub-system Cr33.3Co33.3Ni33.3 which were reported in the literature to exhibit attractive mechanical properties. Both alloys are single phase fcc prior to oxidation and were simultaneously exposed to different oxygen containing atmospheres at 700° C and 800° C for durations up to 288 h. Cr20Mn20Fe20Co20Ni20 showed poor oxidation resistance at high temperatures due to its high amount of manganese leading to the formation of non-protective Mn-oxide scales. In contrast, a relatively homogeneous and protective chromia layer was found to form on CrCoNi at 700° C and 800° C after each exposure time. Mass change-, SEM- and XRD analysis of the oxide layers were performed in the present study and provide a better understanding of the oxidation mechanisms as well as the impact of the alloy composition on oxidation behavior.
The common fatigue life certification of aircrafts according to the certification Standards 23 and 25 follows a building block approach. Static tests at room temperature as well in humid and high temperature conditions are done on the coupon level. Additionally, a full-scale static and fatigue test must be performed on the complete airframe (minimum on the fuselage together with the wing). For each type-certificate the complete building block approach test program must be performed.
Traditionally in Germany, the certification of sailplanes (Certification Standard 22) follows rather a family concept. A shared data base was created over the last 50 years based upon a large number of material testing. In addition to static tests at room temperature and hot-humid conditions, fatigue tests are also done on the coupon level. Additional static and fatigue tests were done on complex structures such as spar-beams, fuselages and full-scale wing structures. However, for each type-certificate, only static tests should be performed in full-scale. This concept is determined by the certification memorandum CM-S-006 “Composite Lightweight Aircraft” 2017.
The presentation was given as an introduction to the discussion about the future expectations and developments of the EASA concerning the type-certification of lightweight aircrafts according to CS22 at the OSTIVE Sailplane Development Panel Meeting at the EASA in Cologne on the 11th of October 2019.
Over the past years economic and environmental considerations have led to a markedly increased demand for efficiency and flexibility in petrochemical plants. The operational temperatures and pressures required today can only be achieved by using new creep-resistant grades of steel. The modified 13CrMoV9-10 vanadium steel shows a good resistance against creep and compressed hydrogen and has been in use for the construction of petrochemical reactors since the mid-1990s. Nevertheless, processing of this type of steel requires extreme care during the welding procedure. This is due to its low toughness and high strength in the welded state when not post weld heat treated combined with increased susceptibility to cracking during stress relaxation. Previous research into crack formation in creep-resistant steels has largely focused on thermal and metallurgical factors; however, little knowledge has been gathered regarding the influence of the welding procedure on crack formation during post weld heat treatment considering real-life manufacturing conditions. The influence of heat control on the mechanical properties has been investigated by simulating the welding and subsequent post weld heat treatment operations during the construction of petrochemical reactors using a special 3-D testing facility on the laboratory scale.
This work is subdivided in two parts. In part I of this study the stresses resulting from preheating, welding, dehydrogenation heat treatment and the final post weld heat treatment were analyzed during experiments under varied heat control. In all experiments stress relief cracks formed during post weld heat treatment could be observed. The total crack lengths correlated with the welding induced stresses.
Part II of this work is dedicated to the characterization of the cracks and the microstructure. The application of a special acoustic emission analysis indicated that the cracks formed in a temperature range between 300 °C and 500 °C during the post weld heat treatment. In comparison to small scale specimens welded without additional shrinkage restraint, the toughness of the restrained welds was significantly decreased. SEM and TEM analyses of all samples revealed accelerated aging due to early precipitation of special carbides during post weld heat treatment under component relevant restraint.
Using magnetic materials for energy conversion as an example, this lecture shows how X-ray tomography investigations can contribute to structure elucidation in composites and solid samples. The components are tested non-destructively in order to characterize cracks, pores and other defects and their influence on the functional properties three-dimensionally and in good time in the life cycle of the material. If you combine microtomography with other methods of magnetic material characterization, you can make unique statements about the structure and the functional properties.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
To date, there are very few technologies available for the conversion of low-temperature waste heat into electricity. Thermomagnetic generators are one approach proposed more than a century ago. Such devices are based on a cyclic change of magnetization with temperature. For thermomagnetic materials, we used a commercial magnetocaloric alloy with a transition temperature of 300 K.
To date, there are very few technologies available for the conversion of low-temperature waste heat into electricity. Thermomagnetic generators are one approach proposed more than a century ago. Such devices are based on a cyclic change of magnetization with temperature. For thermomagnetic materials, we used a commercial magnetocaloric alloy with a transition temperature of 300 K.
Using magnetic materials for energy conversion as an example, this lecture shows how X-ray tomography investigations can contribute to structure elucidation in composites and solid samples. The components are tested non-destructively in order to characterize cracks, pores and other defects and their influence on the functional properties three-dimensionally and in good time in the life cycle of the material. If you combine microtomography with other methods of magnetic material characterization, you can make unique statements about the structure and the functional properties.
Ink recipes from the islamic era: Texts, manuscripts, ink reproductions and scientific analyses
(2019)
Ink recipes can often be found in Arabic manuscripts. They may be included in treatises of diverse subjects – from handbooks for secretaries or calligraphers to books on arts and crafts, to alchemical and astrological essays. Recipes can also appear, with or without relation to the main text in the manuscript, in the form of lists or collections or even added in empty spaces as single entries. Why were these recipes written down? Were they used by the many professionals dealing with inks in their every-day work? Or were they part of the literary genre of adab with little or no practical application? To answer these questions a research project was set up: ink recipes have been collected from written Arabic sources, their feasibility has been assessed and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, most non-invasive and non-destructive, and the results compared to the data obtained by the application of the same analyses on concrete manuscripts. The codicological characteristics of the manuscripts have also been studied. My aim in this talk is to show how such an interdisciplinary approach could be beneficial for the study of material culture.
Fifty shades of black: Typologies and terminology of black inks in the light of new discoveries
(2019)
The identification of the materials constituting an artefact is the basis of any correct conservation project. For this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies of illuminated manuscripts where the black media used to write the text is largely overlooked. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources, their feasibility has been assessed, and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and to verify the detection limits of the equipment employed. Finally, the results were compared to the data collected from historical manuscripts.
In this talk I will focus on the ink typologies and the terminology (ancient and modern) used to describe them. In particular I will highlight how even the modern classification fails to capture the variety encountered in both recipes and manuscripts, particularly in the light of recent discoveries. I will address especially the terminological and conceptual issues of mixed inks – in the form of carbon inks and tannins, of carbon and iron gall inks, and of carbon and metallic salts –, iron gall inks made without vitriol and iron gall inks made with sources of tannins different from gall nuts.
Papyrus was in use in the Islamic world until the 11th century and few ink recipes collected from treatises about the art of the books are dedicated to this support. But papyrus was also burnt in order to obtain soot used as an ingredient for a particular type of ink (midād al-qarāṭīs). In this talk I will give an overview of the recipes – in particular those by ar-Rāzī –, their context and transmission in order to evaluate this double nature of papyrus, which is considered at the same time a writing support and a material to be recycled. Moreover, I will discuss what kinds of ink are most likely to be found, according to these literary sources, on Arabic manuscripts and documents written on papyrus and compare them to the typologies mentioned for paper and parchment. These results are the premises of a research project starting at the beginning of 2019, in which a number of dated fragments from several European institutions will be analysed with non-destructive techniques in order to establish a profile of the main writing media used in the early centuries of the Islamic Era.
Statistically the mean time between damage events on rotor blades is 6 years (Deutscher Windenergie Report 2006). Due to imperfection in the production the shell structures get cracks after a few years fare before the designed life time. A shell test rig was built at BAM for efficient research on the effects of defects in production.
In-situ and ex-situ NDT give a better understanding from degradation processes in composite materials.
With advanced methods in the research on the fatigue behaviour of FRP it was found a load level of infinite life for GFRP and CFRP. This is in the range of typical strain values of airliners and rotor blades in normal operation.
Due to the fibre-composite nature NDT techniques have to be suitable to a wide length scale to image micro cracking as well as bigger defects. Therefore different techniques have to be applied and developed.
Even for the basic measurements of material data for design and engineering of composite structures there is a need to upgrade standards. With a new shear frame test rig more precise values can be obtained.
With advanced methods in the research on the fatigue behaviour of FRP it was found a load level of infinite life for GFRP and CFRP. This is in the range of typical strain values of airliners and rotor blades in normal operation.
Statistically the mean time between damage events on rotor blades is 6 years (Deutscher Windenergie Report 2006). Due to imperfection in the production the shell structures get cracks after a few years fare before the designed life time. A shell test rig was built at BAM for efficient research on the effects of defects in production.
Test blades of ~10m are an efficient way for SHM research and evaluation of NDT-methods and blade geometry.
The Interdisciplinary Alchemist: Reproduction and Study of Black Inks from the Islamicate World
(2019)
The identification of the materials constituting an artefact is the basis of any correct conservation project, for this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies, often producing unclear results, especially for black inks. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources on bookmaking, their feasibility has been assessed, and finally some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. In this talk I will present some instances of how this approach can help textual criticism, for example in evaluating variants and determining the competence of authors and compilers. At the same time the research highlights how much this scientific work depends on textual studies, especially concerning the identification of ingredients. Moreover, I will focus on some of the problematics I faced both during the textual interpretation and the actual reproduction of the recipes and how they influenced the results of the scientific analyses. In particular I’ll look into the role played by the degree of purity of the components and the function (real and perceived) of some of the ingredients.
Functional materials for energy conversion are important technology drivers needed for the implementation of low carbon energy. Therefore, researchers commonly focus on improving the intrinsic properties of a functional material. However, for applications, the extrinsic properties are at least as important as the intrinsic ones. Consequently, it is important to investigate and understand the external and internal structure of semi-finished products and especially defect dependent properties. The extrinsic properties may change during application and the life cycle of the material as well as through processing and molding steps.
Our studies show how X-ray tomographic (XCT) investigations can contribute to structure investigations in composites and massive samples using the example of magnetic materials for energy conversion. The components are tested non-destructively in 3D in order to localize and characterize cracks, pores, inclusions as well as other defects and their influence on the functional properties and also “in-time” during the life cycle of the material. Exsitu and in-situ experiments performed with non-destructive XCT are predestinated to follow damaging mechanisms of materials under certain load conditions, atmospheres or liquids, e.g. went through several working cycles of a functional material. By combining microtomography with other methods of magnetic and classical material characterization, unique statements about the structure and the functional properties can be made.
From the applications point of view, sometimes complex, three-dimensional geometries are needed to fully exploit the functional properties of the materials, e.g. to ensure a high surface area for heat exchange. Since many functional materials are brittle and difficult to form, shaping is often a big challenge. In principle, additive manufacturing processes offer the possibility to produce complex, porous components from poorly formable alloys.
If all stages of additive manufacturing are accompanied by X-ray tomographic imaging, the process of finding the optimal parameters for material processing can be significantly accelerated.
Based on the quality control of the initial powder material used and also investigations of the shape and arrangement of defects within the molten structure and their relationship with the melting path scanning strategy, Xray tomography has proven to be an ideal tool for additive manufacturing, even for functional materials. Overall, tomographic methods are important tools for the development of functional materials to application maturity.
The deep penetration laser beam welding (LBW) has developed to one of the most promising metal joining methods in the modern manufacturing industry. It has well-known advantages of good penetration capacity, low heat input, high reachable welding speed and low welding distortion in comparison to conventional arc welding techniques. However, there are still challenges in LBW making the realization of the advantages difficult, such as porosity or inhomogeneous element distribution when using filler material. The magnetohydrodynamics technique is a promising way to solve these issues by introducing a suitable electromagnetic field, and correspondingly Lorentz force, to control the Transport phenomena in the weld pool.
The underlying physics in wire feed laser beam welding with electromagnetic stirring were investigated numerically and experimentally. A three-dimensional transient heat transfer and fluid flow model coupled with dynamic keyhole, magnetic induction and element transport was developed for the first time. The electromagnetic behaviour as well as the temperature and velocity profiles, solidification parameters, keyhole evolution and element transport are calculated.
The model is well tested against the experimental results. The beneficial effects from electromagnetic stirring (element homogenization and grain refinement) are explained quantitatively using the numerical data and the results from high-speed imaging, OM, EDX and EBSD.
In this presentation the main requirements of BAM-GGR 016 regarding maintenance and periodic inspections were explained. BAM ensures during acceptance of the quality management program that specific and relevant instructions for maintenance and periodic inspections are developed and handed to the operator of the packaging. Examples are given.
It was found for inorganic/polymer nanocomposites that a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate into the entire system, affecting the overall nanocomposite properties. Here, the structure and molecular mobility of epoxy-based PNCs with different nanofillers (layered double hydroxide and boehmite) was studied by a combination of calorimetric and X-Ray scattering techniques. Temperature modulated DSC (TMDSC) showed that depending on the nanofiller, RAF can reach up to 40 wt % of the system or, on the contrary, the overall mobility of the matrix might increase due to the presence of particles. Such contrasting results, including the high amount of RAF, which was never shown before for epoxy-based PNCs, emphasize the importance of interfaces. Additionally, glass transition and glassy dynamics were investigated by a novel technique, Flash DSC (heating rates up to 10 kK/s) employed for the first time to a thermosetting system and electrospun fibers, which did not result in their degradation. It was used to study both the vitrification kinetics and glassy dynamics of the PNCs, for instance further confirming the presence of RAF and its impact on the overall material properties.
Challenges in Traceable Size Measurement of Non-Spherical, Non-Monodisperse Nanoparticles - nPSize
(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.zeige mehr
Laser beam welding of aluminum die casting is challenging. A large quantity of gases (in particular hydrogen) is absorbed by aluminum during the die-cast manufacturing process and is contained in the base material in solved or bound form. After re-melting by the laser, the gases are released and are present in the melt as pores. Many of these metallurgic pores remain in the weld seam as a result of the high solidification velocities. The natural (Archimedean) buoyancy is not sufficient to remove the pores from the weld pool leading to process instabilities and poor mechanical properties of the weld. Therefore, an electromagnetic (EM) system is used to apply an additional buoyancy component to the pores. The physical mechanism is based on the generation of Lorentz forces, whereby an electromagnetic pressure is introduced into the weld pool. The EM system exploits the difference in electrical conductivity between poorly conducting pores (inclusions) and the comparatively better conducting aluminum melt to increase the resulting buoyancy velocity of the pores. Within the present study, the electromagnetic supported degassing is investigated in dependence on the laser beam power, welding velocity and electromagnetic flux density. By means of a design of experiments a systematic variation of these parameters is carried out for partial penetration laser beam welding of 6 mm thick sheets of wrought aluminum alloy AlMg3 and die-cast aluminum alloy AlSi12(Fe) where the wrought alloy serves as a reference. The proportion of pores in the weld seams is determined using X-ray images, computed tomography (CT-) images and cross-section images. The results prove a significant reduction of the porosity up to 70 % for both materials as a function of the magnetic flux density
Diffraction-based experimental determination of Residual Stress in AM parts: A critical discussion
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, not always paralleled by the knowledge about the materials properties and performance. In particular, residual stress (RS) has been soon recognized as an issue in AM parts, so that parts are always post-heat-treated. Moreover, much effort has been spent on simulating RS, especially using finite element methods.
The experimental determination of RS has thereby become increasingly important, and even simple data constitute (to date) a piece of knowledge to fill the above-mentioned gap. In particular, diffraction methods, which are basically non-destructive, offer enormous possibilities to gain knowledge on real components, since neutrons and synchrotron radiation can penetrate even heavy metals up to several millimeters (or even centimeters). Indeed, some success has been obtained, and the knowledge about the origins of the RS fields, as well as their variation as a consequence of heat or mechanical treatments, has been greatly expanded.
In this talk, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with focus on those produced by laser powder bed fusion) has even allowed showing that process parameters that were considered unimportant play a major role in the onset of stress.
However, while RS is starting to be considered in the part 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 investigated about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even to date unclear will also be discussed, such as the determination of the reference unstrained samples and of the principal axes of stress. All these aspects will draw the path towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Localized laser surface treatments are able to produce tailor-made surface properties to fulfill requirements of a variety of technical applications. Especially micrometric surface topologies can be beneficial for optimizing tribological contact situations. Structures with lowered surface features are already utilized for bearings or cylinders of combustion engines. There are also other fields of application, where the potential of protruding surface features is known, e. g. for metal forming tools.
A promising approach for a tailored surface treatment working in the microsecond range is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This technique is able to produce micrometric surface structures and to improve simultaneously the wear resistance by creating metal matrix composites.
In this talk, the laser implantation technique is described and compared to the state of the art. The potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces is demonstrated by means of microstructural and topographical investigations of different ceramic materials and steel substrates. Finally, results of research projects are presented aiming on the application of such structured surfaces. Their capability to change and optimize friction and wear are demonstrated for fully lubricated contacts, tools for hot sheet metal forming and tools for cold rolling of sheets for automotive applications.
Polymers of intrinsic microporosity (PIMs) have recently emerged as novel materials for a broad range of high-performance applications from gas separation to electronic devices. The very rigid, contorted polymer chains show only limited molecular mobility and therefore pack inefficiently giving rise to intrinsic microporosity with pore sizes generally smaller than 1 nm resulting in BET surface areas larger than 700 m2/g. Using conventional thermal analysis techniques, no glass transition temperature (Tg) of PIMs could be unambiguously detected up to now. Employing fast scanning calorimetry (FSC) based on a one chip sensor, decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this limitation. The FSC device is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. Evidence of a glass transition is obtained for a series of PIMs with different chain rigidities. Local small-scale fluctuations are held responsible for the glass transition of highly rigid PIMs rather than segmental motions as in conventional polymers.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Finally, I will show that BAM is very active in standardization and certification, including production of Reference Materials and Methods.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Force-distance curves have been recorded on thin films of lubricants. The lubricants wet the AFM tip, which causes a capillary force. This force depends on the shape of the tip, as well as on physical properties like viscosity and surface tension, which have been determined additionally with other methods. This way, their influence on the shape of the curves could be analyzed.
At BAM, which is a federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes assessment of elastomeric seals applied in the casks. One of the aims is to identify a suitable method for estimating the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to five years. In order to assess sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings were aged as well. In order to understand the underlying ageing mechanisms in each material, material properties such as hardness, density and tensile properties were examined. Additionally, compression set (CS), which represents the recovery behaviour of a seal after release from compression, is measured. For obtaining results closely related to practical conditions, O-rings with a full-scale cord diameter of 10 mm were aged. However, this set-up can lead to heterogeneous ageing caused by diffusion-limited oxidation (DLO) effects especially for HNBR, resulting in distorted bulk properties such as compression set. However, if DLO-affected data is excluded, extrapolations of CS data are possible using time-temperature shifts.
For selecting an appropriate end-of-lifetime criterion, leakage rate measurements were performed, since leakage rate is the only characteristic directly correlated to the performance of the sealing system. A significant increase in leakage rate was considered as the end of the lifetime. However, the O-rings remained leak tight under static conditions even though material properties had already degraded strongly. For this reason, a modified, more demanding leakage test involving a fast small decompression of the seal was developed that allowed determining a more conservative end-of-lifetime criterion with a safety margin for EPDM seals. FKM, which is a very heat and oxidation resistant material, exhibited only little degradation, even though it had the smallest activation energy.
At the Stakeholder meeting of the EMPIR project “Multifunctional ultrafast microprobes for on-the-machine measurements”, details about two measurement modes were presented. Force distance curves and contact resonance measurements are compared. The basic principles are explained and exemplary measurements concerning mechanical properties of polymers are shown.
High heat input leads to grain coarsening and softening in WM and HAZ; the tensile strength is reduced. Low heat input leads to inadmissible hardening in the WM; the impact strength is reduced.
The proposed t8/5-time of 3 s to 15 s could be achieved through the reduced welding velocity.
The concept of electromagnetic weld pool support system allowed single-pass welds in flat position without gravity drop-outs even for reduced welding speeds; in this way the heat input can be controlled.
The adaptation of the electromagnetic weld pool support system to laser and laser hybrid welding process can dramatically increase the potential field of application of these technologies for real industrial implementation.
Microstructure ageing of stainless steel AISI 316L manufactured by selective laser melting (SLM)
(2019)
Additive manufacturing (AM) processes, such as SLM, offer a variety of advantages compared to conventional manufacturing. Today AM parts are still comparatively less cost-effective if they are manufactured in large quantities. To make the AM parts more cost-efficient, the AM process has to be improved. It requires a good understanding of microstructure formation, microstructure-property-relations and ageing processes affected by different loads.
In this work the ageing behavior of SLM manufactured AISI 316L stainless steel is evaluated. The microstructure effected by mechanical, thermal and corrosive loads are investigated and compared to as-built microstructure. Tensile tests are used for mechanical ageing. For thermal and corrosive loads the typical application conditions of 316L apply. The methods of microstructure investigation include SEM, TEM, CT and EBSD. The main object of this work is the description of microstructure and ageing processes of AM parts.
Additive manufacturing (AM) offers diverse advantages compared to conventional manufacturing. In this work the microstructure of austenitic steel 316L, manufactured with Selective Laser Melting (SLM), was analyzed and compared to microstructure of 316L hot rolled material. Methods used for analysis are microprobe, optical microscopy and electron backscatter diffraction.
The distributed measurement of relative humidity is a sought-after capability for a wide range of applications in civil engineering and structural health monitoring. We show that polymethyl methacrylate (PMMA) optical fi-bers can be employed as a sensor medium to conduct distributed humidity measurement by analyzing Rayleigh backscattering traces obtained by OTDR. We make use of the effect that water penetrates the fiber core and directly influences the local fiber attenuation and Rayleigh backscatter coefficient. We conducted distributed backscattering analysis for two different pulse wavelengths: 500 nm and 650 nm. The 650 nm results are susceptible to both, attenuation changes and backscatter changes, whereas backscatter results at 500 nm are not affected by humidity-induced attenuation and only exhibit a change of Rayleigh backscattered power as a function of humidity. The combined measurement and analysis of both parameters at these two wavelengths has the advantage that cross-sensitivities on backscatter change and attenuation, such as strain and tempera-ture changes, could be separated from the humidity response of the fiber. We present laboratory results for a humidity range between 30% and 90% for both pulse wavelengths: including step responses, humidity cycles and hysteresis analysis. In addition to the attenuation and backscatter coefficient dependence, we also analyze optical runtime changes as a function of humidity. POFs have the advantage that they can be directly embed-ded into materials such as concrete or soil to measure water content or localize water ingress. Standard step-index PMMA POFs can be used as a distributed relative humidity sensor up to 200 m distance.
Composite pressure vessels for transporting dangerous goods and for hydrogen and natural gas vehicles consist of a load-bearing composite and a gas-tight, metallic or polymeric barrier layer (liner). To investigate the aging behavior of such composite pressure vessels, BAM carried out the interdisciplinary project COD-AGE. The aim of the project was the development of methods and models for the description and determination of the aging behavior of carbon fiber composites using the example of pressure vessels in order to better predict aging and safe working life. One focus of this project was the provision of suitable NDT methods. These included both test-related tests and the possible development of test equipment for later practical use.
In the lecture, test results of the age-related eddy current test on composite pressure vessels are presented.
In aging tests, pressure vessels made of an approximately 4 mm thick aluminum liner and approx. 8 mm thick CFRP layer were examined. Typical application of such pressure vessels are respiratory protective devices of the fire department. The pressure vessels were tested using conventional eddy current technology from the outer and inner side as well as with high-frequency eddy current technology. Both damage to the metallic liner and structures of the CFRP could be detected. A particular mechanical challenge was the inspection of the inside of the liners, since a cylindrical surface with an inside diameter of 150 mm has to be tested with an access of only 15 mm diameter.
Chemical compositions of the welds have significant effect on weld quality. Current inspection methods for the weld seams employ mostly post factum methods and cannot prevent weld defects.Elemental burn offs may significantly affect solidification leading to embrittlement or cracking. Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects.
An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies.
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.
Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured (AM) parts and important factors for residual stress formation which have implications on structural integrity. This study examined the influence of heat input on the distribution of residual stresses in two prisms produced by laser powder bed fusion (L-PBF) of austenitic stainless steel 316L.
The layers of the prisms were exposed using two distinct helix scanning strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. Residual stresses were characterised at one plane perpendicular to the building direction at half of its build height using neutron diffraction. In addition, the defect distribution was analysed via micro X-ray computed tomography (µCT) in a twin specimen.
Both scanning strategies reveal residual stress distributions typical for AM: compressive stresses in the bulk and tensile stresses at the surface. However, temperature gradients and maximum stress levels differ due to the different heat input. Regarding the X-ray µCT results, they show an accumulation of defects at the corners where the laser direction turned through 90°.
The results demonstrate that neutron diffraction and X-ray µCT can be successfully used as non-destructive methods to analyse through-thickness residual stress and defect distribution in AM parts, and in the presented case, illustrate the influence of scanning strategies. This approach contributes to deeper assessment of structural integrity of AM materials and components.
Laser based Powder Bed Fusion (L-PBF) is an additive manufacturing technique that has been continuously developed in the past years. It offers unparalleled design freedom and the resulting mechanical properties match, in some cases even exceed, those of materials processed by conventional manufacturing techniques. Nonetheless the process is prone to create Residual Stresses (RS) resulting from the sequential melting and solidification of the material. RS can reduce load bearing capacity and generate unwanted distortions thus diminishing the potential of L-PBF. This research activity aimed at characterizing the RS state in Inconel 718 L-PBF specimens using multiple diffraction methods. The microstructure as well as the surface and bulk residual stresses were investigated. The RS analysis was performed using X-ray, synchrotron and neutron diffraction methods to provide information at different depths within the specimen. The measurements were performed at the Bundesanstalt für Materialforschung und –prüfung (BAM), the EDDI beamline at BESSY II synchrotron and E3 line at BER II neutron reactor of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results revealed a depth depending RS state. The longitudinal and transverse stress components measured by X-ray and synchrotron at the surface agree well, exhibiting stress values around the yield strength of the material. In addition, synchrotron mapping showed gradients along the width and length of the sample for the longitudinal and transverse stress components. Lower RS values compared to surface RS were measured in the bulk of the material using neutron diffraction. The longitudinal stress component in the bulk was tensile and gradually decreased towards the edge of the specimen. The normal component however did not change significantly along the specimen dimensions and was of compressive nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers, which has to be further investigated.
Welding residual stress engineering by means of an adjusted martensite phase transformation would be highly attractive as detrimental tensile residual stresses may be prevented already during welding without time and cost intensive post processing. The present study shows a synchrotron diffraction analysis of a martensitic steel subjected to thermo-mechanical load cycles. Experiments were conducted regarding the microstructural strain response during the austenite to martensite transformation. The strains are a function of the temperature and the specific loads applied during cooling. The relation between the transformation plasticity of the material, the amount of martensite formed and the arising strains can thus be assessed. The lattice plane specific strains were compared to experimental findings from (macro) dilatation tests. It is shown that the microscopic material behavior differs remarkably from the one observed on the macroscopic scale, what leads to characteristic residual stresses in the material.
Residual stresses are crucial when assessing the performance of welded components. The present work deals with the possibilities of transferring the real-life boundary conditions of welding, which influence the residual stress, into the laboratory. The possibilities of a test system with a load capacity of 2 MN specifically developed for online monitoring of stress formation and cracking are shown. Due to the structural design, global process, geometry and material-dependent stresses are induced, which can be quantified in-situ during welding and post weld heat treatment. Examples are presented how the conditions to be found during production are simulated in the laboratory. It is shown how welding residual stresses in high-strength steels are affected by the heat control. Elevated working temperatures significantly increase the tensile residual stresses in the heat affected zone (HAZ). The effect of mechanical stresses resulting from welding on stress relief cracking is demonstrated by the example of a creep resistant steel. Reheat cracks were monitored online during post weld heat treatment.
Microbiologically induced corrosion due to bacterial biofilms causes several problems in industrial systems, technical applications and in medicine. Prior to the formation of a biofilm on a substrate, planktonic cells attach on the surface. Hence, the properties of the surface play a key role in biofilm formation and are of great importance for the development of strategies to prevent bacterial attachment and biofilm formation.
This project aims at clarifying to which extent surface micro-/nanostructuring and chemical functionalization affects bacterial attachment and whether a synergistic combination of the two can be used to control bacterial adhesion. To answer these questions, model surfaces with regular patterns of 5-10 micrometers in size have been prepared, which provide distinct zones differing in terms of their chemistry or nano-roughness. This was achieved by micro contact printing of self-assembled monolayers with different functional groups and deposition of patterned ZnO nanorod arrays for studying the effect of surface chemistry and morphology, respectively. Typical contrasts studied were combinations of positively/negatively charged, hydrophobic/hydrophilic or flat/rough.
The attachment behavior of bacteria on tailored surfaces were studied in a flow chamber as a function of time. The strain Pseudomonas fluorescens SBW25 was chosen as a model organism. DNA-intercalating dyes such as Syto9 have a high affinity to adsorb on ZnO nanorods. To overcome this limitation a genetic modification was performed by introducing a gene which expresses a green fluorescent protein in P. fluorescens SBW25 enabling the quantitative evaluation of the flow chamber studies by means of fluorescence microscopy. Further analysis of the attachment behavior was performed by means of scanning electron microscopy.
The presentation will summarize the results of our systematic study on the role of individual parameters on bacterial attachment and highlight synergistic combinations, showing an inhibition or enhancing effect. As the investigations with model substrates enable a precise control of the surface parameters, this approach can be applied to different microorganisms and material systems to achieve a correlative description of bacterial adhesion on solid surfaces.
Weathering reference materials are used to characterize the harshness of an exposure, aiming on either reproducibility of a specific exposure or on the comparability between various kinds of weathering exposure.
The materials that are used as weathering reference materials differ in their sensitivities (as well as in interactions and interferences of the latter), conditioned by the different processes which lead to the respective property change. It is also essential to take into account the necessary measurement equipment for the respective property change, in order to allow timely intervention.
What are the key issues on choosing a weathering reference material?
What can be learned from the weathering reference materials, investigated so far?
Possibilities and limitations are discussed on the basis of existing weathering reference materials. Conclusions are drawn, for establishing new weathering reference materials.
Oxidation effects on the functionality and formation of laser-induced periodic surface structures
(2019)
In the last decades, the formation of laser-induced periodic surface structures (LIPSS) has been widely studied, not only to stablish a general understanding of the main mechanisms present during the irradiation with ultrashort laser pulses, but also to identify the main processing parameters for its fabrication on various technical materials. However, an important and almost always present effect that is typically set aside is the material oxidation during or after the laser processing. Usually, this leads to optical, chemical, structural and mechanical alterations that are seldomly studied in detail. Therefore, in this work we present a study that includes the formation of LIPSS on Ti6Al4V alloy for tribological applications were different oxidations layers are involved.
The material characterization using different techniques, such as energy dispersive X-ray analyses (EDX), X-ray photoelectron spectroscopy (XPS), micro Raman spectroscopy (µ-RS), and depth-profiling Auger electron microscopy (AEM), and other techniques, confirms the formation of a non-negligible superficial oxide layer – strongly dependent on the specific processing parameters. We perform tribological experiments on laser irradiated samples oxidized by alternative ways to have a comparison on its friction performance. The obtained results show significant differences that depend directly on the thickness and the quality of the oxidized layer. This may open a fertile research area until now barely explored with clear impact on LIPSS based applications.
This presentation reviews current and expected developments in the field of laser-induced periodic surface structures (LIPSS, ripples). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized radiation. LIPSS are formed in a “self-ordered” way and are often accompanying laser material processing applications. The structures can be produced in a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their spatial periods typically range from several micrometers down to less than 100 nanometers, exhibiting a clear correlation with the polarization direction of the laser radiation used. Various types of LIPSS have been classified, relevant control parameters were identified, and 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. Special attention will be paid to a comparison of the currently available formation theories for LIPSS with a discussion of their respective strengths and weaknesses. Currrently explored applications featuring surface functionalization in the fields of optics, surface wetting, medicine, and tribology will be discussed.
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.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range. During the past years significantly increasing industrial and research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical, biological, or chemical surface properties. In this contribution the mechanisms of formation and current trends and applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animals, the tailoring of surface colonization by bacterial biofilms, the advancement of leadless medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces.
Aluminum alloys are extensively used in the automotive industry. Particularly, squeeze casting production of Al-Si alloys is employed in the conception of metal matrix composites (MMC) for combustion engines. Such materials are of a high interest since they allow combining improved mechanical properties and reduced weight and hence improve efficiency. We investigate two types of MMCs, which can be potentially used for production of combustion engine pistons: 1) a near-eutectic cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 random planar oriented short fibers and 2) the same alloy reinforced with 7%vol. Al2O3 random planar oriented short fibers + 15%vol. SiC particles.
Complex 3D microstructure of the samples in as-cast condition, consisting of four and five phases (Al matrix, eutectic Si, intermetallics, Al2O3 fibers and SiC particles) was investigated by synchrotron computed tomography (CT). Advanced methods based on machine learning were applied for segmentation of all phases. This allowed extracting quantitative information such as volume fraction, shape and interconnectivity of every phase.
In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while CT on pre-strained samples to monitor and quantify damage. A micromechanical model was developed to simulate the evolution of the internal stress of each phase during uniaxial compression. We showed that in composites with the Al2O3 fiber mat plane perpendicular to the load axis the Al-alloy matrix presents a large hydrostatic stress component, i.e. undergoes compression also in the direction transverse to the external load. This feature holds with and without the addition of SiC ceramic reinforcement and is absent in the case when the Al2O3 fiber mat plane is parallel to the load axis. We show, that the intermetallics play a decisive role at very high loads, when all other reinforcement phases suffer (extensive) damage. The addition of SiC particles does alleviate the load on the Al2O3 fibers, on the eutectic Si, and on the intermetallic phases in both cases of parallel and orthogonal (to the load axis) Al2O3 fiber orientation. Apart from the beneficial addition of ceramic reinforcement, the presence of intermetallic phase and eutectic silicon, forming an interconnected network even at high loads, when single particles break, confers peculiar properties to these multi-phase composites.
Are we ready for putting a human footprint on Mars? Obviously, it is possible to send technologically challenging missions to our earth neighbors with a high level of complexity, such as enabling autonomous planetary mobility. As humanity contemplates mounting manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments safely working in space for years. Humans require water and air provided by complicated equipment. Its safe operation is a great challenge and implies being prepared for all eventualities. Instead of foreseeing and preparing for all possible scenarios of machine failures and accidents, it appears logic taking advantage of the flexibility of humans and providing essential equipment for the reaction on critical situations. The supply of spare parts for repair and replacement of lost equipment would be one key pillar of such a strategy. Bearing in mind the absolute distance and flight trajectories for manned missions to Mars, supplying spare parts from Earth is impossible. Thus, in space manufacturing remains the only option for a timely supply. With a high flexibility in design and the ability to manufacture ready to use components directly from a computer aided model, additive manufacturing technologies appear extremely attractive. For metal parts manufacturing the Laser Beam Melting process is the most widely used additive manufacturing process in industrial application. However, envisioning the handling of metal powders in the absence of gravitation is one prerequisite for its successful application in space. A gas flow throughout the powder bed has been successfully applied to compensate for missing gravitational forces in micro gravity experiments. The so-called Gas Flow Assisted Powder Deposition is based on a porous building platform acting as a filter for the fixation of metal particles in a gas flow driven by a pressure difference maintained by a vacuum pump.
Are we ready for putting a human footprint on Mars? Obviously, it is possible to send technologically challenging missions to our earth neighbors with a high level of complexity, such as enabling autonomous planetary mobility. As humanity contemplates mounting manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments safely working in space for years. Humans require water and air provided by complicated equipment. Its safe operation is a great challenge and implies being prepared for all eventualities. Instead of foreseeing and preparing for all possible scenarios of machine failures and accidents, it appears logic taking advantage of the flexibility of humans and providing essential equipment for the reaction on critical situations. The supply of spare parts for repair and replacement of lost equipment would be one key pillar of such a strategy. Bearing in mind the absolute distance and flight trajectories for manned missions to Mars, supplying spare parts from Earth is impossible. Thus, in space manufacturing remains the only option for a timely supply. With a high flexibility in design and the ability to manufacture ready to use components directly from a computer aided model, additive manufacturing technologies appear extremely attractive. For metal parts manufacturing the Laser Beam Melting process is the most widely used additive manufacturing process in industrial application. However, envisioning the handling of metal powders in the absence of gravitation is one prerequisite for its successful application in space. A gas flow throughout the powder bed has been successfully applied to compensate for missing gravitational forces in micro gravity experiments. The so-called Gas Flow Assisted Powder Deposition is based on a porous building platform acting as a filter for the fixation of metal particles in a gas flow driven by a pressure difference maintained by a vacuum pump.
Many of the most successful and precise additive manufacturing (AM) technologies are based on the deposition layer-by-layer of a flowable powder. Since the first pioneering work at the end of the 1980th many developments have been introduced, greatly extending the use of different materials, improving the physical properties of the components built and enhancing the accuracy of the process. Still very important issues remain nowadays, hampering a completely autonomous production of parts and even restricting the freedom of design by means of these technologies. One of the major issues is the low density and stability of the parts during the building process, which implies the need of support structures: The powder bed surrounding the part has an essential role, since it should support the structure during building, until it’s ready for removal. Moreover, the microstructure of the powder bed is a template for the microstructure of the part produced. In this context, the use of submicron ceramic powders is still a challenge. Three approaches for the stabilization and densification of powder beds will be presented: The Layerwise Slurry Deposition process LSD, the gas flow assisted powder deposition and the Laser Induced Slipcasting (LIS) of ceramic powder compacts.
Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductive and osteoinductive properties. However, resorption of modern materials for bone grafting (hydroxyapatite (HA) and tricalcium phosphate (TCP)) is reported, in some cases, to be not enough, this is why the search for more soluble compounds compared to HA and TCP looks very perspective. A possible way to increase ceramics solubility leads to partial substitution of Ca2+ -ions in Ca3(PO4)2 by alkali cations, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as the increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in the sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making the study of sintering of the ceramics mentioned above highly important.
To control Ca3(PO4)2 - CaKPO4 - CaNaPO4 based ceramic microstructure it is necessary to know possible phase transformations in the system and the way to manage microstructure by sintering schedule or sintering process.
In this work, an isothermal section for phase diagram of Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system is studied with several techniques. According to the XRD of quenched samples, this phase triangle has four single-phase areas at 1200˚C (Figure 1). It was shown that single-phase CaK0.6Na0.4PO4 cannot be sintered to full-dense ceramics by conventional sintering regardless time-temperature schedule. Two-step sintering technique, beneficial in the case of HA-ceramics, was unsuccessful in all cases of calcium-alkali phosphate compositions. However, field-assisted sintering techniques like, e.g. Spark Plasma Sintering (SPS), can overcome this problem due to significant impact on grain boundary diffusion. In connection with this fact, grains grow much slower retaining sintering process in a pore control regime. In this work CaK0.6Na0.4PO4 low-porous ceramics was also fabricated by FAST-methods of sintering. Moreover, other alternative sintering techniques, such as reaction sintering, may be useful in accelerating ions diffusion but stopping excessive grain growth.Strength properties of ceramics were evaluated by B3B-testing, micro- and nanoindentation techniques. Fracture toughness also becomes higher with potassium content increase, guiding porosity level.
Resorption properties of sintered ceramics were studied in different solutions with pH=5 and 7.4.
Acknowledgements. The research of sintering processes in calcium phosphate materials were funded by RFBR according to the research project № 18-33-00974.
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning.
Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures.
CEQAT-DGHS Interlaboratory Test Programme for Chemical Safety - Need of Test Methods Validation -
(2019)
Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory. Via the eChemPortal lots of data from the REACH registration dossiers are available. However, the quality and correctness of the information remains in the responsibility of the data submitter. Unfortunately, we found more or less appropriate information on physicochemical properties and concluded that more quality or adequacy of any data submitted will be needed.
Interlaboratory tests play a decisive role in assessing the reliability of test results. Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method.
In view of the interlaboratory test results the following conclusions can be drawn:
• To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty.
• A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods and not on proficiency tests.
• The laboratory management and the practical execution of the tests need to be improved in many laboratories.
• The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results.
Ambient water influences sub-critical crack growth (SCCG) from microscopic surface flaws, leading to stress corrosion at the crack tip. The complex influence of humidity accelerating slow crack propagation (region I) is well studied only for dry commercial NCS glass (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG water-bearing glasses. For this purpose, water-bearing silicate glasses of 8 wt% total water were synthesized at 0.5 GPa and compared to dry glasses. SCCG was measured in double cantilever beam geometry. For dry glasses, 3 trends in crack velocity vs. stress intensity, KI, curve were found. The slope in region I increases in the order NCS < NBS < BaCS < NZnS < NAS glass. The velocity range of region II, reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among these glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam0.5. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg internal friction peak caused by molecular water, and makes the glasses more prone to SCCG. The observed trends will be discussed in terms of the effects of Youngs Modulus on the strain energy release rate and energy dissipation related to mechanical glass relaxation phenomena.
Alkali silica reaction (ASR) is a major concrete durability problem resulting in significant maintenance and reconstruction costs for concrete infrastructures all over the world. To determine whether an aggregate is potentially reactive, accelerated concrete tests are used. Aim of this study is the chemical and microstructural characterization of ASR-products formed under the performance conditions of motorway pavements and during subsequent tests on the remaining ASR susceptibility. Samples were taken from concrete motorway pavements. Some of the samples already showed first indications for beginning damages whereas others showed deteriorations only after applying a performance testing procedure for the estimation of future risk of ASR damage. In a first step ASR-products were identified by polarized light microscopy in thin sections. The reaction products where then analyzed by Raman Spectroscopy and finally the chemical composition of the ASR-products was identified by SEM with EDX.
The results indicate that most reaction products show an increasing Ca/Si-ratio with progressive crack length. If an ASR-product develops inside an aggregate and moves through the cement paste, it has a high (Na+K)/Si-ratio at the beginning which decreases with increasing distance from its place of origin. The Raman spectra of the ASR-products are characterized by two broad bands indicating specific Q-species of different amorphous gel networks. Within the scope of the analysis distinctions in the microstructure and the chemical composition of the ASR-gels were detected relating to various conditions of accelerated testing.
Predictive Methods for Determining the Thermal Decomposition Properties of Hazardous Substances
(2019)
Due to the fast development and availability of computers, predictive approaches are increasingly used in the evaluation process of hazardous substances complementary to experiments. Their use was recommended as alternative to experimental testing by the REACH regulation to complete the lack of knowledge on properties for existing substances that must be registered before 2018 (upon quantities). Among the proposed predictive approaches, Quantitative Structure Property Relationships (QSPR) are powerful methods to predict macroscopic properties from the only molecular structure of substances.
In that context, the HAZPRED project (2015-2018, founded by the SAF€RA consortium) aims to develop theoretical models (e.g. QSPR) and small-scale tests to predict complex physico-chemical properties (e.g. thermal stability, explosivity) of hazardous substances to complete the lack of knowledge on these hazardous substances quickly or to understand their decomposition behaviour better.
In particular, this contribution will present the work done in this project on the physical hazards of organic peroxides and self-reactive substances: gathering of existing experimental data, new experimental campaigns, review of existing models and proposition of new estimation methods.
Despite of the significant advances in AM process optimization there is still a lack of experimental results and understanding regarding the mechanical behavior and microstructural evolution of AMparts, especially in loading conditions typical for safety-relevant applications e.g. in the aerospace or power engineering. Within the scope of the presented investigations, a characterization of the fatigue behavior of additively manufactured Ti-6Al-4V in the low cycle fatigue regime was carried out in the range of 0.3 to 1.0 % strain amplitude at room temperature, 250°C and 400°C. The Ti-6Al-4V specimens are machined out of lean cylindrical rods, which were fabricated using powder laser metal deposition (LMD) with an improved build-up strategy. The improved strategy incorporates variable track overlap ratios to achieve a constant growth in the shell and core area. The low-cycle-fatigue behavior is described based on cyclic deformation curves and strain-based fatigue life curves. The lifetimes are fitted based on the Manson-Coffin-Basquin relationship. A characterization of the microstructure and the Lack-of-Fusion (LoF)-defect-structure in the as-built state is performed using optical light microscopy and high-resolution computed tomography (CT) respectively. The failure mechanism under loading is described in terms of LoF-defects-evolution and crack growth mechanism based on an interrupted LCF test with selected test parameters. After failure, scanning electron microscopy, digital and optical light microscopy and CT are used to describe the failure mechanisms both in the longitudinal direction and in the cross section of the specimens. The fatigue lives obtained are comparable with results from previous related studies and are shorter than those of traditionally manufactured (wrought) Ti-6Al-4V. In this study new experimental data and understanding of the mechanical behavior under application-relevant loading conditions (high temperature, cyclic plasticity) is gained. Furthermore, a better understanding of the role of LoFdefects and AM-typical microstructural features on the failure mechanism of LMD Ti-6Al-4V is achieved.
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