5 Werkstofftechnik
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- 5 Werkstofftechnik (187)
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Eingeladener Vortrag
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As humanity contemplates manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments to safely work in space for years. The supply of spare parts for repair and replacement of lost equipment will be one key need, but in-space manufacturing remains the only option for a timely supply. With high flexibility in design and the ability to manufacture ready-to-use components directly from a computeraided model, additive manufacturing (AM) technologies appear extremely attractive. For the manufacturing of metal parts, laser-beam melting is the most widely used AM process. However, the handling of metal powders in the absence of gravity is one prerequisite for its successful application in space. A gas flow throughout the powder bed is successfully applied to compensate for missing gravitational forces in microgravity experiments. This 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.
Additive manufacturing of SiSiC by layerwise slurry deposition and binder jetting (LSD-print)
(2019)
The current work presents for the first time results on the Additive Manufacturing of SiSiC complex parts based on the Layerwise Slurry Deposition (LSD) process. This technology allows to deposit highly packed powder layers by spreading a ceramic slurry and drying. The capillary forces acting during the process are responsible for the dense powder packing and the good joining between layers. The LSD process can be combined with binder jetting to print 2D cross-sections of an object in each successive layer, thus forming a 3D part. This process is named LSD-print.
By LSD-print and silicon infiltration, SiSiC parts with complex geometries and features down to 1mm and an aspect ratio up to 4:1 could be demonstrated.
The density and morphology were investigated for a large number of samples. Furthermore, the density and the mechanical properties, measured by ball-on-three-balls method, were in all three building directions close to isostatic pressed references.
The layerwise slurry deposition (LSD) has been established in the recent years as a method for the deposition of ceramic powder layers. The LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade; each layer is sequentially deposited and dried to achieve a highly packed powder layer.
The combination of binder jetting and LSD was introduced as a novel technology named LSD-print. The LSD-print takes advantage of the speed of binder jetting to print large areas, parallel to the flexibility of the LSD, which allows the deposition of highly packed powder layers with a variety of ceramic materials.
The working principle and history of the LSD technology will be shortly discussed. A theoretical background will be also discussed, highlighting advantages and drawbacks of the LSD compared to the deposition of a dry powder.
The last part of the talk will be dedicated to highlight recent results on the LSD-print of SiSiC of geometrically complex components, in collaboration between BAM and HC Starck Ceramics GmbH. Density, microstructure and mechanical properties of LSD-printed and isostatic pressed samples will be discussed and compared.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles.
In powder bed Additive Manufacturing (AM) technologies, a part is produced by depositing and piling up thin powder layers. In each layer, the cross section of the object to build is defined by locally consolidating the powder, by sintering/melting the material (powder bed fusion technologies) or by ink jetting a binder (binder jetting technologies).
These are already leading AM technologies for metals and polymers, thanks to their high productivity and scalability. The application of these techniques to most ceramics has been challenging so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer. The LSD offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and enables the production of parts with physical and mechanical properties comparable to pressed or slip-casted parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles. Another technology, the Gas Flow Assisted Powder Deposition, can increase the stability of the powder bed and the packing density, even in extreme conditions such as in absence of gravitational forces.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer, which can be used for SLM or for 3DP. This technique offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and is capable of producing parts with physical and mechanical properties comparable to traditionally shaped parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
This third part of the review on defects as root cause of fatigue failure addresses cavities (pores, micro-shrinkages, unmelted regions), defective microstructures and microcracks as material defects and defects due to local damage during manufacturing, service and maintenance such as dents, scratches and localized corrosion. In addition, damage due to contact fatigue and the effect of surface roughness are discussed in the context of fatigue failure. Also addressed is the competition between different kinds of defects in controlling the initiation and early growth of fatigue cracks.
According to the definition of the ASM handbook [1,3], a defect is "an imperfection. that can be shown to cause failure by a quantitative analysis and that would not have occurred in the absence of the imperfection". The topic of the present three-part review is a discussion of defects which can cause failure in cyclically loaded structures. The features discussed comprise material defects such as non-metallic inclusions, pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches which have their origin in manufacturing, and defects such as surface damage due to scratches, impact events or contact fatigue as well as corrosion pits which arise in service. In this first part, the discussion is prefaced by an introduction to basic aspects which are essential for a deeper understanding of the characteristics and mechanisms how the defects influence fatigue crack initiation and propagation. These include the life cycle of a fatigue crack from initiation up to fracture, crack arrest, multiple crack initiation and coalescence, and the material and geometrical properties affecting these.
Defects as a root cause of fatigue failure of metallic components. II: Non-metallic inclusions
(2019)
This second part of the review on defects as root cause of fatigue failure comprises the origin, the nature and the effects of non-metallic inclusions. Topics addressed are the different kinds of inclusions formed during the manufacturing process, various types of mis-match causing local stresses and, as a consequence, fatigue crack initiation, and effects of characteristics such as size, morphology, localization, spatial distribution and orientation of the defects on the fatigue behavior. Methods for inclusion counting and sizing are discussed along with statistical aspects necessary to be considered when evaluating structural components.
Spherical mesoporous bioactive glasses in the silicon dioxide (SiO2)-phosphorus pentoxide (P2O5)–calcium oxide (CaO) system with a high specific surface area of up to 300m2/g and a medium pore radius of 4 nm were synthesized by using a simple one-pot surfactant-assisted sol–gel synthesis method followed by calcination at 500–700°C. The authors were able to control the particle properties by varying synthesis parameters to achieve microscale powders with spherical morphology and a particle size of around 5–10 mm by employing one structure-directing agent. Due to a high Calcium oxide content of 33·6mol% and a phosphorus pentoxide content of 4·0mol%, the powder showed very good bioactivity up to 7 d of immersion in simulated Body fluid. The resulting microspheres are promising materials for a variety of life science applications, as further processing – for example, granulation – is unnecessary. Microspheres can be applied as materials for powder-based additive manufacturing or in stable suspensions for drug release, in bone cements or fillers.
Quality Aspects of Additively Manufactured Medical Implants - Defect Detection in Lattice Parts
(2019)
Additive Manufacturing technologies are developing fast to enable a rapid and flexible production of parts. Tailoring products to individual needs is a big advantage of this technology, which makes it of special interest for the medical device industry and the direct manufacturing of final products. Due to the fast development, standards to assure reliability of the AM process and quality of the printed products are often lacking. The EU project Metrology for Additively Manufactured Medical Implants (MetAMMI) is aiming to fill this gap by investigating alternative and cost efficient non-destructive measurement methods.
Hydrogen gas diffusivity of fourteen glasses of the Na2O-Al2O3-SiO2 system are studied along the joins quartzalbite-jadeite-nepheline (Qz-Ab-Jd-Np, fully polymerized) and albite-sodium disilicate (Ab-Ds, depolymerized).
Density measurements show that ionic porosity decreases from 54.4% (Qz) to 51.5% (Np) and from 52.4% (Ab) to 50.2% (Ds). Hydrogen diffusivity D follows similar trends but at another scale. D at 523 K decreases from 4×10−12 to 3×10−14m2 s−1 (Qz-Np) and from 4×10−13 to 3×10−15m2 s−1 (Ab-Ds). Charge compensating Na+ acting as a filling agent in fully polymerized network structures leads to up to one order of Magnitude higher diffusivities as depolymerized glass structures of the same SiO2 content where Na+ takes the role of a
modifier ion. Temperature dependence of the diffusivity indicates that both the activation energy involved with the moving H2 molecule as well as the accessible volume in the structure contribute to this compositional trend.
The precise analysis of cation diffusion profiles through corrosion scales is an important aspect to evaluate corrosion phenomena under multicomponent chemical load, as during high‐temperature corrosion under deposits and salts. The present study shows a comprehensive analysis of cation diffusion profiles by electron microprobe analysis and microbeam X‐ray absorption near edge structure (µ‐XANES) spectroscopy in mixed oxide/sulfide scales grown on Fe–Cr model alloys after exposing them to 0.5% SO2. The results presented here correspond to depth‐dependent phase identification of oxides and sulfides in the corrosion scales by µ‐XANES and the description of oxidation‐state‐dependent diffusion profiles. Scales grown on low‐ and high‐alloyed materials show both a well‐pronounced diffusion profile with a high concentration of Fe3+ at the gas and a high concentration of Fe2+ at the alloy interface. The distribution of the cations within a close‐packed oxide lattice is strongly influencing the lattice diffusion phenomena due to their different oxidation states and therefore different crystal‐field preference energies. This issue is discussed based on the results obtained by µ‐XANES analysis.
Glass strength and fatigue is limited by surface cracks. As subcritical crack growth (SCCG) is governed by ambient humidity, stress corrosion at the crack tip is widely accepted to be the underlying mechanism. However, as water is known to have decisive effect on glass properties and can rapidly enter the crack tip near glass region, SCCG could be affected by such water related phenomena. We tried to mimic these effects studying water dissolution and speciation, mechanical properties, and SCCG in water-bearing glasses. For this purpose, glasses up to 8 wt% water have been prepared by means of high-pressure melting of glass powder - water mixtures.
As part of this effort, SCCG in dry and hydrous commercial micros¬cope slide glass (CW = 6 wt%) was studied in double cantilever beam (DCB) geometry and sub-Tg relaxation was measured by Dynamic Mechanical Analysis (DMA).
For SCCG in ambient air (24% r.h.), SCCG was promoted by the presence of 6wt% bulk water with respect to the dry glass. On the other hand, stress intensity values, KI, required to cause slow crack growth (v < 10-6 ms-1) resemble literature findings for float glass of similar composition in liquid water, which might represent the maximum possible promoting effect of ambient water on SCCG.
For SCCG in vacuum (10-3 mbar), dissolved bulk water causes even more pronounced effects. Most strikingly, it strongly decreases the slope of the log v(KI)-curve, which is a measure of dissipated energy during fracture. A strong increase of sub-Tg relaxation with increasing water content was confirmed by DMA. As a consequence, slow crack growth occurs at KI values as measured in the dry glass whereas fast crack growth occurs at much larger KI than that of the dry glass. Kinks and shoulders shown by the inert log v(KI)-curve indicate that bulk water does not simply affect bulk mechanical properties.
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.
Environmental conditions are known to influence sub-critical crack growth (SCCG) that starts from microscopic flaws at the glass surface, leading to stress corrosion phenomena at the crack tip. The processes at the crack tip are complex and water has been identified as a key component governing SCCG at low crack velocities (region I). In particular, the influence of humidity accelerating crack propagation is well studied for dry industrial soda-lime silicate glasses (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG in water-bearing glasses. For this purpose, water-bearing silicate glasses of up to 8 wt% total water were synthesized in an internally heated pressure vessel at 0.5 GPa and compared to dry glasses. SCCG was measured using the double cantilever beam technique. For dry glasses, three trends in the crack growth velocity versus stress intensity, KI, curve were found. The slope in region I, limited by environmental corrosion, increases in the order soda-lime silicate < sodium borosilicate < barium calcium silicate < sodium zinc silicate < sodium aluminosilicate 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 MPam1/2. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg relaxation 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 strain energy release rate and energy dissipation related to glass relaxation phenomena.
The freeze casting technique assisted with cryo thiol-ene photopolymerization is successfully employed for the fabrication of macroporous polymer-derived silicon oxycarbide with highly aligned porosity. It is demonstrated that the free radical initiated thiol-ene click reaction effectively cross-linked the vinyl-containing liquid polysiloxanes into infusible thermosets even at low temperatures. Furthermore, mixed solution- and suspension-based freeze casting is employed by adding silica nanopowders. SiOC/SiO2 foams with almost perfect cylindrical shapes are obtained, demonstrating that the presence of nano-SiO2 does not restrict the complete photoinduced cross-linking. The post-pyrolysis HF acid treatments of produced SiOC monoliths yields hierarchical porosities, with SiOC/SiO2 nanocomposites after etching demonstrating the highest specific surface area of 494 m2/g and pore sizes across the macro-, meso- and micropores ranges. The newly developed approach gives a versatile solution for the fabrication of bulk polymer-derived ceramics with controlled porosity.
Determination of Distribution Function used in MCS on Safety Analysis of Hydrogen Pressure Vessel
(2019)
The test data of static burst strength and load cycle strength of composite pressure vessels are often described by GAUSSian normal or WEIBULL distribution function to perform safety analyses. The goodness of assumed distribution function plays a significant role in the inferential statistics to predict the population properties by using limited test data. Often, GAUSSian and WEIBULL probability nets are empirical methods used to validate the distribution function; Anderson-Darling and Kolmogorov-Smirnov tests are the mostly favorable approaches for Goodness of Fit. However, the different approaches used to determine the parameters of distribution function lead mostly to different conclusions for safety assessments. In this study, six different methods are investigated to show the variations on the rates for accepting the composite pressure vessels according to GTR No. 13 life test procedure. The six methods are: a) Norm-Log based method, b) Least squares regression, c) Weighted least squares regression, d) A linear approach based on good linear unbiased estimators, e) Maximum likelihood estimation and f) The method of moments estimation. In addition, various approaches of ranking function are considered. In the study, Monte Carlo simulations are conducted to generate basic populations based on the distribution functions which are determined using different methods. Then the samples are extracted randomly from a population and evaluated to obtain acceptance rate. Here, the “populations” and “samples” are corresponding to the burst strength or load cycle strength of the pressure vessels made from composite material and a plastic liner (type 4) for the storage of hydrogen. To the end, the results are discussed, and the best reliable methods are proposed.
Determination of Distribution Function used in MCS on Safety Analysis of Hydrogen Pressure Vessel
(2019)
The test data of static burst strength and load cycle strength of composite pressure vessels are often described by GAUSSian normal or WEIBULL distribution function to perform safety analyses. The goodness of assumed distribution function plays a significant role in the inferential statistics to predict the population properties by using limited test data. Often, GAUSSian and WEIBULL probability nets are empirical methods used to validate the distribution function; Anderson-Darling and KolmogorovSmirnov tests are the mostly favorable approaches for Goodness of Fit. However, the different approaches used to determine the parameters of distribution function lead mostly to different conclusions for safety assessments. In this study, six different methods are investigated to show the variations on the rates for accepting the composite pressure vessels according to GTR No. 13 life test procedure. The six methods are: a) NormLog based method, b) Least squares regression, c) Weighted least squares regression, d) A linear approach based on good linear unbiased estimators, e) Maximum likelihood estimation and f) The method of moments estimation. In addition, various approaches of ranking function are considered. In the study, Monte Carlo simulations are conducted to generate basic populations based on the distribution functions which are determined using different methods. Then the samples are extracted randomly from a population and evaluated to obtain acceptance rate. Here, the “populations” and “samples” are corresponding to the burst strength or load cycle strength of the pressure vessels made from composite material and a plastic liner (type 4) for the storage of hydrogen. To the end, the results are discussed, and the best reliable methods are proposed.
Diese DIN SPEC legt ein Verfahren für die Prüfung von unverstärkten und partikel- und kurzfaserverstärkten Kunststoffen mittels Zug-Druck-Schubprüfung fest. Dieses Verfahren findet Anwendung zur Bestimmung der Schwingfestigkeit im Bereich von 103 bis 107 Schwingspielen und der Nachgiebigkeiten unter statischer Belastung sowie der Zugfestigkeit. Alle Beanspruchungen und berechneten Größen sind nennspannungs-basiert.
Grundsätzlich besteht bei Rohrprobekörpern auch die Möglichkeit eine Beanspruchung in Längs- und in Umfangsrichtung durch Innendruck zu erzeugen. Dies wird in dieser Spezifikation nicht berücksichtigt, um die Anwendung überschaubar zu halten. Bei Rohrproben mit ausgeprägter Querschnittsverkleinerung (z. B. der Prüfkörper Typ B), entsteht eine Umfangsspannung auch aufgrund einer Zugkraft (siehe Anhang C). Die Umfangsspannung muss dann mittels FEA lokal berechnet werden.
Das Verfahren gilt für rohrförmige Prüfkörper deren spezifische Form den Anforderungen der Werkstoff-prüfung und bei Kurzfaserverstärkung einer hohen Vorzugsausrichtung in Probenlängsrichtung genügen.
Diese DIN SPEC gilt nicht für endlosfaserverstärkte Kunststoffe. Wegen der vollkommen unterschiedlichen Fertigungstechnologien und der zu erwartenden hohen Prüflasten, sind hier die Anforderungen an die Prüfkörpergeometrie gesondert zu betrachten. Es wird nicht zielführend sein, beide Werkstoffklassen in einer Norm zu behandeln.
Der Fachbereich Mechanik der Polymerwerkstoffe befasst sich mit der Charakterisierung der mechanischen Eigenschaften und der Degradation von Polymeren und Faserverbundwerkstoffen, die in hochbeanspruchten, sicherheitsrelevanten Konstruktionen wie jenen des Flugzeugbaus, des Automobilbaus und der Windenergie-Industrie eingesetzt werden. Auch die Analyse der chemischen und physikalischen Eigenschaften von Polymeren zählt zu unserem Aufgabenbereich.
Das Spektrum reicht von der statischen Festigkeit über die Betriebsfestigkeit, die Messung bruchmechanischer und viskoelastischer Parameter bis hin zur Formulierung molekularer Schädigungsmechanismen.
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.
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.
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.
An effective method for evaluating the fatigue strength of thick unidirectional composite laminates of wing spar caps has been presented here. A typical width-tapered bending specimen has been developed for a four-point loading set up. Static and fatigue loading was performed at a load ratio R = -1. The complex stress state has been investigated numerically by finite element analysis. Finally, the concept is proven experimentally on specimens made of pultruded fibre rods.
The fatigue behavior of the continuously tapered width by water Jet cutting has been compared to discrete tapering via rod-drop. The new method enables a screening of material fatigue behavior caused by normal and shear loading.
Fiber reinforced polymers (FRPs) are a well established material in lightweight applications, e.g. in automotive, aerospace or wind energy. The FRP components are subjected to multiaxial mechanical as well as hygrothermal loads. Common operation temperatures are in the range of 213 K and 373 K (-60 °C and 100 °C) at a relative humidity of 10% to 90%. In spacecraft applications, the environmental conditions are even more extreme. However, the correlation between multiaxial mechanical loading and harsh environment conditions have to-date not been investigated in detail. The project aims to investigate the fatigue behavior of FRPs dependent on multiaxial mechanical loading, temperature, and humidity. Extensive experimental testing is performed on flat plate and cylindrical tube specimens, accompanied by numerical and analytical calculations.
Overview about the surface initiated microstructure formation in glass surfaces. Samples which are exposed to a temperature treatment, can develop a crystalline microstructure above Tg at the surface. These separated crystals can be preferably oriented towards the surface of the sample. First experiments about the origin of these orientation phenomenon as well as the potentially causing mechanisms are presented and discussed within the presentation.
Thermodynamic study of a refractory complex concentrated alloy (rCCA) using the CALPHAD method
(2019)
Multi-principal-element alloys (MPEAs), have recently come to the attention of the scientific community due to their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime. The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed.
Introduction/purpose:
Multi-principal-element alloys (MPEAs), also known as complex concentrated alloys (CCAs), have recently come to the attention of the scientific community due to some interesting and unexpected microstructures, and their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime.
Methods:
In this contribution, the CALPHAD method is used to calculate phase equilibria for the AlMo0.5NbTa0.5TiZr CCA in the presence and absence of oxygen. Equilibrium phase amount evolution with temperature and Scheil Model for solidification (e.g. Fig.1a and Fig.1b, respectively) are analyzed, which are obtained using the databases TCNI9 and TTNI7 and the Gibbs energy minimizer in the Thermo-Calc software.
Results:
The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed. Results obtained by both databases, as well as discrepancies between property phase and Scheil approaches are discussed on the base of experimental results.
Conclusions:
A modeling tool is used to support alloy characterization and development, providing also the possibility to feedback information to improve existing thermodynamic databases.
Konventionelle und innovative Hochtemperaturwerkstoffe sind im technischen Betrieb einer Vielzahl an Belastungen ausgesetzt. Neben mechanischen Beanspruchungen stellt die chemische Belastung durch das Vorhandensein von aggressiven und korrosiven Medien (SO2, CO2, O2, H2O…) bei hoher Temperatur einen Schlüsselfaktor dar, der die Langlebigkeit der Materialien im Einsatz beeinflusst. Neben konventionellen, mikroskopischen Analyseverfahren bieten röntgenbasierte Techniken Möglichkeiten, die Grenzflächenreaktionen zwischen dem Werkstoff und den Medien während der chemischen Belastung (in situ) zu untersuchen. Neuartige Einblicke in die zugrunde liegenden Prozesse der Schädigungsmechanismen werden anhand von klassischen ferritischen Legierungen beschrieben. Das Verständnis von Schlüsselfaktoren zur Induzierung eines Schutzmechanismus ist insbesondere für die Entwicklung von neuartigen Materialklassen wie Hochentropie- und chemisch komplexe Legierungen notwendig. Erste Einblicke in Schädigungsmechanismen durch Gaskorrosion dieser innovativen Materialsysteme werden vorgestellt.
Die Metal Magnetic Memory (MMM) Methode ist ein standardisiertes, zerstörungsfreies Prüfverfahren, das für die Detektion von lokal geschädigten Materialbereichen in ferromagnetischen Bauteilen oder Proben verwendet wird. Es basiert auf der Annahme lokaler magnetoelastischer Wechselwirkungen an Spannungskonzentrationsstellen, die schwache magnetische Streufelder an den geschädigten Prüfkörperoberflächen hervorrufen. Die MMM-Methode überträgt dabei die für einachsige und elastische Verformungen entwickelten magnetoelastischen Modellvorstellungen ohne weitere Anpassungen in den Schädigungskontext, der jedoch mehrachsige Beanspruchungen und elastisch-plastische Deformationsprozesse erwarten lässt. Das Ziel der Arbeit ist es daher, die gängigen MMM-Hypothesen zur Signalentstehung fach- und skalenübergreifend und unter stärkerer Berücksichtigung mechanischer und mikrostruktureller Aspekte zu überprüfen.
Zu diesem Zweck wurden zum einen gekerbte Flachzugproben aus einem unlegierten Baustahl inhomogen elastisch-plastisch verformt und die entstehenden magnetischen Streufelder an deren Oberflächen mit einem Drei-Achsen-GMR-Magnetometer detektiert. Die so ermittelten Magnetfeld-verteilungen wurden für unterschiedliche Verformungszustände ortsaufgelöst und richtungsabhängig mit gemessenen Dehnungsverteilungen (digitale Bildkorrelation) und mit simulierten Lastspannungs-verteilungen korreliert. Die eingeschnürten Probenbereiche wurden zusätzlich topographisch mittels Streifenlichtprojektion und Weißlichtinterferenzmikroskopie vermessen, um den Magnetisierungs-prozess ebenfalls vor dem Hintergrund geometrischer Effekte diskutieren zu können.
Um systematische, verformungsinduzierte Veränderungen der magnetischen Mikrostruktur (magnetischer Domänen) im polykristallinen, quasi-isotropen Material nachzuweisen, wurde zum anderen ein in dieser Arbeit entwickelter statistischer Ansatz der Domänenanalyse angewandt. Hierfür wurde das Material zunächst durch Härteeindrücke mehrachsig elastisch-plastisch verformt, und die verformten Probenbereiche wurden anschließend mit Hilfe der Bitterstreifentechnik hauptsächlich bei niedriger Vergrößerung lichtmikroskopisch untersucht. Die beobachteten makroskopischen Domänen-kontraste wurden über ein analytisches, kontaktmechanisches (ECM-) Modell und über Makro-Eigen-spannungsmessungen (energiedispersive Synchrotron-Beugungsuntersuchungen) charakteristischen Verformungszonen unter den Härteeindrücken zugeordnet.
Die Ergebnisse dieser Untersuchungen belegen, dass die Entstehung der Streufelder – entgegen bisheriger Annahmen – nicht allein auf mechanische Spannungs- und Verformungsgradienten im Material zurückzuführen, sondern auch topographisch bedingt ist. Die Vernachlässigung überlagerter geometrischer Effekte kann zu sicherheitsrelevanten Fehlinterpretationen der magnetischen Signale führen. Einachsige magnetoelastische Modellvorstellungen sollten zudem nicht ohne Anpassungen auf komplexe Beanspruchungen übertragen werden, da u. a. sowohl mechanische Größen (wie Spannungen oder Dehnungen) als auch mikrostrukturelle Parameter (wie z. B. Versetzungsdichten) bei komplexen Belastungen als ortsabhängige Variablen behandelt werden müssen. Die in dieser Arbeit beobachteten Domänenkontraste lassen sich zweifelsfrei charakteristischen Verformungszonen zuordnen, mikro-strukturell jedoch nicht allein mit anzunehmenden Gradienten der Versetzungsdichte erklären. Statt-dessen entstehen beispielsweise lokale Verformungstexturen, die zusätzliche magnetische Anisotropien bewirken könnten. Da bisher weder die makroskopischen noch die mikrostrukturellen Ursachen der Streufeldentstehung hinreichend verstanden sind, scheint die MMM-Methode für die quantitative Bewertung des Schädigungszustands derzeit ungeeignet.
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.
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.
Der Aufbau der Werkstoffe wird durch Merkmale wie Bindungsart, atomare Strukturen, Kristallstrukturen einschließlich ihrer Gitterbaufehler, Körner und Phasen bestimmt. Die Mikrostruktur (Gefüge) stellt den Verbund der Kristalle, Phasen und Gitterbaufehler auf mikroskopischer und nanoskopischer Skala dar. Die Grundlagen der Phasenumwandlungen werden behandelt und die Bedeutung von Diffusionsprozessen erläutert. Werkstoffe sind bedeutend für Kultur, Wirtschaft, Technik und Umwelt. Ihre Herstellung benötigt Ressourcen und Energie. Recycling ist eine Möglichkeit zur Erhöhung der Ressourcenproduktivität.
Materialprüfung
(2019)
Die Materialprüfung dient der Analyse der Eigenschaften, der Qualität und der Sicherheit vonMaterialien undWerkstoffen. Die häufigsten Verfahren umfassen die Analyse der chemischen Zusammensetzung und der Mikrostruktur sowie die Ermittlung von Werkstoffkennwerten. Dazu zählt auch die Bestimmung des Materialverhaltens unter verschiedenen Beanspruchungen bis hin zu komplexen Beanspruchungen. Die Verwendung von Referenzmaterialien, Referenzorganismen und Referenzverfahren dient der Zuverlässigkeit und Richtigkeit von Messungen, Prüfungen und Analysen.
Die warmfeste austenitische Gusseisenlegierung EN-GJSA-XNiSiCr35-5-2 (häufig auch als Ni-Resist D-5S bezeichnet) wurde hinsichtlich ihres mechanischen Verhal-tens bei hoher Temperatur charakterisiert. Dazu wurden (isotherme) niederzyklische (LCF-) und (nicht-isotherme) thermomechanische Ermüdungsversuche (TMF) zwischen Raumtemperatur und 900 °C durchgeführt. Diese Ergebnisse dienten (zu-sammen mit weiteren Versuchsdaten) der Kalibrierung werkstoffmechanischer Modelle. Bei den höchsten Prüftemperaturen wurde Schädigung in Form von Kriechen beobachtet und metallographisch dokumentiert.
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.
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 presentation.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
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.
Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography
(SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands.
Friction stir welding (FSW) of high-melting temperature alloys, such as steel and Inconel, requires tooling that can survive under the applied loads at the elevated temperatures. Tungsten-Rhenium (W-Re) alloys are a suitable candidate for this application; however, the costs typically associated with achieving the required densities and grain structure for the tooling are high due to the lengthy traditional processing required. Further costs are incurred in machining the starting bar stock to the final FSW tooling configuration. An alternate processing method is used in this study to shorten the fabrication time using direct current sintering which rapidly consolidates the starting powders at lower temperatures than used in traditional powder metallurgy. Although this process enables retention of the fine grain size, the sintering time is too short to form the desired single, solid phase. Therefore, the specimens were subjected to a post-consolidation heat treatment to fully solutionize the W matrix. Once the desired density and solid solution phase was verified in coupons, the final processing parameters were used to consolidate a net shape tool for FSW.