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Dry pressing of ceramic materials requires homogeneously soft granules with good flowability to allow rapid die filling and to avoid packing defects. Spray-drying granulation appears to be the best method for obtaining granules with high flowability in industrial scale. But, strength reducing internal microstructural defects caused by spray-dried granules with hollow and hard shells are often observed using nano and/or multi-component starting powders.
Using the example of a ZTA composite, the potential of slurry optimization, ultrasound atomization and infrared drying for better granule properties and compaction behavior were investigated. Starting granules produced in a conventional spray dryer (Niro, Denmark) with a two fluid nozzle showed typical defects like large central pores and dimples.
The early step of slurry preparation already possesses an essential optimization possibility in the form of stability adjustments. Granule compaction was clearly improved upon a specific reduction in slurry stability. The second optimization opportunity to improve the granule quality was the atomization step. Implementation of an ultrasound atomizing unit into the conventional spray dryer positively affected granule size distribution and therefor flowability and as well granule yield. But, a combination of both process optimizations delivered the best sinter bodies with highest density and strength due to further reduction in maximum size and fraction of pores.
As last step of a spray drying process, the drying is the focus of further investigations. A current setup implying a spray dryer prototype utilizes stacked infrared heater in a countercurrent setup delivering a further increase in granule yield and enduring spraying process stability.
Homogeneous introduction of organic additives is a key of ceramic powder processing. Addition of organics to ceramic slurries holds advantages compared to dry processing like organic content reduction and a more homogeneous additive distribution on the particle surface.
Investigations of the alumina slurries were primarily based on zeta potential measurements and sedimentation analysis by optical centrifugation. Both methods were combined to determine a suitable additive type, amount and composition, whereas the spray drying suitability has been ensured by viscosity measurements. Granules, yielded by spray drying of such ideally dispersed alumina slurries, are mostly hollow and possess a hard shell. Those granules cannot easily be processed and can only hardly be destroyed in the following shaping step, leading to sinter bodies with many defects and poor strength and density.
The precise slurry destabilization, carried out after ideally dispersing the ceramic powder, shows a strong influence on the drying behavior of the granules and hence on the granule properties. A promising degree of destabilization and partial flocculation was quantified by optical centrifugation and resulted in improved granule properties. Spray drying the destabilized alumina slurries yielded homogeneous “non-hollow” granules without the above mentioned hard shell. Sample bodies produced of these granules exhibited a reduction of defect size and number, leading to better results for sinter body density and strength.
The positive effect of the slurry destabilization has been further improved, by exchanging the atomizing unit from a two-fluid one to an ultrasound atomizer with only minor slurry adjustments necessary. The controlled destabilization and ultrasound atomization of the ceramic slurry show excellent transferability for zirconia and even ZTA (zirconia toughened alumina) composite materials.
Efficient studies of scarce or expensive materials require material saving processes. Therefore, a high yield concept for small batch preparation of ready-to-press powder is exemplarily presented for yttria stabilized nano-zirconia (d50 < 50 nm).
The concept involves small batch preparation in an ultrasound resonator, dispersant selection based on zeta potential measurements, evaluation of slurry stability using an analytical centrifuge, and preparation of ready-to-press powder by freeze drying.
Freeze drying offers key advantages. Process efficiency and high yield above 95 % are independent of sample size. The dried product does not require further mechanical treatment like milling or grinding. Side effects like migration of additives are avoided.
An optimized freeze drying process tolerates slurries with moderate stability. Thus, efforts for slurry development can be reduced. Generally, identifying a suitable dispersing agent requires only 3-5 zeta potential measurements. Slurry stability is rechecked using an analytical centrifuge, which also accounts for steric stabilization. An ultrasound resonator is used to disperse the powder without contamination, which becomes critical for small batches.
The described route is exemplarily presented for the development of an additive recipe for nano-sized zirconia powder, targeting for good pressing behavior and high green density. Therefore, a variety of binding and lubricating agents were tested.
Following the presented route, 80 g zirconia powder were sufficient to conduct a study including slurry development and five sample sets with varying composition, each set comprising five discs (d = 20 mm and h = 2 mm).
Metalle
(2019)
Dieses Standardwerk bietet eine Darstellung der Struktur und Eigenschaften der Metalle und ihrer Anwendungen als Werkstoffe. Im ersten, wissenschaftlichen Teil werden der atomare und mikroskopische Aufbau, die thermodynamischen und die grundlegenden physikalischen und mechanischen Eigenschaften der Metalle beschrieben sowie die Grundlagen der thermisch aktivierten Reaktionen und der Phasenumwandlungen. Die wichtigsten experimentellen Untersuchungsmethoden werden erläutert, wobei die mikroskopischen und Beugungsverfahren einen Schwerpunkt bilden.
Im zweiten, technischen Teil werden die Werkstoffgruppen der Metalle und ihre anwendungsbezogenen Eigenschaften behandelt. Dabei wird auf die zugrunde liegenden Legierungen und die Verfahren zur gezielten Einstellung ihrer Eigenschaften eingegangen. Schwerpunkte bei der Darstellung der Werkstoffe sind die Stähle, die teilchengehärteten Legierungen, die Magnetwerkstoffe und die pulvermetallurgisch hergestellten Werkstoffe. Außerdem werden die Oberflächeneigenschaften und die Verfahren zur Oberflächenbehandlung dargestellt.
The search for strong and tough oxide glasses is important for making safer, more environmentally friendly, thinner glass products. However, this task remains generally difficult due to the material’s inherent brittleness. In search for tougher glasses, fracture toughness (KIC) prediction models are helpful tools to screen for promising candidates.
In this work, a novel model to predict KIC via the fracture surface energy, γ, is presented. Our approach uses readily available crystallographic structure data of the glass’s isochemical crystal and tabled diatomic chemical bond energies, D0. The method assumes that γ of a glass equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were not only in excellent agreement with those calculated with a former well-working model, but also demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces.
Finally, the effectiveness of fracture toughness enhancement by chemical substitution is discussed based on our results and alternative toughening strategies will be suggested.
Enhancing the fracture toughness is still one of the major challenges in the field of oxide glasses. To screen different glass systems for promising candidates, a theoretical expression for the fracture surface energy, G, linked to the fracture toughness, KIc, is thus of interest. Extending our earlier work on nucleation and surface energies [1], we present a simple approach for predicting the fracture surface energy of oxide glasses, G using readily available crystallographic structure data and diatomic bond energies. The proposed method assumes that G of glass equals the surface fracture energy of the weakest fracture (cleavage) plane of the isochemical crystal. For non-isochemically crystallizing glasses, an average G is calculated from the weighed fracture energy data of the constitutional crystal phases according to Conradt [2]. Our predictions yield good agreement with the glass density- and chemical bond energy-based prediction model of Rouxel [3] and with experimentally obtained G values known at present.
[1] C. Tielemann, S. Reinsch, R. Maass, J. Deubener, R. Müller, J. Non-Cryst. Solids 2022, 14, 100093
[2] R. Conradt, J. Non-Cryst. Solids 2004, 345-346, 16
[3] R., Tanguy, Scripta Materialia 2017, 109-13, 137
The search for strong and tough oxide glasses is important for making safer, environment-friendlier, thinner glasses. As fracture toughness experiments in brittle materials are complicated and time-consuming , modelling glass fracture surface energy, G, and fracture toughness, KIc, is of interest for screening promising candidates. Inspired by Rouxel´s idea of preferred crack growth along cutting weakest bonds within a glass structure and a study by Tielemann et al. , which indicates a correlation between crystal fracture surface and glass-crys¬tal interfacial energies, we present a new approach for predicting G. Combining both ideas, we used diatomic bond energies and readily available crystallographic structure data for estimating G. The proposed method assumes that G of the glass equals the surface fracture energy of the cleavage plane in its respective isochemical crystal. We calculated G- values for more than 25 iso-chemical silicate systems and compared them to calculated values from Rouxel’s widely used procedure, which is well working and based on glass densities and chemical bond energies. Not only does our model yields good agreement with [3], but it also enables an estimation for glasses with unknown density and can therefore contribute to broaden the data basis for glass property modelling tools. Most interestingly, however, this agreement indicates an interesting similarity between cleavage planes in a crystal and its corresponding glass state in terms of fracture processes.
A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation.
Additive manufacturing of alkali-activated materials currently attracts a lot of attention, because of the possibility to produce customized high-performance elements for a range of applications, potentially being more resource-efficient than conventionally produced parts. Here, we describe a new additive manufacturing process for alkali-activated materials that is based on selective laser-heating of lithium aluminate/microsilica slurries. The new process-material combination allows to manufacture elements with complex geometries at high building rates and high accuracy. The process is versatile and transferrable to structures of sizes differing by orders of magnitude. The mechanical strength of the obtained materials was in the range of values reported for conventional metakaolin-based geopolymers, and superior to what has been hitherto reported for alkali-activated materials produced by additive manufacturing. This mechanical performance was obtained despite the fact that the degree of reaction of the lithium aluminate and the microsilica was low, suggesting that significant reactions took place only at the surface of the microsilica particles.
For the additive manufacturing of large components typically powder-based methods are used. A powder is deposited layer by layer by means of a recoater, then, the component structure is printed into each individual layer. We introduce here the new method of local laser drying, which is a suspension-based method specially developed for the manufacturing of large voluminous ceramic parts. The structure information is directly written into the freshly deposited layer of suspension by laser drying. Initially, the technology was developed for ceramic suspensions, however, first experiments with geopolymers reveal a high potential for this class of materials. Metakaolin, fly ash and lithium aluminate-based one-part geopolymers were used in first experiments. The local annealing of the geopolymer slurry results in a drying and crosslinking reaction and, thus, in a local consolidation of the material. First parts made are introduced and their properties are discussed.
Additive manufacturing is well established for plastics and metals, and it gets more and more implemented in a variety of industrial processes. Beside these well-established material platforms, additive manufacturing processes are highly interesting for ceramics, especially regarding resource conservation and for the production of complex three-dimensional shapes and structures with specific feature sizes in the µm and mm range with high accuracy. The usage of ceramics in 3D printing is, however, just at the beginning of a technical implementation in a continuously and fast rising field of research and development. The flexible fabrication of highly complex and precise 3D structures by means of light-induced photopolymerization that are difficult to realize using traditional ceramic fabrication methods such as casting and machining is of high importance. Generally, slurry-based ceramic 3D printing technologies involve liquid or semi-liquid polymeric systems dispersed with ceramic particles as feedstock (inks or pastes), depending on the solid loading and viscosity of the system. This paper includes all types of photo-curable polymer-ceramic-mixtures (feedstock), while demonstrating our own work on 3D printed alumina toughened zirconia based ceramic slurries with light induced polymerization on the basis of two-photon absorption (TPA) for the first time. As a proven exemplary on cuboids with varying edge length and double pyramids in the µm-range we state that real 3D micro-stereolithographic fabrication of ceramic products will be generally possible in the near future by means of TPA. This technology enables the fabrication of 3D structures with high accuracy in comparison to ceramic technologies that apply single-photon excitation. In sum, our work is intended to contribute to the fundamental development of this technology for the representation of oxide-ceramic components (proof-of-principle) and helps to exploit the high potential of additive processes in the field of bio-ceramics in the medium to long-term future.
High conductive silver-glass-metallization-pastes are key components in photovoltaics and advanced microelectronics. However, the underlying mechanisms of liquid phase sintering as silver dissolution, diffusion and reprecipitation are poorly understood so far.
In the current work, the influence of different network modifier in alkali-zinc-borate paste-glasses on liquid phase sintering of silver-glass-composites was studied. Therefore, silver-glass-composites containing 30 vol% glass were prepared, using low melting X2O-ZnO-B2O3 glasses with X = Na, Li, and Rb (NZB, LZB, and RZB). Glass transition temperature, viscosity, glass-silver wetting, crystallization and sintering behavior was studied by means of thermal analysis, dilatometry, heating microscopy and microscopy.
Similar glass transition temperatures of 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB) were found by means of thermal analysis for glasses under study. Also, all glasses have a similar crystallization onset at about 550 °C, even though exhibiting with a different degree of crystallization.
Despite these similarities, however, the sintering behavior, measured in terms of area shrinkage, significantly differs for the composites. This finding indicates a different degree of silver dissolution. Assuming that dissolved silver reduces the viscosity, this effect could explain why glass crystallization starts at lower temperature in the composites. For example, the crystallization peak of LZB at 629 °C measured for pure glass powder compacts was decreased to 586 °C for the composite. Confirmatively, microstructure analyses indicate different degrees of silver dissolution, as e.g. revealed by different amount of silver precipitates within the residual glass phase, and reprecipitation. Best silver dissolution appeared for the RZB glass. Nevertheless, the final densification of RZB was retarded probably due to swelling and crystallization.
Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices.
Low melting Li2O-PbO-B2O3, Me2O-ZnO-B2O3, Me = Li, Na, K, Rb and CaO-ZnO-B2O3 glasses were studied with Raman and infrared spectroscopies to advance the structural understanding of zinc borate glasses as potential candidates for substitution of lead containing glasses. Although the effect of type of alkali ions on the number (N4) of fourfold coordinated boron (B4) in the glasses is small, the alkali ions direct the type of borate groups, i.e., pentaborate in lithium, sodium, and calcium zinc borate glasses, as well as diborate in potassium and rubidium containing ones. Both groups were simultaneously found in Li2O-PbO-B2O3. Alkali ions are mainly responsible for the formation of B4-units and metaborate. Zinc ions favorably compensate non-bridging oxygen and partially form ZnO4. With decreasing N4 and field strength of the alkali ions the atomic packing density, glass transition temper ature and Young’s Modulus also decrease. The coefficient of thermal expansion increases with decreasing N4.
Since decades electric contacts based on silver metallization pastes are key components of photovoltaics and advanced microelectronics. For the metallization of commercial Si solar cells, high conductive silver glass pastes are cost effectively applicated by screen printing. Nevertheless, silver pastes are still one of the most crucial and expensive none Si materials in solar cells. Ever shorter time to market as well as increasing demands on reduced Ag consumption and line width require the targeted development of silver-glass-pastes with increased sinter ability and electrical conductivity. As a main difficulty, however, the liquid phase sintering of silver glass pastes is poorly understood so far.
In the present study, the influence of different network modifier in alkali-zinc-borate paste glasses on liquid phase sintering of silver-glass-pastes was investigated. Low melting X2O-ZnO-B2O3 glasses with X = Na, Li and Rb (abbr. LZB, NZB, and RZB) were utilized to prepare silver-glass-composites containing 30 %Vol glass. Shrinkage behavior of the silver-glass-composites compared with that of pure silver and pure glass powder compacts was studied with heating microscopy. The powder compacts were uniaxially pressed and heated at 5 K/min to the glass softening temperature. Glass transformation temperature and viscosity of the glasses were respectively measured with dilatometry and rotational viscometry. The thermal behavior of the pure glasses was analyzed with thermal analysis. Additionally, the contact angle of glass on pure silver foil was determined by means of heating microscopy between room temperature and 830 °C.
Thermal analysis of the alkali-zinc-borate-glasses under study has shown transformation temperatures between 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB). For all glasses crystallization was found to start approximately at about 550 °C. However, different peak areas hint on a different degree of crystallization. Conformingly, the sintering behavior, measured in terms of area shrinkage, significantly differed for the silver-pastes under study. For silver-pastes with NZB or LZB-glass, sintering starts at 464 °C for NZB Ag pastes and at 451 °C for LZB Ag pastes and ends at 597 °C for NZB Ag paste and at 594 °C for LZB Ag paste. The sintering of the RZB Ag paste proceeds between 426 °C and 703 °C. The final densification was retarded possibly due to crystallization or swelling. The low sinter onset at 426 °C seems to correlate with the good wetting behavior of the RZB glass. Thus, the lowest apparent contact angle between the just densified powder compact sintered at a silver substrate was found for this glass. Moreover, microstructure analyses of the various composites indicate differences in silver dissolution and reprecipitation.
Low melting zinc borate glasses awake interest to replace lead borate glasses in the silver metallization pastes for solar cells or microelectronics. In the current study, characteristic properties of alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) were compared to an earth alkali zinc borate glass (CaO-ZnO-B2O3). Additionally, zinc oxide is partially substituted by lead oxide or cooper oxide in the borate glasses (Li2O-PbO-B2O3, Na2O ZnO CuO-B2O3). The alkali zinc borate glasses indicate less differences in Raman spectra, and thus in structural properties, in comparison to the Ca and Pb ions influence. LPbB (Tg = 401 °C) has a lower viscosity than LZB (Tg = 468 °C) and CaZB has the highest glass transition temperature (Tg = 580 °C). The Angell plot for the alkali zinc borate glasses shows a high fragility m = 80. Besides Tg, the density measured by means of the Archimedean principle, molar volume, and coefficient of thermal expansion (CTE) of the glasses were investigated. Trends could be found according to alkali ions or intermediate oxides. The density increases with decreasing alkali ion size from KZB (2.632 g/cm3) to LZB (2.829 g/cm3) and increases from LZB to LPbB (3.764 g/cm3). CTE ranges between 7.09 10-6 K-1 for CaZB and 11.5 10 6 K 1 for KZB and RZB. The differential thermal analysis (DTA) and X ray diffraction (XRD) indicate crystallization of various crystalline phases during heating with 5 K/min in most cases.
Network modifier ions can decisively influence properties and structure of low melting alkali-zinc-borate glasses and thus cause complex effects on the liquid phase sintering of silver-glass metallization pastes. This effect was studied for X2O-ZnO-B2O3 (X = Li, Na, Rb) glasses for silver-glass metallization pastes. Viscosity and the glass transition temperature, Tg, were measured with rotational viscometry and dilatometry. Dried model pastes with 30 vol% LZB, NZB or RZB glass were prepared for sintering studies by means of heating microscopy measuring the silhouette area shrinkage of uniaxially pressed powder compacts during heating at 5 K/min. For comparison, the silhouette area shrinkage of pure glass and silver powder compacts were determined. Glass-silver wetting was investigated during heating of bulk glass cylinders placed on silver substrates. Glass RZB turned out to have the lowest viscosity among the glasses under study. Its glass transformation temperature, Tg, was found at 444 °C and it caused the lowest sintering onset for its glass and paste powder compacts. Slightly increased values of Tg were found for NZB and LZB (468 °C and 466 °C, respectively) and a slightly retarded sintering was found for both paste powder compacts. These results indicate that liquid phase sintering of silver-glass pastes under air atmosphere is mainly influenced by glass viscosity.
Liquid phase sintering of glass bearing silver pastes used in photovoltaics and microelectronics is poorly understood. In particular, the role of different network modifiers acting in the glass component and the question of the most suitable atmospheric oxygen level during sintering are still under considerable debate. To tackle these issues, low-melting and lead-free X2O-ZnO-B2O3 glasses with X = Li, Na, K and Rb (LZB, NZB, KZB and RZB) were prepared. Infrared spectroscopy showed that the glass structure was similar to each other, while an increase of tetrahedrally coordinated boron with increasing field strength of the alkali was evident. In turn, the glass transition temperature (from differential thermal analysis) increased in the order: RZB (449 °C) < KZB (460 °C) < NZB (465 °C) < LZB (472 °C). Powders of each glass were mixed with organics to receive silver-glass-pastes containing 30 vol% glass and these were subjected to heating microscopy in air. Although similar onset temperatures of sintering were recorded for Ag-NZB and Ag-LZB glass pastes, and for Ag-RZB paste and KZB-Ag-paste, respectively, differences in the crystallization behavior and final densification were observed between the former and the latter group. These were translated in terms of differences in silver dissolution and reprecipitation among the two groups. Further, running the experiments in nitrogen gas showed that sintering of all pastes was considerably hampered. The slow-down of the sinter kinetics was found to be in line with the assumed lower oxidation and dissolution of silver ions into the glass-forming liquid.
Melting of Na2CO3-ZnO-B2O3 batches containing up to 16.8 wt% AgNO3 (5 mol% Ag2O in the target glass composition) was observed in situ by means of hot stage microscopy. In all batches metallic silver precipitation took place as most of the silver nitrate was reduced to metallic silver before Ag+ ions could be dissolved in the evolving borate melts. In turn, only traces of Ag+ (<300 ppmw) were dissolved in the sodium zinc borate glass melts under study. It is assumed that the oxidation to Ag+ was limited due to poor availability of reducible oxygen in the glass melts and presence of Na2O being a stronger base than Ag2O. Thus, the precipitated metallic silver formed droplets of different sizes. The larger droplets (d > 20 µm) were already settled at the bottom of the container and remained constant in size upon dwelling for 1 h at 1050 °C of about one hour and the subsequent cooling (45 K/min) to room temperature, whereas the smaller droplets (d < 20 µm) were mobile in the borate melt due to Marangoni and Stokes motion. For the latter droplets, coalescence was observed in situ. A growth of larger droplets at the expense of smaller ones, i.e., Ostwald ripening was also expected but could not be studied with the used experimental equipment.
Silber-Glas Wechselwirkungen spielen eine wichtige Rolle zum Beispiel in Glas-haltigen Silberpasten, die in der Photovoltaik oder Mikroelektronik verwendet werden. Um ein besseres Verständnis der Vorgänge zu erhalten, werden niedrig-schmelzende, bleifreie X2O ZnO B2O3 Gläser (X = Li, Na, K und Rb, Abk.: LZB, NZB, KZB and RZB) zur Untersuchung der Pasten verwendet.
Raman und Infrarot Spektroskopie zeigen, dass die Glasstruktur weitgehend vergleichbar ist, aber Unterschiede in der Bildung von Pentaboratgruppen in LZB und NZB oder Diboratgruppen in KZB und RZB auftreten. Die Anzahl an vierfach koordinierten Bor-Ionen (N4) sinkt mit zunehmendem Alkaliionenradius. Die Verringerung von N4 führt zu einer niedrigeren Glasübergangstemperatur in der Reihe LZB (472 °C) < NZB (465 °C) < KZB (460 °C) < RZB (449 °C).
Zur Herstellung der Pasten wurde kommerzielles Silber-Pulver mit 30 Vol.-% Glas und Organik gemischt. Das Sinterverhalten der gepressten Pulver wurde mittels Erhitzungsmikrospie untersucht. Der Sinterbeginn der Pasten ist vergleichbar und korrespondiert mit den geringen Unterschieden der Viskosität bei vergleichbarer Partikelgröße der Gläser. In den Ag-KZB- und Ag-RZB-Pasten ist die Schwindung durch die stärker einsetzende Kristallisation im Vergleich zu LZB und NZB verzögert.
High conductive silver metallization pastes are key components in advanced electronics and photovoltaics. Increasing demands on efficiency, miniaturization and ever shorter time-to-market require tailored glass-silver-pastes. In these pastes, low-melting glasses act as a sintering aid achieving better sintering, adhesion and contact formation for solar cells. Yet, the related liquid phase sintering of silver-glass-composites and the underlying mechanism of silver dissolution, transport and reprecipitation are rarely investigated. In this study, systematically varied low melting alkaline zinc borate, alkaline earth borate, and Pb- and Bi-glasses are investigated. Glass transition and crystallization are studied with dilatometry, DTA and XRD. Sintering of the pure glasses, pure silver and silver-glass-composites is analyzed with Hot Stage Microscopy, optical and electron microscopy. Since oxygen dissolved in silver powders can affect the silver dissolution as silver oxide in the matrix oxide glasses, the O2-content of silver powders is determined by Vacuum Hot Extraction. The glass transition temperature of the glasses under study varies between 370 °C and 590 °C whereas the sinter onset largely ranges between 400 °C and 600 °C. On the other hand, it scattered between 200 °C and 450 °C for selected commercial Ag-powders of different particle size and morphology.
In many late-breaking research fields as in photovoltaics, microelectronics, nuclear waste glasses or at least mirror glasses silver diffusion in glasses is relevant to the issues of high-level functionality and recycling. The present study is focused on silver diffusion in innovative, low-melting alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) potentially usable for silver metallization-pastes in solar cells. The glasses were coated with a thin metallic silver layer and heat treatments in air and nitrogen close to Tg at 470 °C for 2 h were performed. After heat treatment under air and nitrogen atmospheres the coating thickness, measured by a white light interferometer, was about 1.8 µm thick. Silver depth profiles determined by means of secondary neutral mass spectrometry (SNMS) indicate the fastest silver diffusion to a depth of 3.5 µm for Li2O-ZnO-B2O3 (LZB) glass. Nevertheless, the influence of the different alkali ions on the silver diffusion is small. The oxygen availability determines the silver diffusion into the glasses. The oxygen promotes the oxidation of the silver layer enabling Ag+ to diffuse into the glass and to precipitate as Ag0. Both species were detected by x-ray absorption spectroscopy (XAS). The precipitated metallic silver particles in Na2O-ZnO-B2O3 (NZB) glass have a mean size of 5.9 nm ± 1.2 nm diameter, which was determined using transmission electron microscopy (TEM). Phase separation in zinc-rich and zinc-poor phases with a mean diameter of 75 nm ± 20 nm occurred in NZB glass after heat treatment. Ion diffusion of the glasses into the silver layer was suggested by EDX-line scans.
Substitution of lead oxide in low-melting glasses, e.g., for application in silver metallization pastes, is a current research goal. This work is focused on the investigation of silver diffusion in alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb). In addition, the redox state of silver (Ag) and thus the type of diffusing silver species were studied. For this purpose, a metallic silver coating was applied on glass cubes by means of sputtering. Heat treatment of the samples was performed close to the glass transition temperatures at 470 °C for 2 h under air and nitrogen atmosphere. Coating thickness was 1.8 µm after heat treatment, measured by a white light interferometer.
Silver diffusion profiles were measured by means of secondary neutral mass spectrometry. The silver diffusion coefficients are in the range of ~10-14 cm2/s and indicate no significant differences depending on the type of alkali ions in the glass. Dissolved Ag+-ions and [Agm]n+-clusters in the glasses were differentiated using fluorescence spectroscopy.
Precipitated metallic silver particles in the sodium containing glass were observed by means of transmission electron microcopy. Their mean particle diameter was ~6 nm.
Die Abbildung von Bruchflächen im Rasterelektronenmikroskop (REM) liefert hochaufgelöste Bilddaten, die für die mikrofraktografische Bewertung von Bruchmechanismen unerlässlich sind. Die Ermittlung von Bruchmechanismen ist oft ein wichtiger Teil von Schadensanalysen zur Ermittlung der Bruchursache. Durch den Abbildungsprozess im REM gehen räumliche Informationen im Normalfall größtenteils verloren und können daher nicht zur Präzisierung des Bruchmechanismus herangezogen werden.
Um räumliche Informationen von Probenoberflächen im REM zu erfassen, gibt es verschiedene Methoden. Die für die Ermittlung der 3D-Topografie bereits länger eingeführten Verfahren mittels Proben- oder Strahlkippung können die Berechnung des Oberflächenmodells erst nach der seriellen Aufnahme mehrerer Bilder vornehmen. Mit der Verwendung eines segmentierten Rückstreudetektors ist dagegen die Erzeugung eines 3D-Oberflächenmodells während der Bildaufnahme praktisch in Echtzeit möglich. Die Probentopografie wird gleichzeitig mit dem Bildeinzug dargestellt und gespeichert.
Die Abbildung von Bruchflächen im REM liefert hochaufgelöste Bilddaten, die für die mikrofraktografische Bewertung von Bruchmechanismen unerlässlich sind. Durch den Abbildungsprozess im REM gehen räumliche Informationen im Normalfall größtenteils verloren. Mit der Verwendung eines segmentierten Rückstreudetektors ist dagegen die Erzeugung eines 3D-Oberflächenmodells während der Bildaufnahme praktisch in Echtzeit möglich. Die hier beschriebene Untersuchung soll die Anwendbarkeit des Verfahrens auf Bruchflächen zeigen. Zukünftig können Topografiedaten dazu beitragen, Bruchflächen besser zu interpretieren.
The aim of a fractographic investigation is the evaluation of macroscopic and microscopic fracture surface characteristics and, as a result, the determination of the fracture mechanism of a component from a failure case. The basis for such evaluations of fracture characteristics comes from actual comparative mechanical testing and from the literature. A fractographic analysis can be very complex and, in any case, requires considerable experience.
Machine learning methods enables the quantitative determination of fracture characteristics and fracture mechanisms utilizing digitized expert knowledge [1]. Although the application of SE images provides promising results, additional information is required to obtain reliable solutions. As expected, BSE and 3D information helps to improve the classification (Fig. 1). But only a fast, widely integrated, and automated topography measurement can provide the required amount of referenced surface data for the application of machine learning methods.
To fulfil these requirements, topographical data are obtained from a BSE detector with four symmetric segments (4Q-BSE) using shape-from-shading technology [2]. Surface height calculation is performed live during image acquisition and provides immediate feedback in three dimensions. All available signals (SE, BSE and more if applicable) are recorded simultaneously together with the surface topography and stored in a multichannel data file. This guaranties the same geometrical reference for all data, which is required for further analysis (Fig. 2).
When applying machine learning methods to topographic data together with SEM images, topographic information must be provided as depth image. Consequently, a unique height scale is required for all applied data with different magnifications. This requires a calibrated height measurement, which is ensured with the integrated 3D calibration of the topographic acquisition and a dedicated calibration sample. Thus, a large number of data sets from different fracture samples was generated and used as training data for machine learning.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced. Finally, the extended research data management in this project is highlighted and its advantages for sustainable use in material science and engineering applications are shown.
In this study, the influence of aging and mean stress on fatigue of the aluminium-alloy EN AW-2618A is investigated. Therefore axial fatigue tests are carried out on smooth specimens. The experiments show that the fatigue life decreases with increasing mean stress. Furthermore, the tests with the overaged specimens demonstrate that the number of cycles to failure is decreasing with increasing aging time.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced.
The presentation shows the results of high cycle fatigue (HCF) tests from the aluminium alloy EN AW-2618A. This study investigates the mean stress influence in the T61 condition and the effect of overaging. For this purpose, axial HCF tests were carried out at room temperature and different stress ratios (R=-1, R=0.1) as well as with overaged conditions (T61+10h@230°C, T61+1000h@230°C). After completion of the tests, the fracture surfaces were examined to study crack initiation.
Regarding feedstocks for the additive manufacturing (AM) of ceramics, two features are most critical in classical powder based AM processes: a high particle packing density (typically >50% TD) must be achieved with very fine particles (typically submicron) in order to ensure sufficient sintering activity. Three innovative approaches will be introduced to overcome this problem:
1. Layer wise slurry deposition: The use of water based ceramic slurries as feedstock for the additive manufacture of ceramics has many advantages which are not fully exploit yet. In the layerwise slurry deposition (LSD) process a slurry with no or low organic content is repetitively spread as thin layers on each other by means of a doctor blade. During the deposition, the ceramic particles settle on the previously deposited and dried material to form thin layers with a high packing density (55-60%). The LSD therefore shares aspects both of tape casting and slip casting. The LSD differentiates from the classical powder-based AM layer deposition, which typically achieves with a flowable coarse grained powder a low packing density (35-50%) only, consequently hindering the ability of sintering ceramic parts to full density. The LSD is coupled with the principles of selective laser sintering (SLS) or binder jetting, to generate novel processes which take advantage of the possibility of achieving a highly dense powder-bed.
2. Laser induced slip casting: Contrary to the LSD process, which requires drying of each individual layer, the direct interaction of ceramic slurries with intense laser radiation, for the laser induced slip casting (LIS), is a promising approach for the additive manufacture of voluminous parts.
3. Gas flow assisted powder deposition: By the application of a vacuum pump a gas flow is realized throughout the powder bed. This gas flow stabilizes the powder bed and results into an enhanced flowability and packing density of the powder during layer deposition.
The presentation will provide a detailed discussion of potentialities and issues connected to the mentioned technologies and will describe the most recent developments in their application to technical ceramics.
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with laser light into the volume of a ceramic powder compound its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP) for the additive manufacture of filigree structures within the volume of ceramic slurries.
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with laser light into the volume of a ceramic powder compound its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP) for the additive manufacture of filigree structures within the volume of ceramic slurries.
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with light into the volume of a ceramic powder compound, its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP), and other volumetric methods for the additive manufacture of filigree structures within the volume of ceramic slurries.
At the Workshop "Neutron and Synchrotron Monitoring in Aerospace Advanced Manufacturing" at the Institute of Materials Physics in Space, German Aerospace Center (DLR) in Cologne, we presented on the opportunities and our experiences of using a powder based additive manufacturing process for in-space manufacturing applications in microgravity.
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.
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.
The Binder Jetting BJ process is one of the most versatile additive manufacturing technologies in use. In this process a binder is locally jetted into a powder bed for the consolidation of a 3D structure, layer by layer. Basically, all materials which can be provided as a flowable powder and, thus, spreadable to a thin layer, can be processed. Metals, ceramics and polymers are processable, but also materials from nature, such as sand, wood sawdust and insect frass. Moreover, the BJ technology is adapted to large building volumes of some cubic meters easily. Besides these striking advantages, the manufacture of ceramic parts by BJ is still challenging, as the packing density of the powder bed is generally too low and the particle size of a flowable powder too large for a successful densification of printed parts in a subsequent sintering step to an advanced ceramic product. After an introduction of binder jetting in general and highlighting some examples, strategies for obtaining dense ceramic parts by BJ will be introduced.
In order to be able to manipulate ceramic powder compacts and ceramic suspensions (slurries) within their volume with light, a minimum transparency of the materials is required. Compared to polymers and metals, ceramic materials are characterized by the fact that they have a wide electronic band gap and therefore a wide optical window of transparency. The optical window generally ranges from less than 0.3 µm to 5 µm wavelength. In order to focus light into the volume of a ceramic powder compact, its light scattering properties must therefore be tailored. In this study, we present the physical background and material development strategies for the application of two-photon polymerization (2PP) and selective volumetric sintering for the additive manufacturing of structures in the volume of ceramic slips and green compacts.
Charakterisierung von Hochtemperaturwerkstoffen durch Zug- und Ermüdungsversuche an Kleinproben
(2019)
Die Verwendung von miniaturisierten Probengeometrien in der mechanischen Prüfung ermöglicht die Entnahme des Probenmaterials direkt aus kritischen Bereichen wie Fügeverbindungen und ermöglicht die Prüfung von kleinen Bauteilen wie additiv gefertigten Strukturen. In der vorliegenden Arbeit werden exemplarisch die Ergebnisse von vergleichenden Zug- und niederzyklischen Schwing-versuchen (LCF) an dem austenitischen Stahl AISI 316L und der Nickelbasislegierung IN718 vorgestellt. Die Prüfergebnisse der Kleinproben aus AISI 316L weisen die charakteristischen Eigenschaften des Werkstoffs auf, und die Analyse der Zug- und Ermüdungsdaten führt zu Werten, die den Literaturdaten weitgehend entsprechen. Der direkte Vergleich mit Standardprobendaten zeigt jedoch systematische Abweichungen bei Zugfestigkeit, Dehngrenze und Gleichmaßdehnung, die in diesem Beitrag diskutiert werden.
Charakterisierung von Hochtemperaturwerkstoffen durch Zug- und Ermüdungsversuche an Kleinproben
(2019)
Die Verwendung von miniaturisierten Probengeometrien in der mechanischen Prüfung ermöglicht die Entnahme des Probenmaterials direkt aus kritischen Bereichen wie Fügeverbindungen und ermöglicht die Prüfung von kleinen Bauteilen wie additiv gefertigten Strukturen. In der vorliegenden Arbeit werden exemplarisch die Ergebnisse von vergleichenden Zug- und niederzyklischen Schwingversuchen (LCF) an dem austenitischen Stahl AISI 316L und der Nickelbasislegierung IN718 vorgestellt. Die Prüfergebnisse der Kleinproben aus AISI 316L weisen die charakteristischen Eigenschaften des Werkstoffs auf, und die Analyse der Zug- und Ermüdungsdaten führt zu Werten, die den Literaturdaten weitgehend entsprechen. Der direkte Vergleich mit Standardprobendaten zeigt jedoch systematische Abweichungen bei Zugfestigkeit, Dehngrenze und Gleichmaßdehnung, die in diesem Beitrag diskutiert werden.
In Germany spent nuclear fuel and high level radioactive waste is stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. The used metal seals consist of three components as can be seen in the cross-sectional view in Figure 1. The innermost part is a helical spring that is surrounded by an inner jacket made of stainless steel. The outer jacket that is made of a softer material which in case of assembly in the aforementioned storage containers is silver or aluminum (i.e. Al 99.5). During application the seal is compressed and due to the restoring force of the helical spring, the outer jacket is plastically deformed and adapts to the sealing surface. Hence, leakage paths are closed and the sealing function is generated. In Germany the above-mentioned containers are licensed for up to 40 years of interim storage, which in case extended storage becomes necessary before a final repository is available will have to be extended to even longer periods. Therefore, the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads as well.
At Bundesanstalt für Materialforschung und –prüfung (BAM) long-term investigations are being conducted in which seals are assembled in test flanges and aged at temperatures ranging from room temperature to 150°C for accelerated aging. The aged seals are tested semi-annually (after the first 6 months in which the seals are tested more frequently) regarding the sealing performance, the remaining seal force, and the useable resilience upon decompression. Results of these investigations have been published over the past years (e.g. Grelle, Wolff, Probst, Jaunich, & Völzke, 2017; Völzke, Wolff, Probst, Nagelschmidt, & Schulz, 2014). It was found that the seal force and the useable resilience decrease with time and temperature, which is in agreement with the result of other studies (Sassoulas et al., 2006; Wataru et al., 2016) as well. Geometry change of the outer jacket has been identified as the main reason for this seal behavior. At the prevailing operating temperatures and stresses the aluminum is subjected to creep deformation leading to a thinning of the outer jacket. Since the seal groove depth remains unchanged the helical spring expands, which in turn leads to a decrease of the generated spring and seal force.
Although the main reason for the change of seal parameters over time and temperature is known, a detailed characterization of the seal behavior and a reliable prediction of the parameter development for aging times that exceed the experimental time frame have not been possible, yet.
For deeper understanding of the aging processes, an Investigation program, which is covered in this contribution, is conducted at Bundesanstalt für Materialforschung und –prüfung (BAM) that focusses on the behavior of the aluminum jacket and its influence on the long-term sealing performance. The program investigates properties of material samples as well as the behavior of the seal as a component.
Original sheet material of the same aluminum that is used for manufacturing of the seals is investigated in compression creep tests. For this, a DMA (dynamic mechanical analysis) machine is employed (here used for static tests) that allows for a measurement of the specimens deformation under forces of up to 500 N. The advantage of this method is that the original material can be tested in the same shape as used for the seals which is 0.5 mm thick sheet material. For investigation of tensile creep standard specimens are used, that were machined from surrogate material of the same composition and annealing condition.
Furthermore, aluminum seals that are cut into smaller segments are assembled in flanges and placed in heating chambers at temperatures ranging from 23°C to 150°C. After different periods of time from 3 days to 300 days the segments are taken out of the flanges and are investigated, thus giving information on different states of aging. Measurements of the development of the seal contact width and the aluminum jacket thickness are done with an optical microscope. Further investigations on the segments will include metallography and hardness measurements.
From the detailed material and component behavior including the results of the long-term seal force and useable resilience investigations a better understanding of the overall seal behavior can be gained. The aim is to contribute to the development of material models and analytical approaches for the prediction of the sealing behavior in dependence of time and temperature.
In Germany spent nuclear fuel (SNF) and high level radioactive waste (HLW) are stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. Being licensed for up to 40 years of interim storage the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads.
The process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down.
The presence of large quantities of plastic waste and its fragmentation in various environmental compartments are an important subject of current research. In the environment, (photo ) oxidation processes and mechanical abrasion lead to the formation of microplastics. However, until now, there are no established quality assurance concepts for the analysis of microplastic (<5 mm) in environmental compartments, including sampling, processing and analysis.
The aim of the present work is the development of suitable examination methods and protocols (sampling, sample preparation and detection) to qualify and quantify microplastic in urbane water management systems. At first a fractional filtration system for sampling and the analytical tool, the so-called TED-GC-MS (thermal desorption gas chromatography mass spectrometry) were developed. The TED-GC-MS method is a two-step analytical procedure which consists of a thermal extraction where the sample is annealed and characteristic decomposition products of the polymers are collected on a solid phase. Afterwards these products are analysed using GC-MS. The developed fractional filtration for sampling and the TED-GC-MS for detection were used for quantitative analysis to screen the waste water influent and effluent of a Berlin waste water treatment plant for the most relevant polymers, polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA).
The results of the study revealed that the polymeres PE, PS and PP were detected in the effluent, and PE and PS were find in the raw waste water of the sewage treatment plant in Ruhleben, Berlin. Differences in polymer types and amounts were detected at different sampling dates and within different sieve fractions. Much higher amounts of polymers were observed in the raw waste water. The peak areas of the decomposition products, used for quantification of the polymers, were adjusted using so-called response factors since the TED-GC-MS method is more sensitive for PP and PS than for PE. It has been shown that PE is the most dominant polymer in the samples. Comparing the masses of polymers in the effluent and in the raw sewage, a removal of 99 % of the polymers in the water treatment plant can be assumed. These results are consistent with the literature where removal rates between 98-99 % were described.
Fully-reversed fatigue behavior of scarf joint repairs for wind turbine blade shell applications
(2022)
To enable a quick and cost-effective return to service for wind turbine blades, localized repairs can be executed by technicians in the field. Scarf repairs, shown to be highly efficient with a smooth load transition across angled joint walls and a restored aerodynamic profile, are the focus of this work. The failure mechanisms of these structures were examined under quasi-static tensile and fully-reversed cyclic loading. While the scarf ratio was held constant at 1:50, the repair layup was varied between large-to-small and small-to-large. The effect of the presence of resin pockets and the fiber orientation mismatch between parent and repair material on the restored strength of BIAX ±45° glass fiber reinforced polymer scarf joint structures was studied.
Localized patches are a cost- and time-effective method for repairing fiber-reinforced polymer (FRP) sandwich wind turbine rotor blade shells. To increase the understanding of their effect on the fatigue of the blades, this study examines the effect of various layup methods of localized repair patches on the structural integrity of composite sandwich structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the shell test specimens are produced as a curved structure with glass fiber reinforced polymer (GFRP) sandwiching a polyvinyl chloride (PVC) foam core. Patch repairs are then introduced with varying layup techniques, and material properties are examined with cyclic fatigue tests. The transition region between patch and parent material is studied in greater detail with finite element method (FEM) simulations, with a focus on the effect of fiber orientation mismatch. Damage onset, crack development, and eventual failure are monitored with in-situ non-destructive testing methods to develop a robust understanding of the effects of repair concepts on material stiffness and strength.
Wind turbine rotor blades commonly fail before their projected 20-year lifespan largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production. A potential repair alternative to restoring the mechanical properties of such lightweight fiber reinforced polymer (FRP) structures is to locally patch these areas with scarf joints. This type of repair allows for a smoother load distribution across the joint, and is favored especially on structures where minor aerodynamic contour changes are key. The effects of such repairs on the structural integrity, however, is still largely unknown. Building upon an understanding of the static load failure mechanism of GFRP scarf joints, presented at the ICCS23 Joint Event in 2020, the influence of the fiber orientation mismatch between parent and repair materials of 1:50 scarf joints on the failure mechanism of monolithic glass FRP specimens under cyclic fatigue load were examined in this study. Specimens with various layups were produced with the vacuum-assisted resin infusion (VARI) process using biaxial E-glass non-crimp fabric (NCF). The patch layers were then joined directly to the parent structure with the VARI using biaxial E-glass NCF with half the areal weight of the parent side to allow for better drapability. This mimics the soft-to-hard patch style utilized in wind turbine blade shell field repairs. The specimens were tested under uniaxial fatigue load, during which they were periodically monitored for damage onset. A comparison of the +45/-45° and 0/90° layups allowed for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. In addition to the tensile strength and stiffness property recovery assessment, a grayscale analysis using in-situ camera images determined the damage state leading to failure in each region across the scarf joint, which varied in the parent material versus scarf joint region, providing insight to the critical regions in this composite structure under cyclic loading.
As a type of high-performance composite material, glass-fiber reinforced plastics (GFRP) are favored for the construction of wind turbine rotor blades due to their high specific strength and stiffness properties (Grasse et al, 2010). During the blade manufacturing process, however, imperfections are often introduced, then further propagated due to harsh environmental conditions and a variety of loads (Caminero et al, 2013; Trappe et al, 2018). This leads to failure significantly before their designed lifespan. Since replacement of entire blades can be a costly potential outcome, localized repairs of the damaged region to restore structural integrity and thus lengthen its lifespan can executed in the field by technicians accessing the blades directly by suspended roping. These methods involve replacing the lost load path with a new material that is joined to the parent structure. In recent years, considerable studies have been conducted to investigate the influence of different repair parameters on the stress distribution, ultimate strength, impact behavior, and residual stresses of bonded repaired structures [Caminero et al, 2013; Trappe et al, 2018; Shufeng et al, 2014; Harman and Rider, 2011; Ahn and Springer, 2000; Lekou and Vionis, 2002). However, there currently do not exist any standardized repair procedures for wind turbine rotor blades. Namely, there is a lack of understanding about the effects of the layup of various repair methods, especially on the damage mechanism and fatigue life of the shells of rotor blades (Caminero et al, 2013; Trappe et al, 2018).
This work therefore aims to begin to enrich this knowledge gap by testing the influence of different variables among repair patches on the mechanical properties of sandwich composite structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the test specimens are produced as a GFRP structure to represent the outer shell portion of a wind turbine blade, then repaired with a scarf joint. Scarf repairs are favored as the most efficient of the common structural joints, as the removal of the damaged area with angled walls leads to a nearly uniform shear stress distribution along the bond surface and no eccentricity in the load distribution (Caminero et al, 2013; Lekou and Vionis, 2002; Siener, 1992).
The performance of specific layup methods of repair patches, namely a large-to-small versus small-to-large scheme of repair layers, is studied with static and load-controlled fatigue testing, then compared to pristine test specimens as well as to each other in terms of mechanical property restoration. The transition layer between repair and parent material is especially of interest in the performance of the structure. Damage onset, crack development and eventual failure are monitored in-situ with non-destructive testing methods, including thermography with an infrared camera system and a 3D deformation analysis system, to develop a more robust understanding of the effects of these repair concept variables on wind turbine blade shell structures.
Fully-reversed fatigue behavior of scarf joint repairs for wind turbine blade shell applications
(2022)
Due to manufacturing imperfections which can propagate to damage under in-service loads, wind turbine rotor blades, made primarily of glass fiber reinforced polymers (GFRP), often fail significantly before their design life. To enable a quick and cost-effective return to service, localized repairs can be executed by technicians in the field, directly accessing the blades by suspended roping. Scarf joint repairs, shown to be highly efficient with a smooth load transition across angled joint walls and a restored aerodynamic profile, are the focus of this study. The damage mechanisms of these structures were examined under fully-reversed mechanical cyclic loading with a load ratio R = -1, which was made possible on the coupon scale by a custom designed anti-buckling support. The number of cycles to failure were compared across load levels. While the scarf joint ratio was held constant at 1:50, known from industry and literature to be a good compromise between restored mechanical properties and repair size, the layup sequence was varied between small-to-large and large-to-small. Hereby the effect of the presence of resin pockets and fiber orientation mismatch between the parent and repair structure on the failure mechanism as well as fatigue strength of ±45° GFRP scarf joint repair structures was studied. Strain development across the joint length was measured to assess stiffness degradation in addition to the fatigue strength recovery of scarf joint structures with respect to pristine reference specimens. Grayscale analysis was used to monitor the damage state leading to fracture across the specimens. Post-mortem fractography analysis with light microscopy described the global failure mechanisms as well as local damage distribution within the structure, all of which provided insight to critical variables in scarf joint GFRP structures under fully-reversed mechanical cyclic loading, allowing for the tailoring of such repairs on wind turbine blade shells for maximum restoration of service life.
Wind turbine rotor blades, made of fiber reinforced polymers (FRP), often fail before their projected 20-year lifespan, largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production [1]. A potential repair alternative is to locally patch these areas of the blades with adhesively bonded structural repairs. However, the effects of such repair methods of the outer shell region on the structural integrity of the rotor blades are still largely unknown, and are thus investigated in this project.
The shell components of rotor blades are made of FRP composite material sandwiching a lightweight core, often a rigid foam or Balsa wood. The repair methods involve replacing the lost load path with a new material that is joined to the parent structure [2]. Repairs in this project focus on the scarf method, which allow for a smoother load distribution across the joint, aiming to study the damage mechanism of glass FRP scarf repairs for wind turbine blade shell applications. Namely, the source and path of the damage initiation and propagation, role of the interface between parent and patch material, and the role of the fiber orientation mismatch at this interface are examined. Biaxial ±45° and 0/90° FRP specimens are produced with the vacuum-assisted resin infusion (VARI) process using E-glass non-crimp fabric. The patch layers are then joined using VARI with a scarf ratio of 1:50, using glass FRP fabric with half the areal weight of the parent side to allow for better drapability. The methods and practices in specimen production are based on common industry practice in rotor blade shell manufacturing and repairs.
The specimens are tested under uniaxial tensile load, during which they are periodically monitored for damage onset. A comparison of the ±45° and 0/90° specimens allows for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. Although failure in both orientations begins as delamination at the joint edge, the difference in the mechanisms at play in the two different specimen types leads ultimately to different fracture paths. Namely, in the inter fiber failure mechanism of the ±45° specimens, the higher interlaminar strength compared to the intralaminar strength of the laminate leads to intralaminar failure of the ±45° scarf joint specimens. Alternatively, the competition in the 0/90° specimens lies between the interlaminar strength and fiber failure strength, and here we experience failure primarily across the scarf joint length. The scarf joint in the 0/90° specimens disrupts the continuity of the load-carrying 0° layers, directing the failure path to remain primarily along the scarf joint. Experimental results are compared to finite element analyses of scarf patch repairs on glass FRP sandwich specimens with the same respective layup orientations, where the damage initiation regions are identified and correlated to fiber orientation, serving as a bridge to future work which will experimentally examine the scarf repair patches on sandwich shell specimens.
Wind turbine rotor blade shells are manufactured as sandwich structures with fiber-reinforced polymer (FRP) due to the material’s high specific stiffness and strength. With a growing renewable energy industry and thereby a spread of wind energy farms, especially in offshore applications, the need to fully utilize turbines through their designed lifespan is becoming increasingly essential. However, due to imperfections during manufacturing, which are then propagated by harsh environmental conditions and a variety of loads, blades often fail before their projected lifespan. Thus, the need for localized repair patch methods for the outer shell portions of the blades has become of greater interest in recent years, as it is crucial to the optimal compromise between continuation of wind energy production, cost efficiency, and restoration of structural performance. To increase the understanding of the effect on the fatigue life of the rotor blades, this study tests localized repair patch methods and compares them to each other as well as to reference, non-repaired specimens. Manufactured with the vacuum-assisted resin infusion process, the shell test specimens are produced as a curved structure with glass FRP sandwiching a polyvinyl chloride foam core to best represent a portion of a rotor blade shell. Patch repairs are then introduced with varying layup techniques, and material properties are examined with cyclic fatigue tests. The intermediate scale test specimens allow for the observation of material as well as structural variables, namely of interest being the stiffness and strength restoration due to the repair patches. Damage onset, crack development, and eventual failure are monitored with in-situ non-destructive testing methods to develop a robust understanding of the effects of repair concepts.
Hochleistungsverbundwerkstoffe, bzw. Glasfaser-Kunststoff-Verbunde (GFK), haben sich als Leichtbauwerkstoffe für Leichtflugzeuge und Rotorblätter von Windkraftanlagen etabliert. Die hohe spezifische Festigkeit und Steifigkeit qualifizieren sie besonders für diese Anwendung. Während der Fertigung werden Imperfektionen häufig in die Blattschalen eingebracht. Durch Witterungseinflüsse kommt es zum Schadensfortschritt. Infolgedessen treten Schäden in der Blattschale, die den sicheren Betrieb gefährden können, weit vor der projektierten Lebensdauer von 20 Jahren auf. Da der Austausch von ganzen Blättern sehr kostintensiv ist, ist eine lokale Reparatur des geschädigten Bereichs zur Wiederherstellung der strukturellen Integrität, viel preisgünstiger. Die Reparatur von Rotorblättern ist in den letzten Jahren zu einem wichtigen Thema geworden. Derzeit werden verschiedenste Reparaturkonzepte angewendet. Eine einheitliche Reparaturvorgabe gibt es bisher nicht. Die Auswirkungen der angewendeten Reparaturkonzepte auf die Betriebsfestigkeit der Reparaturstelle sind weitestgehend unbekannt und sollen deshalb in diesem Projekt untersucht werden. Gekrümmte Voll-Laminat sowie Sandwich Prüfkörper werden mit dem Vacuum-Assisted-Resin-Infusion-Prozess (VARI) produziert. Um einen Teil einer Rotorblattschale darzustellen, sind sie als GFK aufgebaut, beziehungsweise die Sandwich Strukturen mit einem Polyvinylchlorid-Schaumkern (PVC) Kern, wie im Original. Schalenreparaturen in verschiedenen Layup-Techniken und Geometrie werden eingebracht und die Materialeigenschaften mit zyklischen Ermüdungstests untersucht. Im Projekt werden ideal im Labor erzeugte Reparaturstellen mit in der Praxis angewendeten Ausführungstechniken eines Industriepartners experimentell verglichen. Für die in-situ Detektion der Schadensentwicklung während des Ermüdungsversuches kommt ein kombiniertes Felddehnungs- und Thermografie-Kamerasystem zum Einsatz. Das mechanische Verhalten und die Schadensentwicklung in den verschiedenen reparierten Prüfkörper wird miteinander sowie mit den Referenzproben ohne Reparaturstellen verglichen. Zudem wird in numerischen Modellen für die verschiedenen Reparaturtechniken eine Spannungsanalyse durchgeführt um hinsichtlich der Betriebsbeanspruchung eine Bewertung angeben zu können.
High-performance composites, including glass-fiber reinforced plastic (GFRP) materials, are favored as a construction material for wind turbine rotor blades due to their high specific strength and stiffness properties. During the manufacturing process, however, imperfections are often introduced, then further propagated due to harsh environmental conditions and a variety of loads. This leads to failure significantly before their projected 20-year lifespan. As replacement of entire blades can be a costly potential outcome, localized repair of the damaged region to restore structural integrity and thus lengthen its lifespan has become an important issue in recent years. Rotor blades are often repaired using a common technique for composite laminates: adhesively bonded structural repair patches. These methods involve replacing the lost load path with a new material that is joined to the parent structure, and include scarf or plug repairs. However, there currently do not exist any standardized repair procedures for wind turbine rotor blades, as comparisons of blade properties repaired with the existing methods have not been studied in depth. Namely, there is a lack of understanding about the effects of various repair methods on the fatigue life of the shells of rotor blades. This study therefore aims to begin to fill this knowledge gap by testing the influence of different repair patches on the blades’ mechanical properties. Manufactured with the vacuum-assisted resin infusion process, the test specimens are produced as a curved structure with GFRP sandwiching a polyvinyl chloride foam core to best represent a portion of a rotor blade shell. Scarf repairs are then introduced with varying layup techniques, and material properties are examined with cyclical fatigue tests. Crack growth and development is monitored during fatigue testing by various non-destructive testing methods, including passive thermography with an infrared camera system, and a 3D deformation analysis system with ARAMIS. Large deformation fields and detection of in- and out-of-plane deformations is thus possible in-situ. The mechanical behavior and development of defects in the various repaired specimens is compared to each other as well as to reference test specimens with no repair patches. In-situ test data is combined with further non-destructive testing methods, including laminography, and active thermography, to develop a robust understanding of the effects of repair concepts.
The introduction of the 5G technology and automotive radar applications moving into higher frequency ranges trigger further miniaturization of LTCC technology (low temperature co-fired ceramics). To assess dimensional tolerances of inner metal structures of an industrially produced LTCC multilayer, computer tomography (CT) scans were evaluated by machine learning segmentation.
The tested multilayer consists of several layers of a glass ceramic substrate with low resistance silver-based vertical interconnect access (VIA). The VIAs are punched into the LTCC green tape and then filled with silver-based pastes before stacking and sintering. These geometries must abide by strict tolerance requirements to ensure the high frequency properties.
This poster presents a method to extract shape and size specific data from these VIAs. For this purpose, 4 measurements, each containing 3 to 4 samples, were segmented using the trainable WEKA segmentation, a non-commercial machine learning tool. The dimensional stability of the VIA can be evaluated regarding the edge-displacement as well as the cross-sectional area. Deviation from the ideal tubular shape is best measured by aspect ratio of each individual layer. The herein described method allows for a fast and semi-automatic analysis of considerable amount of structural data. This data can then be quantified by shape descriptors to illustrate 3-dimensional information in a concise manner. Inter alia, a 45 % periodical change of cross-sectional area is demonstrated.
Die Steigerung der Leistung und des thermodynamischen Wirkungsgrades von Verbrennungsmotoren führt zu erhöhten Anforderungen an die Festigkeit abgasführender Komponenten wie z. Bsp. Abgasturbolader. Als Folge erhöhter thermomechanischer Wechselbeanspruchungen (TMF) im Betrieb kommt es an den mechanisch und/oder thermisch höchst beanspruchten Stellen der Bauteile zur Bildung von Rissen, wodurch die Lebensdauer der Komponenten begrenzt wird. Derzeit werden bei Turboladern heißgehende Bauteile mit detektierten Rissen zumeist prophylaktisch ersetzt, da die weitere Ausbreitung der Risse während des Betriebs nicht vorhergesagt werden kann. Um diese aufwändige und un- ökonomische Praxis zu vermeiden, wurde im vorliegenden Forschungsvorhaben eine rechnerische Bewertungsmethode auf Basis der experimentellen und numerischen Bruchmechanik erarbeitet, mit deren Hilfe bereits in der Auslegungsphase oder während des Betriebs die (restliche) Lebensdauer der abgasführenden Komponenten vorhergesagt werden kann. Damit wird erstmalig die quantitative Vorhersage der Rissentwicklung bei TMF-Beanspruchungsbedingungen unter Berücksichtigung großer zyklischer viskoplastischer Verformungen ermöglicht.
Zentrales Ergebnis des Vorhabens ist eine automatisierte Berechnungsprozedur auf der Basis spezieller Finite-Elemente-Techniken (FEM), womit sowohl der Pfad als auch die Größe eines Risses als Funktion der Anzahl der Lastwechsel in Bauteilen unter TMF-Bedingungen berechnet werden kann. Als geeigneter Beanspruchungsparameter zur Bewertung des Rissfortschritts unter TMF wurde die zyklische Rissöffnungsverschiebung ΔCTOD verwendet. Das Werkstoffverhalten des betrachteten austenitischen Gusseisens Ni-Resist D-5S wurde mit einem validierten viskoplastischen, temperaturabhängigen Materialmodell modelliert, das zur Berücksichtigung große Verzerrungen und Rotationen am Riss erweitert wurde. Für die genaue Berechnung des ΔCTOD bei TMF wurden effiziente FEM-Techniken erarbeitet. Zur Simulation der Rissausbreitung wurde ein automatischer FEM-Algorithmus mit inkrementeller adaptiver Neuvernetzung entwickelt, bei dem die Verformungen und inelastischen Zustandsvariablen jeweils vom alten auf das neue Netz übertragen werden. Dieser Algorithmus wurde im Software-Paket ProCrackPlast implementiert, das in Verbindung mit dem kommerziellen FEM-Code Abaqus zur Lösung dreidimensionaler Rissprobleme zur Verfügung steht. Ziel der umfangreichen experimentellen Arbeiten war es, an isothermen LCF und anisothermen TMF-Versuchen mit gekerbten Flachzugproben (SENT) das Risswachstum im Temperaturbereich von 20 °C bis 700 °C zu ermitteln. Mit Hilfe begleitender 2D FEM Simulationen wurden anhand dieser Datenbasis die Rissfortschrittskurven des Werkstoffs unter Anwendung des ΔCTOD-Konzepts bestimmt und in geeigneter, parametrisierter Form den Nutzern zur Verfügung gestellt. Die Versuche an SENT-Proben wurden mit der entwickelten Software ProCrackPlast als 3D Modell simuliert. Der Vergleich der 2D und 3D Simulationen ergab einen systematischen Unterschied im CTOD und CTOD, der mit Hilfe eines Übertragungsfaktors korrigiert wurde. Der Vergleich der 3D Berechnungen mit den Experimenten zeigte eine zufriedenstellende Übereinstimmung der er- reichten Risslänge mit der Zahl der Lastzyklen im gesamten Temperaturbereich, wobei die numerische Prognose meist auf der konservativen / sicheren Seite lag. Die Übertragbarkeit der Ergebnisse der 2D Parameteridentifikation auf 3D Risskonfigurationen mit Mixed-Mode Beanspruchung ist mit zusätzlichen Versagenshypothesen verbunden, die aufgrund fehlender Versuchsdaten im Vorhaben nicht endgültig geklärt werden konnten. Zur Validierung des Gesamtkonzeptes wurden LCF-Proben mit einem bauteil- typischen Oberflächenriss experimentell und numerisch untersucht. In der Simulation konnte die komplexe Form und Größe der Rissentwicklung zufriedenstellend (richtig) vorhergesagt werden. Die Leis- tungsfähigkeit der erarbeiteten rechnerische Bewertungsmethode wurde an weiteren TMF-Beispielen vorgestellt und diskutiert. Die Software ProCrackPlast und die viskoplastische Materialroutine wurden dem Anwenderkreis des Vorhabens zusammen mit einem Nutzer-Handbuch und Verifikationsbeispielen zur Verfügung gestellt.
Das Ziel des Forschungsvorhabens ist erreicht worden.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
Due to combined cyclic mechanical and thermal loading during operation, the material of exhaust gas conducting components of combustion engines is exposed to thermomechanical fatigue (TMF). This leads to formation and growth of cracks, especially at the most highly stressed points of these components. In order to better predict the service life of cracked components before failure, it is necessary to identify a crack propagation law for the material used. Isothermal crack propagation tests have been carried out at several temperatures with a typical cast iron to identify such a law. The crack length is measured by the potential drop method. The compliance method, fractography and thermographic camera measurements have been used to validate and calibrate the potential drop measurements. Each of the isothermal tests has been simulated using a specially developed FEM-algorithm based on remeshing and remapping. This algorithm has been implemented in python and ABAQUS. Thereby, the crack tip region is modeled by collapsed Quad8 elements. From the individual simulations, the cyclic crack tip opening displacement (ΔCTOD) is extracted and regarded as a potential fracture mechanics parameter which controls the crack growth rate. By combining the data from the experiments and the simulations, the crack propagation law has been identified. Finally, anisothermal crack propagation tests have been performed for validation of the crack growth law.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The finite element software ProCrackPlast is developed for the automated simulation of fatigue crack growth in arbitrarily loaded three-dimensional components with large scale plastic deformations, in particular under cyclic thermomechanical (TMF) loading.
ProCrackPlast is developed by extending the software Procrack, created at TU Freiberg for linear-elastic crack growth simulations. The pre-processing, FEM analysis, and the post-processing in ProCrackPlast are done by the commercial software ABAQUS. ProCrackPlast resorts to a crack growth procedure which adaptively updates the crack in finite increments based on the fracture-mechanical parameter, cyclic crack tip opening displacement ΔCTOD . Features of this software along with two application examples of fatigue crack growth in a typical cast steel, Ni-Resist, are presented in this paper to show its capability and performance.
Recently, detection and conversion of high energy radiation such as ultraviolet and X-rays has gained renewed attention. In part, technological applications in radioimaging and tomography have developed considerably as to allow lower dosages and higher resolutions, which require optimized scintillators and dosimeters. On the other hand, the increasing effort to reduce carbon footprint in energy production has triggered an intensive search for materials that can be excited with sunlight, ranging from photocatalysts to solar concentrators. At LEMAF – Laboratory of Spectroscopy of Functional Materials at IFSC/USP, we have been developing bulk glasses, polycrystalline and composite materials designed to target both challenges and, in this work an overview of recent progresses and of the state of art of these materials will be given.
For instance, the few available comercial scintillators are crystalline materials with costly and time consuming growth which hinders the development of new compositions. Glasses and glass ceramics, such as the NaPGaW composition developed in our lab, present high density, very good optical properties and high chemical stability which allow them radioluminescent response when doped with low concentrations of Ce3+, Eu3+ and Tb3+ offering a promise as alternatives to crystal scintillators. On the other hand, phosphor in glass (PiG) composites based on the persistent luminescent polycrystalline material Sr2MgSi2O7:Eu2+,Dy3+ (SMSO) embedded into NaPGa glasses offer interesting perspectives for the of UV light into visible, useful for white light generation (lighting), improved harvesting and conversion of solar light when coupled to c-Si PV cells and photocatalysis. These and other examples will be discussed.
The glasses are prepared through the conventional melt quenching technique, followed by controlled heating when glass ceramics are desired. The persistent luminescent phosphor is prepared by the microwave assisted technique (MAS) much faster and with considerable energy consumption reduction than in the usual solid state synthesis. The materials are characterized from the structural, morphological and spectroscopic (optical – UV-Vis, PL, PLE, and structural – NMR, EPR) points of view such that structure-property correlations are constantly sought to feedback synthesis and processing. Fig. 1, illustrates two examples of scintillator glasses doped with Tb3+ and PiG composites doped with Eu2+ and Dy3+.
The glass system (50NaPO3–20BaF2–10CaF2–20GdF3)-xTbCl3 with x = 0.3, 1, 3, 5, and 10 wt % was investigated. We successfully produced transparent glass ceramic (GC) scintillators with x = 1 through a melt-quenching process followed by thermal treatment. The luminescence and crystallization characteristics of these materials were thoroughly examined using various analytical methods. The nanocrystallization of Tb3+-doped Na5Gd9F32 within the doped fluoride-phosphate glasses resulted in enhanced photoluminescence (PL) and radioluminescence (RL) of the Tb3+ ions. The GC exhibited an internal PL quantum yield of 33 % and the integrated RL intensity across the UV-visible range was 36 % of that reported for the commercial BGO powder scintillator. This research showcases that Tb-doped fluoridephosphate GCs containing nanocrystalline Na5Gd9F32 have the potential to serve as efficient scintillators while having lower melting temperature compared to traditional silicate and germanate glasses.
Compared to mechanisms like solid solution strengthening, the stacking fault energy (SFE) should be considered as a further factor that influences the material properties. The effect of SFE of alloys or individual elements on strength and resistance can vary considerably. In the high-temperature regime above 700 ◦C, there are still significant gaps in the knowledge about the effect of the SFE on the mechanical properties of single-phase alloys. The effect of SFE on creep resistance of two face-entered cubic equiatomic medium and high entropy alloys, CrCoNi and CrMnFeCoNi, respectively, is evaluated to fill parts of these gaps. Using the Bridgman solidification process, the alloys were produced as single crystals and crept under vacuum at 700 ◦C up to 1100 ◦C. This work shows a significant impact of the lower SFE of CrCoNi on the creep behavior compared to the results of previous investigations of CrMnFeCoNi. The creep resistance of the former is higher over the complete temperature range. At very high temperatures, the strengthening effect of the stacking faults is significantly present. The formation of tetragonal stacking faults and extended dislocation nodes can be identified as the reason for this effect.
The main deference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which moves from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Investigation of temperature dependent solid solution strengthening in single phase multicomponent alloys with medium and high entropy using creep testing was performed. Creep tests carried out on single phase SX CrCoNi , CrMnFeCoNi and pure Ni from 700 to 1200 °C excluding oxidation, grain boundaries and multiphase effects. It was found that the influence of solid solution strengthening of CrCoNi and CrMnFeCoNi increases by decreasing temperature (1200 to 700 °C), and dislocation forests occur in CrCoNi and CrMnFeCoNi in comparison to pure Ni.
Um den sicheren Betrieb von Windkraftanlagen zu gewährleisten, werden Rotorblätter nach der Fertigung und nach Reparatur mit verschiedenen zerstörungsfreien Verfahren auf Schaden untersucht. Bei der Fertigung von Blattschalen, die in einer Sandwich-Schalenbauweise gefertigt werden, entstehen Imperfektionen, die unter Belastung zu großen Rissen führen können. Zur Prüfung von Blattschalen wird unter anderem Ultraschallprüfung in Kontakttechnik eingesetzt. Um den Wartungsaufwand von Ultraschallanlagen zu reduzieren und um manche Kompositstrukturen vor Koppelmittel zu schützen, wird die Anwendung von Luftultraschall erforscht. Insbesondere große Fortschritte gibt es im Bereich der Entwicklung neuer Wandler.
In diesem Beitrag berichten wir über die Luftultraschallprüfung von Schalen für Rotorblätter. Es wurden typische Sandwichschalenstrukturen hergestellt und mit einem eigenentwickelten Schalenprüfstand unter simulierter Betriebsbeanspruchung belastet. Die in den Schalenprüfkörpern entstandenen Schäden wurden außerhalb des Prüfstandes mit Luftultraschall in Durchschallung untersucht. Es wurden fokussierende Wandler auf Basis von Ferroelektreten entwickelt und für diese Prüfungen eingesetzt. Mit zusätzlicher elektrischer Vorspannung konnte die Empfindlichkeit der Empfänger deutlich erhöht werden. Die nach dem Lastwechsel entstandenen Schäden in den Rotorblattschalen waren eindeutig zu detektieren.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
Um den sicheren Betrieb von Windkraftanlagen zu gewährleisten, werden Rotorblätter nach der Fertigung und nach Reparatur mit verschiedenen zerstörungsfreien Verfahren auf Schaden untersucht. Bei der Fertigung von Blattschalen, die in einer Sandwich-Schalenbauweise gefertigt werden, entstehen Imperfektionen, die unter Belastung zu großen Rissen führen können. Zur Prüfung von Blattschalen wird unter anderem Ultraschallprüfung in Kontakttechnik eingesetzt. Um den Wartungsaufwand von Ultraschallanlagen zu reduzieren und um manche Kompositstrukturen vor Koppelmittel zu schützen, wird die Anwendung von Luftultraschall erforscht. Insbesondere große Fortschritte gibt es im Bereich der Entwicklung neuer Wandler.
In diesem Beitrag berichten wir über die Luftultraschallprüfung von Schalen für Rotorblätter. Es wurden typische Sandwichschalenstrukturen hergestellt und mit einem eigenentwickelten Schalenprüfstand unter simulierter Betriebsbeanspruchung belastet. Die in den Schalenprüfkörpern entstandenen Schäden wurden außerhalb des Prüfstandes mit Luftultraschall in Durchschallung untersucht. Es wurden fokussierende Wandler auf Basis von Ferroelektreten entwickelt und für diese Prüfungen eingesetzt. Mit zusätzlicher elektrischer Vorspannung konnte die Empfindlichkeit der Empfänger deutlich erhöht werden. Die nach dem Lastwechsel entstandenen Schäden in den Rotorblattschalen waren eindeutig zu detektieren.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
Recently, additive manufacturing of ceramics has achieved the maturity to be transferred from scientific laboratories to industrial applications. At the same time, research is progressing to expand the boundaries of this field into the territory of novel materials and applications. This feature issue addresses current progress in all aspects of additive manufacturing of ceramics, from parts design to feedstock selection, from technological development to characterization of printed components.
Fresnoite glass with excess SiO2 exhibits oriented surface crystallization, in contrast to the stoichiometric glass composition. Recent EBSD studies documented that the crystals in BTS (2BaO-TiO2-xSiO2, x=0-3) can occur in a distinct [101]-orientation perpendicular to the surface and claimed that this orientation is not a result of growth selection. During these previous studies, however, the effect of surface preparation and surrounding atmosphere during the crystallization experiments were not considered. As these parameters may influence crystal orientation, we studied the surface crystallization of a BTS glass (2BaO-TiO2–2.75SiO2) under controlled conditions with the help of light, electron and polarisation microscopy as well as EBSD. Heat treatments for one hour at 840°C of fractured BTS glass surfaces in air resulted in a large number of not-separable surface crystals. This large number of crystals can be caused by dust particles, which act as nucleation agents. As crystal growth velocity could further be influenced by humidity, our experiments are performed in a filtered and dried air atmosphere. The crystal morphology and orientation will be analysed in dependence of the sample preparation and a differing surrounding atmosphere.
Inconel 718 (IN718) is a traditional age-hardenable nickel-based alloy that has been increasingly processed by additive manufacturing (AM) in recent years. In the as-solidified condition, IN718 exhibits chemical segregation and the undesired Laves phase, requiring a solution annealing (SA) prior to aging. The material produced by AM does not respond to the established thermal routines in the same way as conventionally produced IN718, and there is still no consensus on which routine yields optimal results. This work aims to provide a fundamental understanding of the heat treatment (HT) response by continuously monitoring the microstructural evolution during SA via time-resolved synchrotron x-ray diffraction, complemented by ex-situ scanning electron microscopy (SEM). The samples were produced by laser powder bed fusion to a geometry of 10x20x90 mm³, from which Ø1x5 mm³ cylindric specimens were extracted. Two different scanning strategies – incremental 67° rotations, Rot, and alternating 0°/67° tracks, Alt – were used, leading to two different as-built conditions. 1-hour SAs were carried out in the beamline ID22 of the ESRF at 50 KeV. Two SA temperatures, SA1 = 1020 °C, and SA2 = 1080 °C were tested for each scanning strategy. Data were processed using the software PDIndexer. In the as-built state, all samples showed typical subgrain columnar cell structures with predominant Nb/Mo segregation and Laves phase at the cell walls, as seen by SEM. The Alt scan induced higher intensity on the Laves peaks than the Rot scan, suggesting a greater content of Laves. Chemical homogenization in the SA was largely achieved during the heating ramp (Fig. 1). SA2 eliminated the Laves peaks just before reaching 1080 °C, and mitigated differences between Rot and Alt samples. On the other hand, SA1 induced the precipitation of the generally detrimental δ phase, also observed by SEM. Furthermore, the Rot scan showed higher δ peak intensities than the Alt scan, indicating a higher content of δ in the latter. No signs of recrystallization were observed in any of the investigated SAs.
In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
The elastic constants are the most basic mechanical properties of a material and are needed for any structural analysis of a component. For example, they have a major influence on the eigenfrequencies of vibrating parts. Single crystals of Ni-base superalloys are strongly anisotropic, which means that the observed properties are orientation dependent. Tensor algebra is then required to mathematically formulate the elastic properties and their relations to the crystal orientation. Hence, this chapter first summarizes some basic definitions and calculation rules for Rotation matrices, including the definition of the Euler angles, which are most commonly used to define the relative orientations of the crystal and the component. Parts of this chapter closely follow the lines of the excellent exposition of the topic by Olschewski.
The large number of TEM investigations and the regular microstructure
of single-crystal nickel-base superalloys has boosted the development of a number of physically motivated constitutive laws. In contrast to the more phenomenological models discussed in the next chapter, these models use dislocation densities as internal variables. Obvious advantages are that the computed densities can be compared to TEM observations and the Deformation mechanisms can be easier translated into mathematical equations.
Single crystal superalloys usually contain pores of sizes 5-10 micro-m after casting and heat treatment. These pores can be reduced under compression by combined creep and diffusion in a subsequent treatment called Hot Isostatic Pressing (HIP). The paper presents a methodology to simulate pore shrinkage under HIP conditions in two dimensions (2D).
At the scale of the pores, which is also the scale of the sub-grains (<50 micro-m) the dislocation sources cannot be assumed to be homogeneously distributed. Thus, the applicability of classical crystal plasticity is questionable. In this case, the transport of dislocations under an applied stress from the location where they are nucleated must be explicitly modelled. This is done by solving the transport equations for the dislocation densities and the elasticity equations in 2D. The dislocations are assumed to be nucleated at Low Angle Boundaries. They glide or climb through the sub-grains with a stress dependent velocity.
The transport equations are solved by the Flux-Corrected Transport method, which belongs to the predictor-corrector class of algorithms. In the first step, an artificial diffusion is introduced, which suppresses spurious oscillations of the solution. In a second step, the solution is corrected in such a way that no additional extremes appear and that the extremes do not grow. The algorithm is validated by simulating the transport of simple distributions with a constant velocity field.
With the dislocation velocities and the computed dislocation densities, the inelastic shear rate at the slip system level is computed by integrating the Orowan equation. In the 2D-setting, three slip systems are considered. The contributions of these slip systems are summed up to obtain the total inelastic strain rate. Dislocation glide and climb and the coupling of climb with vacancies diffusion are considered.
The resolution of the equilibrium equations from the inelastic strains turned out to be prone to numerical instabilities. As an alternative, the stresses are directly computed from the distribution of geometrically necessary dislocations following the method presented in. The resulting boundary value problem is solved by the Least-Square Finite Element method.
Examples of simulations are presented for a representative region under creep tension and for a pore shrinking under external pressure.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
The creep behavior of single-crystals of the nickel-base superalloy CMSX-4 was investigated at 1288°C, which is the temperature of the hot isostatic pressing (HIP) treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no Gamma’-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g. the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-section area psi of [001] crystals reached nearly 100%, while for a [111] crystal psi=62%. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals didn’t not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. From the shape of deformed specimens and TEM investigations it was concluded that the main strain contribution resulted from <011> {111} octahedral slip.
Turbine blades often contain cylindric holes used to generate an air film that protects the blade alloy from the hot gases. These cooling holes of diameter around one mm are drilled by laser through the thickness of the blades. Unfortunately, the resulting stress concentration and the drilling-induced damage are known to favor crack initiation from the holes. It is thus necessary to assess the impact of these cooling holes on the structural integrity of the blades. Since cracks initiate very readily, the fatigue life of the components is mainly controlled by the propagation of the cracks in the stress gradient induced by the holes.
For this purpose, displacement controlled high-temperature LCF (Low-Cycle-Fatigue) tests were performed with center hole specimens of a coarse-grained Nickel base Superalloy. The tests were stopped after a defined load drop. In addition, crack propagation tests with Double Edge Notch specimens were performed. Moreover, specimens with different hole surface finishes were investigated, which showed a detrimental effect of the hole surface roughness. In parallel, an evaluation of the LCF tests based on a fracture mechanics-based model (Madia et al., Eng. Fract. Mech., 2018) has been applied. Thereby, the specimen life is controlled by the crack propagation time until failure. Crack growth is controlled by a modified NASGRO equation accounting for large-scale yielding and a progressive build-up of crack closure. The initial crack size has been derived from the measurements of defects around the borehole. A reasonable agreement between predicted and measured lifetimes is observed if one keeps in mind the large uncertainty regarding the effective shape of the cracks.
The scatter of fatigue crack growth data can become significant for coarse grained materials. By using a probabilistic description of crack propagation as the foundation of a lifetime prediction model, lifetime scatter of laboratory specimens can be reproduced. However, the lifetime of real components is subjected to additional scattering factors such as surface condition or uncertainty regarding direction and shape of emerging cracks. These factors need to be addressed in order to exploit the advantages of probabilistic description, i.e. the reduction of unnecessary conservatisms.
High temperature LCF (Low-Cycle-Fatigue) tests were performed with center hole specimens of a coarse-grained Nickel base Superalloy. In addition, crack propagation tests with Double Edge Notch specimens were performed. A procedure to detect the shape of the starting crack that combines the potential drop method and induction thermography was developed. The geometry and the number of notches were varied. Moreover, specimen with different hole surface finishes were investigated, which showed a detrimental effect of the roughness of the hole surface.
The results have been compared to predictions of a probabilistic tool for the estimation of lcf lifetime that has been calibrated beforehand on laboratory specimens with and without notches. In parallel, a fracture mechanics-based lifetime model was developed, which includes the initial crack size as a critical parameter. Thereby, the influence of the large grain size (>1mm), and the shape of the starting crack at the notch were considered.
Acknowledgements
The investigations are conducted as part of the joint research program COOREFLEX-Turbo in the frame of AG Turbo. The work is supported by Siemens AG and the Bundesministerium für Wirtschaft und Technologie (BMWi) as per resolution of the German Federal Parliament under grant number 03ET7071E.
Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2018)
This work presents a method for the yield function determination of additively manufactured parts of S316L steel. A crystal plasticity model is calibrated with test results and used afterwards to perform so-called virtual experiments, that account for the specific process-related microstructure including crystallographic and morphological textures. These simulations are undertaken on a representative volume element (RVE), that is generated from EBSD/CT-Scans on in-house additively manufactured specimen, considering grain structure and crystal orientations. The results of the virtual experiments are used to determine an anisotropic Barlat yield function, that can be used in a macroscopical continuum-sense afterwards. This scale-bridging approach enables the calculation of large-scale parts, that would be numerically too expensive to be simulated by a crystal plasticity model.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2018)
This work presents a method for the yield function determination of additively manufactured parts of S316L steel. A crystal plasticity model is calibrated with test results and used afterwards to perform so-called virtual experiments, that account for the specific process-related microstructure including crystallographic and morphological textures. These simulations are undertaken on a representative volume element (RVE), that is generated from EBSD/CT-Scans on in-house additively manufactured specimen, considering grain structure and crystal orientations. The results of the virtual experiments are used to determine an anisotropic Barlat yield function, that can be used in a macroscopical continuum-sense afterwards. This scale-bridging approach enables the calculation of large-scale parts, that would be numerically too expensive to be simulated by a crystal plasticity model.
With the introduction of a mass transport mechanism the entire problem is subjected to a time frame that dictates the time-dependent action of soluted species on mechanical properties. A numerical framework within the phase-field approach is presented with an embrittlement-based coupling mechanism. The underlying functionals are expressed in terms of the displacement, mass concentration and crack phase-field. Within the phase-field approach the modelling of sharp crack discontinuities is replaced by a diffusive crack model facilitating crack initiation and complex crack topologies without the requirement of a predefined crack path. The isotropic hardening of the elasto-plastic deformation model and the local fracture criterion are affected by the species concentration. This allows for embrittlement and leads to an accelerated crack propagation. An extended mass transport equation for hydrogen embrittlement, accounting for mechanical stresses and deformations, is implemented. For stabilisation purposes a staggered scheme is applied to solve the system of partial differential equations by a multi-field finite-element method. A thermodynamically consistent coupling relation that accommodates the required mechanisms is presented.
Sulfur and water have a fundamental impact on the corrosion rate and potential failure of materials. It is therefore necessary to understand the mechanisms, rates, and potential means of transport, as well as the reactions of these elements with an alloy. This work investigates the effect of water vapor in the initial stages of SO2 corrosion of an ferritic model alloy containing 9 wt% Cr and 0.5 wt% Mn.
The exposure experiments were studied at 650°C in situ under laboratory conditions using energy-dispersive x-ray diffraction analysis. Two separate experiments were run, one with a 99.5% Ar + 0.5% SO2 atmosphere and one with a 69.5% Ar + 0.5% SO2 + 30% H2O atmosphere. With a wet atmosphere, the alloy formed a scale with decreasing oxygen content towards the scale–alloy interface. Sulfides were identified above and below a (Fe, Cr)3O4 layer in the inner corrosion zone. In contrast to this, the overall scale growth was slower in a dry SO2 atmosphere.
Chromia forming high alloyed ferritic-austenitic steels are being used as boiler tube materials in biomass and coal-biomass co-fired power plants. Despite thermodynamic and kinetic boundary conditions, microstructural features such as grain orientation, grain sizes or surface deformation contribute to the oxidation resistance and formation of protective chromium-rich oxide layers. This study elucidates the impact of microstructure such as the grain size and number of carbide precipitates on high temperature oxidation at 650°C in 0.5% SO2 atmosphere. Cold-rolled Fe-16Cr-0.2C material was heat-treated to obtain two additional microstructures. After exposure to hot and reactive gases for 10 h < t < 1000 h layer thicknesses and microstructure of oxide scales are observed by scanning electron microscopy and Energy-dispersive X-ray spectroscopy. The two heat treated alloys showed reasonable oxidation resistance after 1000 h of exposure. The oxidation rate was substantially higher for the alloy with a duplex matrix after heat treatment compared to the fine-grained material.
The fundamental impact of sulfur and water on corrosion rates and potential failure of the exposed material is well known. However, the access to the related corrosion mechanism causing material degradation is often a problem to solve. This study investigates the effect of SO2 and water vapor in the initial stages of corrosion of an Fe9Cr0.5Mn model alloy at 650 °C in situ. The analysis was carried out under laboratory conditions using energy-dispersive X-ray diffraction (EDXRD).
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.
Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, with associated potential gains in performance and efficiency. However, high magnitude residual stresses (RS) are often a product of the rapid thermal cycles typical of the layerwise process. Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterisation of these RS is essential for safety related engineering application and supports the development of reliable numerical models. Diffraction-based methods for RS analysis using neutrons and high energy X-rays enable non-destructive spatially resolved characterisation of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys as a function of process parameters. In addition, the challenges posed by the textured and hierarchical microstructures of LPBF materials on diffraction-based RS analysis in AM materials will be discussed. This will include the question of the d0 reference lattice spacing and the appropriate choice of the diffraction elastic constants (DECs) to calculate the level of RS in LPBF manufactured alloys.
Entwicklung der Mikrostruktur der mechanischen Eigenschaften und der Eigenspannungen in L-PBF 316L
(2022)
Die additive Fertigung (AM) metallischer Werkstoffe mittels Laser Powder Bed Fusion (L-PBF) ermöglicht einzigartige hierarchische Mikrostrukturen, die zu Verbesserungen bestimmter mechanischer Eigenschaften gegenüber konventionell hergestellten Varianten derselben Legierung führen können. Allerdings ist das L-PBF-Verfahren häufig durch das Vorhandensein hoher Eigenspannungen gekennzeichnet, die es zu verstehen und zu mindern gilt. Daher ist das Verständnis der Mikrostrukturen, der Eigenspannungen und der daraus resultierenden mechanischen Eigenschaften entscheidend für eine breite Akzeptanz bei sicherheitskritischen Anwendungen. Die BAM hat ein multidisziplinäres Forschungsprogramm gestartet, um diese Aspekte bei LPBF 316L zu untersuchen. Der vorliegende Beitrag stellt einige der wichtigsten Ergebnisse vor: der Einfluss von Prozessparametern auf die Mikrostruktur, der Einfluss von Mikrostruktur und Textur auf die Festigkeit, Kriechverhalten und Schädigung und die Stabilität von Eigenspannungen und Mikrostruktur unter Wärmebehandlungsbedingungen.
In this study an approach for dressing metallic bonded honing stones with hard cutting grains on the basis of electrolysis is investigated. By a combination of concepts from electrochemical machining (ECM) and electropolishing a test rig was designed and put into operation. In general, it can be stated that the Approach investigated in this paper has proved to be a suitable dressing method for honing stones. However, the dressing result is highly dependent on bond components, cutting grain size and concentration which lead to local differences in the material removal and irregular topographies. This could be overcome, for example, by setting the dressing parameters more precisely based on the best results presented in this paper.
The first documentation of fuel biodeterioration dates back to the late 19th century. However, extensive studies concerning the microbial fuel contamination started in 1980’s. Polymeric fuel storage tanks containing diesel and biodiesel provide environmental conditions for microbial growth. Several studies demonstrated that bacteria, which were found in contaminated fuel systems, can use fuels as macronutrient; but such bacteria can also cause microbiologically influenced corrosion and fouling.
The aim of this study is to investigate the initial attachment behavior of bacteria, isolated from a diesel contamination, on neat and photooxidized high-density polyethylene (PE-HD). Two common PE-HD’s, less- and biodiesel-stabilized, were radiated to UV light representing a tank exposed to sunlight. The effect of photooxidiation on PE-HD’s surface were characterized chemically by Fourier-transform infrared spectroscopy (FTIR). The attached bacteria Pseudomonas aeruginosa and Bacillus subtilis on the polymer surface were evaluated by fluorescence microscopy and colony-forming unit tests (CFU).