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- bone (1)
- carbon steel (1)
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- multi scale testing (1)
- oxidation (1)
- particle size determination (1)
- pitting corrosion (1)
- sample preparation (1)
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Organisationseinheit der BAM
- 5 Werkstofftechnik (781)
- 5.2 Metallische Hochtemperaturwerkstoffe (211)
- 5.1 Mikrostruktur Design und Degradation (205)
- 5.4 Multimateriale Fertigungsprozesse (157)
- 5.6 Glas (107)
- 5.3 Polymere Verbundwerkstoffe (95)
- 5.5 Materialmodellierung (71)
- 8 Zerstörungsfreie Prüfung (71)
- 7 Bauwerkssicherheit (61)
- 9 Komponentensicherheit (60)
The influence of prestraining on the aging response of an Al-Cu-Li alloy is investigated by preparation of different strain states (3 %, 4 %, 6 %) of the initial aging state. The Brinell hardness of the subsequently aged samples (up to 60 h aging time) was measured and it was found that the increasing dislocation concentration in the 3 different initial states leads to faster hardness increases and slightly higher maximum hardness.
The influence of prestraining on the aging response of an Al-Cu-Li alloy is investigated by preparation of different strain states (3 %, 4 %, 6 %) of the initial aging state. The Brinell hardness of the subsequently aged samples (up to 60 h aging time) was measured and it was found that the increasing dislocation concentration in the 3 different initial states leads to faster hardness increases and slightly higher maximum hardness.
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.
Ceramic springs offer versatile possibilities for load bearing or sensor applications in challenging environments. Although it may appear unexpected, a wide range of spring constants can be implemented by material selection and especially by the design of the spring. Based on a rectangular cross-section of the windings, it is possible to design a spring geometry that generates the desired spring constant simply by choosing appropriate diameter, height, widths, and number of windings. In a recent research project the calculation of helical compression springs made of rectangular steel (German standard DIN 2090) was applied for the design of ceramic springs. A manufacturing technology has been worked out to fabricate such springs from hollow cylinders of several highly dense technical ceramics by milling. Ceramic springs with precise rectangular section, without edge damage, and mean surface roughness smaller than 0.2 µm were produced after parameter optimization. Tolerances of less than 10 µm were achieved regarding spring diameter, height, and width of cross section. It is shown that the calculations outlined in the standard are valid for a variety of ceramic materials as well. Demonstrator springs with a wide range of spring constants have been fabricated, including zirconia springs with 0.02 N/mm, alumina springs with 1 N/mm and Si3N4 springs with 5 N/mm. A reproducibility study of six zirconia springs with a constant of 0.3 N/mm showed a relative difference in spring constants of less than +/- 1 %. This combination of a valid calculation approach for spring geometry and a reliable manufacturing technology allows for purposeful development and fabrication of ceramic springs with precise mechanical properties and superior chemical stability.
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.
Electrochemical deposition of polyaniline on carbon steel for corrosion study in geothermal solution
(2019)
Polyaniline has been widely developed for many applications, e.g. sensor, supercapacitor components, electrochromic devices, and anticorrosion pigments. Although the addition of polyaniline pigment in organic coatings has been an alternative for corrosion protection in industrial applications, the protection mechanism is still not fully understood. Herein in this study, as a part of the development of polyaniline/silicon dioxide coating for geothermal application, polyaniline has been deposited electrochemically on carbon steel surface in oxalic acid medium and tested in geothermal solution to understand the contribution of polyaniline to the corrosion protection of a polyaniline-based composite in the geothermal system. To observe the surface/interface reaction between the electrolyte and electrode surface during the electrochemical polymerization, electrochemical impedance spectroscopy (EIS) was applied after each cycle. For corrosion study in the geothermal application, an artificial geothermal solution was used with the composition of 1,500 mg/l Cl⁻, 20 mg/l SO₄²⁻, 15 mg/l HCO₃⁻, 200 mg/l Ca²⁺, 250 mg/l K⁺, and 600 mg/l Na⁺, and pH 4 to simulate a geothermal brine found in Sibayak, Indonesia. An electrochemical measurement was performed by monitoring the open circuit potential over seven days, with the interruption by EIS every 22 hours. The experiments were performed at room temperature and 150 °C (1 MPa) in an oxygen-free environment. Impedance spectra showed a reduction of the total impedance value of approximately 10 times for specimens measured at 150 °C compared to the specimens measured at room temperature, suggesting a less stable layer at high temperature.
At high temperatures and in harsh environments ceramic springs are often superior to metallic ones and allow for innovative solutions. A further application was proposed by using ceramic springs as capacitive force sensor. Lower and upper coil surfaces are coated by electrically conducting layers. Deformation of such spring results in a change of capacity. Sensor application calls for helical springs with rectangular cross-section, a linear stress-strain characteristic over entire deformation range and low manufacturing tolerances relating to inner and outer diameter, coil cross section and spring pitch. Furthermore, complex spring design with integrated connecting elements has to be realized.
Alumina, zirconia (Y-TZP) and silicon nitride springs were produced by hard machining starting from sintered hollow cylinders. After external and internal cylindrical grinding the hollow cylinders were filled with hard wax, followed by multi-stage cutting of spring coils with custom-made cutting discs. Finally, hard wax was removed by melting and burnout. Best surface and edge qualities of springs were reached using Y-TZP material and hot isostatic pressed alumina. Y-TZP springs produced with material-specifically selected cutting discs and optimized process parameters show sharp coil edges without spallings and mean roughness values of inner surfaces < 0.2 μm. Manufacturing tolerances of spring diameters, spring pitch, height and width of coil cross section are in the range of ± 10 microns. Good reproducibility of spring geometry by optimized hard machining technology allows for production of Y-TZP springs with spring constants differing less than ± 1 % within a series.
According to DIN 2090 spring constant for rectangular coil cross section is proportional to the square of height and width of coil cross section and indirectly proportional to number of active coils and to the cube of the mean spring diameter. Hence, spring constants can be tailored over a range of many orders of magnitude by changing the spring dimensions. Good agreement was reached between calculated target spring constants and measured values on produced springs.
Alumina and zirconia springs were characterized relating to deformation behavior under dynamic compression load with various deformation speeds and under static tensile loads over long periods of time. Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs was proved in both test series. It is supposed, that pseudoelasticity caused by stress-induced transformation of tetragonal to monoclinic phase is responsible for this special feature of TZP springs. Therefore, TZP material cannot be used for capacitive spring sensors.
Crack healing in glass ceramic solid oxide fuel cell (SOFC) sealants is of utmost importance as cracks caused by thermal cycling remain a bottleneck in developing durable SOFC. Whereas no or low crystal volume fraction seems most favorable for viscous crack healing, it does not for load bearing and undesired diffusion. On the other hand, crystals or filler particles can make the sealant less prone to these disadvantages but it could increase the effective composite viscosity and retard crack healing.
Against this background, the influence of crystal volume fraction, phi, on viscous crack healing in glass matrix composites prepared from soda lime silicate glass and zirconia filler particles was studied. Vickers indention induced radial cracks were healed isothermally during interrupted annealing steps and monitored with optical microscopy. Due to the slow crystallization of the glass under study, phi could be kept constant during crack healing.
For bulk glass samples (phi = =), the decrease in radial crack length was retarded by an initial increase in crack width due to crack rounding. Up to phi = 0.15 the increase in effective viscosity retarded this crack broadening thereby yielding faster crack healing. For phi > 0.15, crack broadening was progressively suppressed but the same was true for crack healing, which was fully prevented above phi = 0.3. Results indicate that optimum micro structures can prevent crack broadening limited by the global effective composite viscosity and this way promote crack healing limited by local glass viscosity.
Within the perspective of increasing reliability of AM processes, real-time monitoring allows part inspection while it is built and simultaneous defect detection. Further developments of real-time monitoring can also bring to self-regulating process controls. Key points to reach such a goal are the extensive research and knowledge of correlations between sensor signals and their causes in the process.
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.
Der Aufbau der Werkstoffe wird durch Merkmale wie Bindungsart, atomare Strukturen, Kristallstrukturen einschließlich ihrer Gitterbaufehler, Körner und Phasen bestimmt. Die Mikrostruktur (Gefüge) stellt den Verbund der Kristalle, Phasen und Gitterbaufehler auf mikroskopischer und nanoskopischer Skala dar. Die Grundlagen der Phasenumwandlungen werden behandelt und die Bedeutung von Diffusionsprozessen erläutert. Werkstoffe sind bedeutend für Kultur, Wirtschaft, Technik und Umwelt. Ihre Herstellung benötigt Ressourcen und Energie. Recycling ist eine Möglichkeit zur Erhöhung der Ressourcenproduktivität.
Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity.
Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. In this presentation, I summarized of the first 15 months the whole project. In this period, the basic crack propagation theory for neat polymers is established and the special fracture experiment sample is prepared and tested at room temperature. In addition, the model of the specimen is first established.
Crack propagation in polymers: Separation of surface energy and irreversible deformation energy
(2019)
Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity.
Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. This poster is the summary of the first part of the whole project. In the first part, the basic crack propagation theory for neat polymers is established and the special fracture experiment sample is prepared and tested at room temperature. In addition, the fracture experiment at room temperature is validated numerically.
Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity.
Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. The fracture tests include the conventional tensile test, the macroscopic peel test and the single fiber peel – off test.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
Die Metal Magnetic Memory (MMM) Methode ist ein standardisiertes, zerstörungsfreies Prüfverfahren, das für die Detektion von lokal geschädigten Materialbereichen in ferromagnetischen Bauteilen oder Proben verwendet wird. Es basiert auf der Annahme lokaler magnetoelastischer Wechselwirkungen an Spannungskonzentrationsstellen, die schwache magnetische Streufelder an den geschädigten Prüfkörperoberflächen hervorrufen. Die MMM-Methode überträgt dabei die für einachsige und elastische Verformungen entwickelten magnetoelastischen Modellvorstellungen ohne weitere Anpassungen in den Schädigungskontext, der jedoch mehrachsige Beanspruchungen und elastisch-plastische Deformationsprozesse erwarten lässt. Das Ziel der Arbeit ist es daher, die gängigen MMM-Hypothesen zur Signalentstehung fach- und skalenübergreifend und unter stärkerer Berücksichtigung mechanischer und mikrostruktureller Aspekte zu überprüfen.
Zu diesem Zweck wurden zum einen gekerbte Flachzugproben aus einem unlegierten Baustahl inhomogen elastisch-plastisch verformt und die entstehenden magnetischen Streufelder an deren Oberflächen mit einem Drei-Achsen-GMR-Magnetometer detektiert. Die so ermittelten Magnetfeld-verteilungen wurden für unterschiedliche Verformungszustände ortsaufgelöst und richtungsabhängig mit gemessenen Dehnungsverteilungen (digitale Bildkorrelation) und mit simulierten Lastspannungs-verteilungen korreliert. Die eingeschnürten Probenbereiche wurden zusätzlich topographisch mittels Streifenlichtprojektion und Weißlichtinterferenzmikroskopie vermessen, um den Magnetisierungs-prozess ebenfalls vor dem Hintergrund geometrischer Effekte diskutieren zu können.
Um systematische, verformungsinduzierte Veränderungen der magnetischen Mikrostruktur (magnetischer Domänen) im polykristallinen, quasi-isotropen Material nachzuweisen, wurde zum anderen ein in dieser Arbeit entwickelter statistischer Ansatz der Domänenanalyse angewandt. Hierfür wurde das Material zunächst durch Härteeindrücke mehrachsig elastisch-plastisch verformt, und die verformten Probenbereiche wurden anschließend mit Hilfe der Bitterstreifentechnik hauptsächlich bei niedriger Vergrößerung lichtmikroskopisch untersucht. Die beobachteten makroskopischen Domänen-kontraste wurden über ein analytisches, kontaktmechanisches (ECM-) Modell und über Makro-Eigen-spannungsmessungen (energiedispersive Synchrotron-Beugungsuntersuchungen) charakteristischen Verformungszonen unter den Härteeindrücken zugeordnet.
Die Ergebnisse dieser Untersuchungen belegen, dass die Entstehung der Streufelder – entgegen bisheriger Annahmen – nicht allein auf mechanische Spannungs- und Verformungsgradienten im Material zurückzuführen, sondern auch topographisch bedingt ist. Die Vernachlässigung überlagerter geometrischer Effekte kann zu sicherheitsrelevanten Fehlinterpretationen der magnetischen Signale führen. Einachsige magnetoelastische Modellvorstellungen sollten zudem nicht ohne Anpassungen auf komplexe Beanspruchungen übertragen werden, da u. a. sowohl mechanische Größen (wie Spannungen oder Dehnungen) als auch mikrostrukturelle Parameter (wie z. B. Versetzungsdichten) bei komplexen Belastungen als ortsabhängige Variablen behandelt werden müssen. Die in dieser Arbeit beobachteten Domänenkontraste lassen sich zweifelsfrei charakteristischen Verformungszonen zuordnen, mikro-strukturell jedoch nicht allein mit anzunehmenden Gradienten der Versetzungsdichte erklären. Statt-dessen entstehen beispielsweise lokale Verformungstexturen, die zusätzliche magnetische Anisotropien bewirken könnten. Da bisher weder die makroskopischen noch die mikrostrukturellen Ursachen der Streufeldentstehung hinreichend verstanden sind, scheint die MMM-Methode für die quantitative Bewertung des Schädigungszustands derzeit ungeeignet.
A continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from statictests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. A multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed.
Depending on the CO2 generating and the capture process as well as on consecutive purification steps applied, CO2 streams from different emitters may differ in their composition. When CO2 streams with different compositions are fed into a larger pipeline network, there are several aspects that must be considered: i) chemical reactions, such as acid formation, may occur within the joint CO2 stream; ii) there may be a variation of mass flow rate and CO2 stream composition within the pipeline network if the feed-in behavior of different CO2 sources changes with time. Potential impacts of changing CO2 stream compositions and mass flow rates in CCS cluster systems were investigated in the collaborative project "CLUSTER" (see also www.bgr.bund.de/CLUSTER). In this presentation, we focus on the experimental investigations of formation and condensation of strong acids and their impacts on the corrosion of pipeline steels. When SO2, NO2, O2 and H2O are present simultaneously in CO2 streams chemical cross-reactions may occur leading to the formation of strong acids such as sulfuric and nitric acid. To prevent this acid formation the concentration of at least one of these four impurities must be kept very low (e.g., Rütters et al., 2016). At temperatures below the acid dew point temperature, acids will condense, e.g., on pipeline steel surfaces. In turn, these acid condensates may trigger steel corrosion. To better understand the process of acid formation and condensation and its implications for steel corrosion, exposure tests were performed on pipeline steel X70 in dense CO2 with varying SO2, NO2 and O2 concentration under high pressure and at 278 K in an observable autoclave, in which water was added as droplets or as vapor. Further, electrochemical tests were carried out with X70 specimens immersed in 500 mL CO2-saturated synthetic condensate solution or in droplets of the same solution on the specimen’s surface. Depending on impurity concentrations in the CO2 streams, condensates consisting of different relative amounts of nitric and sulfuric acid were formed. In condensates containing both nitric and sulfuric acid, corrosion rates were higher than the sum of those of the individual acids. In addition, corrosion products and forms depended on the condensate composition. Investigations of water droplets on steel surfaces in impurity-containing dense-phase CO2 revealed the diffusion of SO2 and NO2, followed by cross-reactions forming corresponding acids. An increase in droplet size (from 1 to 5 µl) lead to higher corrosion rates. However, in comparison to measurements in bulk solution, corrosion reactions in droplets resulted in thick, high-resistance corrosion products and observed droplet corrosion rates were significantly lower. In addition, the possibility of acid droplet formation and growth in impure liquid CO2 is influenced by the wetting behavior of the acid droplet on the steel surface. Thus, the contact angle between a water droplet and the surface steel specimens in a CO2 atmosphere was investigated in a high pressure view cell following the sessile drop method. The contact angle wasand found to be larger at higher CO2 pressures (studied from 5 to 20 MPa) and at higher temperatures (e.g. 278 K to 333 K). Further, measured contact angles were larger on rough than on smooth metal surfaces. In addition, acid formation reduced the contact angle, i.e. lead to better wetting, thereby stimulating condensation that was followed by a corrosion process. These detailed insights on the complex interplay of acid formation, condensation, wetting behavior and corrosion allow a better assessment of material suitability for pipeline transportation of impure CO2 streams
Environmental conditions are known to influence sub-critical crack growth (SCCG) that starts from microscopic flaws at the glass surface, leading to stress corrosion phenomena at the crack tip. The processes at the crack tip are complex and water has been identified as a key component governing SCCG at low crack velocities (region I). In particular, the influence of humidity accelerating crack propagation is well studied for dry industrial soda-lime silicate glasses (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG in water-bearing glasses. For this purpose, water-bearing silicate glasses of up to 8 wt% total water were synthesized in an internally heated pressure vessel at 0.5 GPa and compared to dry glasses. SCCG was measured using the double cantilever beam technique. For dry glasses, three trends in the crack growth velocity versus stress intensity, KI, curve were found. The slope in region I, limited by environmental corrosion, increases in the order soda-lime silicate < sodium borosilicate < barium calcium silicate < sodium zinc silicate < sodium aluminosilicate glass. The velocity range of region II, reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among these glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg relaxation peak caused by molecular water, and makes the glasses more prone to SCCG. The observed trends will be discussed in terms of the effects of Youngs Modulus on strain energy release rate and energy dissipation related to glass relaxation phenomena.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
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).
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.
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.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
The ProboStat is a multi-purpose measurement cell suitable for various electrical and physical measurements under different atmospheres and at high temperatures. Disc and bar shaped samples are sandwiched between platinum electrodes at the top of the tubular cell. The gas tight assembly can be inserted into a furnace. Different gases can be flushed through the tube. For this study, a ProboStat was adapted to measure volume resistivity of ceramic insulators at high temperatures according to standards.
The standardized measurement of volume resistivity of ceramic insulators requires the consideration of many specifications including sample diameter, thickness, electrode design, and the proportion of these characteristics. Measurements are ideally performed in a state of dielectric equilibrium. The time-related slope of resistivity of a specific sample follows a power function. Thus, care must be taken when choosing a charge time or defining the duration of a measurement. As fringing of the guarded electrode occurs under high voltage, the effective electrode area for evaluation of the results should be corrected with respect to sample thickness and electrode design. The demands of effective standards on sample geometry and electrode design are stricter for room temperature measurements than for high temperature measurements.
To perform high temperature measurements on ceramic samples that also fulfill the demands on room temperature measurements, a ProboStat was equipped with a dedicated large sample setup for discs with diameters of up to 60 mm. The volume resistivity of different alumina samples was first measured at room temperature in a standard test fixture and then compared to results obtained with the ProboStat. All measurements were performed for at least 100 min using a 26 mm guarded electrode. High temperature measurements at 500 °C were performed using the same samples. Room temperature values obtained with the standard test fixture are in the order of 10^17 Ohm·cm. The quantitative effect of electrode area correction is presented. Practical issues related to the use of the multi-purpose cell are addressed. These include electrode material selection, application of electrodes, and compensation of leakage currents. High temperature results of volume resistivity of the different alumina samples are presented. The validity is discussed with respect to the suitability of the multi-purpose cell for such measurements.
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.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals.
The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions.
First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur.
Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals.
For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size.
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
The project ProMoAM is presented. The goal of the project is to evaluate which NDT techniques or combination of techniques is suited for in-situ quality assurance in additive manufacturing of metals. To this end, also 3d-data fusion and visualization techniques are applied. Additional ex-situ NDT-techniques are used as references for defect detection and quantification. Feasability studies for NDT-techniques that are presently not applicable for in-situ use are performed as well.
The presentation gives a brief overview of the whole project and the different involved NDT-techniques.
Despite of the significant advances in additive manufacturing (AM) process optimization there is still a lack of experimental results and understanding regarding the mechanical behavior and its relationship with the microstructural features of AM-parts, especially in loading conditions typical for safety-relevant applications. Within the scope of the presented ongoing investigations, a basic microstructural characterization, tensile tests at room and elevated temperature (400°C) as well as a characterization of the fatigue behavior of additively manufactured Ti-6Al-4V in the low cycle fatigue regime are carried out in the as-built state. After failure, different techniques are used to describe the failure mechanisms of the specimens. The AM-Specimens are provided by the Fraunhofer institute for production systems and design technology and investigated at the BAM following the philosophy of the TF-Project AGIL.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2019)
This work aims for a yield function description of additively manufactured parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures. From virtual experiments, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation.
Druckbehälter werden vor ihrer Inbetriebnahme obligatorisch einer hydraulischen Prüfung bis zum sog. Prüfdruck belastet. Damit sollen fehlerhaft gefertigte Individuen erkannt und ausgesondert werden. Mit dieser Prüfung werden aber auch diejenigen Einzelbehälter ausgesondert, die ohne einem nachvollziehbaren Fertigungsfehler, nur auf Basis der statistischen Streuung ggf. eine Festigkeit unterhalb des Prüfdrucks aufweisen.
Da der Prüfdruck im Fall der Wasserstoffspeicher mindestens 20% über dem maximal zulässigem Betriebsdruck liegt, wäre damit ein Versagen im Betrieb ausgenommen, gäbe es die verschiedenen Alterungs- bzw. Ermüdungseffekt nicht.
Um den Einfluss der erstmaligen Prüfung auf eine angenommene ausfallfreie Zeit bewerten zu können, wird hier die Alterung und die erstmalige Prüfung in Kombination analysiert. Hierzu wird auf Basis der Restfestigkeitsdaten aus einer umfangreichen Prüfkampagne ein Ansatz für die Beschreibung der Alterung ermittelt und auf andere Lastzustände übertragen.
So kann für das Baumuster, das der o.g. Prüfkampagne zugrunde lag, mithilfe einer Monte-Carlo-Simulation gezeigt werden, dass mindestens 10.000 LW vor einem ersten Alterungsversagen mit 1 aus 1 Mio. In Abhängigkeit der Anzahl der Individuen, die bei der erstmaligen Prüfung versagen, und der Streuung der gesamten Population, kann diese Mindestfestigkeit auf realistisch 50.000 Lastwechsel steigen.
Damit ist gezeigt, dass aufgrund der erstmaligen Prüfung eine Mindestfestigkeit erzeugt wird, die stark vom Alterungsverhalten abhängt. Im Ergebnis heißt dies, dass in den Vorschriften aktuell die Bedeutung des Mindestberstdrucks in der Baumusterprüfung überschätzt und die möglichst betriebsbegleitende Erfassung der Alterung unterschätzt sind.
At high temperatures and in harsh environments ceramic springs are often superior to metallic springs and allow for innovative solutions. A recently proposed application involves ceramic springs with metallized surfaces as capacitive force sensor. A strictly linear stress-strain characteristic of the spring is a precondition for such a sensor.
Helical ceramic springs with rectangular cross-section have been produced from sintered hollow cylinders. Alumina, ATZ, Y-TZP, and Ce-TZP springs with identical dimensions were characterized and compared regarding deformation behavior.
Spring deformation was investigated under various load scenarios.
Dynamic compression was performed with deformation speeds from 0.3 to 30 mm/min. Spring constants of alumina springs are strain rate independent. By contrast, Y-TZP spring constant increases by approximately 3 % within the experimental framework.
A high-precision test facility was developed to characterize spring displacement in nm range under static tensile load over long periods of time. Spring elongation with asymptotic course was observed for zirconia containing materials at room temperature. This effect is particularly strong in the case of Y-TZP. Up to 0.3 % time-dependent elongation was measured after 24 h under constant load. Deformation is completely reversible after unloading. Alumina springs do not show any time-dependent deformation under identical test conditions.
Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs at room temperature was proved in both test series. It is supposed, that pseudo-elasticity caused by stress-induced phase transformation from tetragonal to monoclinic is responsible for this special behavior of TZP springs.
Dielectric breakdown of ceramics is widely believed to originate from microstructural defects. Still, there is no commonly accepted model for the origin and process of dielectric failure that covers all observed phenomena and dependencies. In analogy to mechanical strength, the Weibull distribution is commonly used to evaluate dielectric strength data. This works well for a given group of specimens with constant geometry. But unlike mechanical strength, dielectric strength scales with the inverse square root of sample thickness. This cannot be explained by the classic Weibull concept. The Griffith type energy release rate model of dielectric breakdown proposed by Schneider is based on space charge injection and conducting filaments from the sample surface. This model incorporates the distinct thickness dependence and the pronounced influence of surface defects. Based on this model and the classic Weibull probability of failure, Schneider’s group theoretically derived a probability of breakdown that predicts an increase of failure probability with increasing electrode area. In our study we tested this model with dielectric strength data measured on dense alumina samples using different electrode areas. Weibull modulus and characteristic dielectric strength (scale parameter) were determined for a set of measurements using small electrodes. These values were used to calculate the failure probability under large electrodes according to the model. The calculated data excellently fits the measured values. Thus, our experiments substantiate the assumptions made in the breakdown model and the significance of surface defects for dielectric failure.
Lifetime aspects including fatigue failure of concrete structures were traditionally only of minor importance. Because of the growing interest in maxing out the capacities of concrete, its fatigue failure under compression has become an issue. A variety of interacting phenomena such as e.g. loss of prestress, degradation due to chemical reactions or creep and shrinkage influence the fatigue resistance. Failure due to cyclic loads is generally not instantaneous, but characterized by a steady damage accumulation. Therefore, a reliable numerical model to predict the performance of concrete over its lifetime is required, which accurately captures order effects and full three-dimensional stress states.
Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales.
However, a key limitation of those models is that they generally do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles. This is due to the computational effort necessary to explicitly resolve every cycle which exceeds the currently available computational resources. The limitation can only be overcome by the application of multiscale methods in time.
The objective of the paper is the development of numerical methods for the simulation of concrete under fatigue loading using temporal multiscale methods.
First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from static tests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level.
Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed.
Finally, the developed methods will be validated and compared to experimental data.
If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology.
This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution.
Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat.
Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods.
Die BAM ist nahezu über die gesamte Wertschöpfungskette hinweg wissenschaftlich tätig. Von der sicheren und effizienten Wasserstofferzeugung (POWER-to-GAS), über die (Zwischen-)Speicherung von Wasserstoff in Druckgasspeichern bis hin zum Transport bspw. mittels Trailerfahrzeug zum Endverbraucher.
Komplettiert werden die Aktivitäten der BAM durch die sicherheitstechnische Beurteilung von wasserstoffhaltigen Gasgemischen, die Verträglichkeitsbewertung von Werkstoffen bis hin zur Detektion von Wasserstoffkonzentrationen über geeignete Sensorik, auch mittels ferngesteuerter Messdrohnen (sog. UAV-Drohnen).
Zudem untersucht die BAM proaktiv Schadensrisiken und Unfallszenarien für die Sicherheitsbetrachtung, um mögliche Schwachstellen aufzeigen und potenzielle Gefährdungen erkennen zu können.
This work examined the factors that influence the droplet corrosion of CO2 pipeline steels caused by oxyfuel flue gases in dense phase CO2 at 278 K, simulating the underground transport conditions. The wetting properties were studied by contact angle measurement, revealing pH and time dependency on the reactive wetting behaviors of carbon steel X70. Exposure tests with CO2 saturated water droplet on steel surface showed that the impurities (220 ppmv SO2 and 6700 ppmv O2) diffused into the droplet and then reacted with metal surfaces in dense phase condition, forming the corrosion products. The corrosion rate was confirmed strongly depending on the droplet volume as well as the SO2 concentration. Condensation experiments carried out on freshly polished coupons in CO2 with 200 ppmv H2O, 220 ppmv SO2 and 6700 ppmv O2, showed that the formation and aggregation of droplets is time and temperature dependent. At 278 K, condensation happened stronger and the corrosion products, mainly consisted of dense hydrated FeSO3/FeSO4. While at 288 K, more fluffy corrosion products consisting of iron oxide/hydroxide and hydrated FeSO3/FeSO4 were found. Further exposure tests on carbon steel coupons with different surface roughness did not reveal the difference in weight loss/gain and therefore the corrosion rate.
Recent studies have shown that even at a very low concentration of impurities (less than 100 ppmv of SO2, NO2, O2 and H2O) the droplet formation and condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. To reveal the mechanism of droplet corrosion in dense phase CO2 at high pressure and low temperature, further studies on factors that affect wettability and resulting corrosion behaviors of transport pipeline steels are needed. In this study, effects of surface morphology were investigated by varying surface roughness of carbon steel coupons exposed to CO2 stream containing impurities to measure the wettability by contact angle and to observe the condensation as well as possible droplet corrosion that followed. Other considered factors were: pH of the droplet, temperature, droplet volume, and exposure time.
Considerations for nanomaterial identification of powders using volume-specific surface area method
(2019)
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming.
For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods.
Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions).
In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful.
One of the measurement methods well suited to probe the size of particulate powder is the determination of the volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer, which can be used for SLM or for 3DP. This technique offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and is capable of producing parts with physical and mechanical properties comparable to traditionally shaped parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles. Another technology, the Gas Flow Assisted Powder Deposition, can increase the stability of the powder bed and the packing density, even in extreme conditions such as in absence of gravitational forces.