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Paper des Monats
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Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation-based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
Iron Oxide Nanocubes as a New Certified Reference Material for Nanoparticle Size Measurements
(2023)
The rational design and increasing industrial use of nanomaterials require a reliable characterization of their physicochemical key properties like size, size distribution, shape, and surface chemistry. This calls for nanoscale reference materials (nanoRMs) for the validation and standardization of commonly used characterization methods closely matching real-world nonspherical nano-objects. This encouraged us to develop a nonspherical nanoRM of very small size consisting of 8 nm iron oxide nanocubes (BAM-N012) to complement spherical gold, silica, and polymer nanoRMs. In the following, the development and production of this nanoRM are highlighted including the characterization by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) as complementary methods for size and shape parameters, homogeneity and stability studies, and calculation of a complete uncertainty budget of the size features. The determination of the nanocubes’ edge length by TEM and SAXS allows a method comparison. In addition, SAXS measurements can also provide the mean particle number density and the mass concentration. The certified size parameters, area equivalent circular diameter and square edge length, determined by TEM with a relative expanded uncertainty below 9%, are metrologically traceable to a natural constant for length, the very precisely known (111) lattice spacing of silicon. Cubic BAM-N012 qualifies as a certified nanoRM for estimating the precision and trueness, validation, and quality assurance of particle size and shape measurements with electron microscopy and SAXS as well as other sizing methods suitable for nanomaterials. The production of this new iron oxide nanocube RM presents an important achievement for the nanomaterial community, nanomaterial manufacturers, and regulators.
Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics.
A technical-safety evaluation of the detonation effects of pyrotechnic compositions can be performed on the basis of TNT/PETN equivalence. The equivalence determination can be carried out by characterization of the blast wave generated because of detonation in free field tests, which however can be highly resource intensive and prone to uncertainties. Here, we present underwater ‘small-scale’ experiments for the determination of such equivalents.
Underwater experiments, as described in the European standard EN 13763-15:2004, are performed to test the capability of detonators to initiate secondary explosives by determining the released energy. At BAM this test was modified to compare the energy output of the pyrotechnic mixtures (those used in air bag gas generators and firework flash compositions) and thus to determine their equivalents of high explosives like TNT or PETN. In the modified tests, small cylindrical copper containers were filled with pyrotechnic substances, which were then attached to standard detonators. This explosive charge assembly was then lowered into a water tank of about 1000 l capacity. At the same depth as the charge assembly, a piezoelectric pressure sensor was immersed in the water at a horizontal distance of about 400 mm from the charge. By recording the time-dependent pressure during the test, the shock energy as well as the energy associated with the expanding gas bubble were determined.
The embrittlement of metallic alloys by liquid metals leads to catastrophic material failure and severely impacts their structural integrity. The weakening of grain boundaries by the ingress of liquid metal and preceding segregation in the solid are thought to promote early fracture. However, the potential of balancing between the segregation of cohesion-enhancing interstitial solutes and embrittling elements inducing grain boundary decohesion is not understood. Here, we unveil the mechanisms of how boron segregation mitigates the detrimental effects of the prime embrittler, zinc, in a Σ5 [0 0 1] tilt grain boundary in α −Fe (4 at.% Al). Zinc forms nanoscale segregation patterns inducing structurally and compositionally complex grain boundary states. Ab-initio simulations reveal that boron hinders zinc segregation and compensates for the zinc induced loss in grain boundary cohesion. Our work sheds new light on how interstitial solutes intimately modify grain boundaries, thereby opening pathways to use them as dopants for preventing disastrous material failure.
The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode.
This presentation summarizes outcomes of the CUSP projects POLYRISK and PlasticsFatE according to thermoanalytical methods.It highlights the importants of analytical methods to measure physical and chemical properties of the test materials. These informations are neccessary for interpretation of the toxicological test results.
Material Selection Strategy
(2023)
Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate
(2023)
Microplastics are everywhere in the environment, but analytics is challenging. Since harmonisation is missing as well es suitable reference materials, BAM did under th umbrella of VAMAS funded by the EU Horizon 2020 project PlasticsFate a ILC for microplastic detection methods. Methods adressed were IR, Raman, Py-GC/MS and TED-GC/MS. The talk gives a first presentation and evaluation on the results.
In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other.
In recent years, the use of simulation-based digital twins for monitoring and assessment of complex mechanical systems has greatly expanded. Their potential to increase the information obtained from limited data makes them an invaluable tool for a broad range of real-world applications. Nonetheless, there usually exists a discrepancy between the predicted response and the measurements of the system once built. One of the main contributors to this difference in addition to miscalibrated model parameters is the model error. Quantifying this socalled model bias (as well as proper values for the model parameters) is critical for the reliable performance of digital twins. Model bias identification is ultimately an inverse problem where information from measurements is used to update the original model. Bayesian formulations can tackle this task. Including the model bias as a parameter to be inferred enables the use of a Bayesian framework to obtain a probability distribution that represents the uncertainty between the measurements and the model. Simultaneously, this procedure can be combined with a classic parameter updating scheme to account for the trainable parameters in the original model. This study evaluates the effectiveness of different model bias identification approaches based on Bayesian inference methods. This includes more classical approaches such as direct parameter estimation using MCMC in a Bayesian setup, as well as more recent proposals such as stat- FEM or orthogonal Gaussian Processes. Their potential use in digital twins, generalization capabilities, and computational cost is extensively analyzed.
In recent years, the use of simulation-based digital twins for monitoring and assessment of complex mechanical systems has greatly expanded. Their potential to increase the information obtained from limited data makes them an invaluable tool for a broad range of real-world applications. Nonetheless, there usually exists a discrepancy between the predicted response and the measurements of the system once built. One of the main contributors to this difference in addition to miscalibrated model parameters is the model error. Quantifying this socalled model bias (as well as proper values for the model parameters) is critical for the reliable performance of digital twins. Model bias identification is ultimately an inverse problem where information from measurements is used to update the original model. Bayesian formulations can tackle this task. Including the model bias as a parameter to be inferred enables the use of a Bayesian framework to obtain a probability distribution that represents the uncertainty between the measurements and the model. Simultaneously, this procedure can be combined with a classic parameter updating scheme to account for the trainable parameters in the original model.
This study evaluates the effectiveness of different model bias identification approaches based on Bayesian inference methods. This includes more classical approaches such as direct parameter estimation using MCMC in a Bayesian setup, as well as more recent proposals such as stat-FEM or orthogonal Gaussian Processes. Their potential use in digital twins, generalization capabilities, and computational cost is extensively analyzed.
Lanthanide-based, spectrally shifting, and multi-color luminescent upconverting nanoparticles (UCNPs) have received much attention in the last decades because of their applicability as reporter for bioimaging, super-resolution microscopy, and sensing as well as barcoding and anti-counterfeiting tags. A prerequisite for the broad application of UCNPs in areas such as sensing and encoding are simple, robust, and easily upscalable synthesis protocols that yield large quantities of UCNPs with sizes of 20 nm or more with precisely controlled and tunable physicochemical properties from lowcost reagents with a high reproducibility. In this context, we studied the reproducibility, robustness, and upscalability of the synthesis of β-NaYF4:Yb, Er UCNPs via thermal decomposition. Reaction parameters included solvent, precursor chemical compositions, ratio, and concentration. The resulting UCNPs were then examined regarding their application-relevant physicochemical properties such as size, size distribution, morphology, crystal phase, chemical composition, and photoluminescence.
Based on these screening studies, we propose a small volume and high-concentration synthesis approach that can provide UCNPs with different, yet controlled size, an excellent phase purity and tunable morphology in batch sizes of up to at least 5 g which are well suited for the fabrication of sensors, printable barcodes or authentication and recycling tags.
FenicsXConcrete
(2023)
The main solidification parameters, namely the crystal axis, the growth rate, and the cross-sectional area of the columnar crystal control the primary microstructure and thus the final weld seam properties.
Limited understanding of solidification parameters due to complexities in experimental and theoretical weld pool boundary determination and
its mathematical description.
Application of local Lamé curves for efficient weld pool boundary reconstruction Derivation of general analytical solutions for the main solidification parameters of a two-dimensional columnar crystal growth during laser beam welding of thin steel sheets.
The Lamé curves approximation technique was successfully applied for the reconstruction of the rear part of the two-dimensional steady-state weld pool boundary. General analytical expressions for the main solidification parameters, namely the crystal axis, the growth rate and the cross-sectional area of the crystal were derived.
The derived expressions and herewith obtained results were verified and validated by comparing them to known theoretical solutions and experimental measurements. Dimensionless analysis of the influence of the size and shape of the rear weld pool boundary on the solidification parameters was provided.
The derived general solutions and the analysis provided allow for critical welding parameters to be estimated and adapted accordingly to improve the welding process.
A technique for calculating the main solidification parameters for a two-dimensional columnar crystal growth during complete penetration laser beam welding of thin steel sheets was developed. Given that the weld pool interface is described by Lamé curves (superellipses) within the horizontal plane of growth, general analytical solutions were derived for the geometry of the crystal axis and the corresponding growth rate and cross-sectional area of the crystal. A dimensionless analysis was performed to provide insights on the dependence of the solidification parameters on the shape and dimensions of the rear part of the weld pool boundary. The derived solutions were applied for the case of complete penetration laser beam keyhole welding of 2 mm thick 316L austenitic chromium-nickel steel sheets. It was shown that the reconstruction of the weld pool boundary with Lamé curves provides higher accuracy and flexibility compared to results obtained with elliptical functions. The validity of the proposed technique and the derived analytical solutions was backed up by a comparison of the obtained solutions to known analytical solutions and experimentally determined shapes and sizes of the crystals on the top surface of the sheet. The dimensions of the calculated crystal axis correlated well with the experimentally obtained results.
A three-dimensional numerical model was developed to accurately predict the steady-state weld pool shape in full penetration laser beam welding. The model accounts for the coupling between the heat transfer and the fluid dynamics by considering the effects of solid/liquid phase transition, thermo-capillary convection, natural convection, and phase-specific and temperature-dependent material properties up to the evaporation temperature. A fixed right circular cone was utilized as a keyhole geometry to consider the heat absorbed from the laser beam. The model was used to analyze the influence of the thermodynamic activity of solutes and turbulence on the weld pool shape. A mesh sensitivity analysis was performed on a hybrid mesh combining hexahedral and tetrahedral elements. For the case of full penetration laser beam welding of 8 mm thick unalloyed steel sheets, the dependence of the weld pool shape on the surface-active element sulfur was found to be negligible. The analysis of the results showed that a laminar formulation is sufficient for accurately predicting the weld pool shape since the turbulence has a minor impact on the flow dynamics in the weld pool. The validity of the numerical results was backed up by experimental measurements and observations, including weld pool length, local temperature history, and a range of metallographic crosssections.
Numerical study on the formation of a bulging region in partial penetration laser beam welding
(2023)
A transient three-dimensional thermo-fluid dynamics numerical model was developed to study the formation of a bulging region in partial penetration laser beam welding. The model accounts for the coupling between the fluid flow, the heat transfer, and the keyhole dynamics by considering the effects of multiple reflections and Fresnel absorption of the laser beam in the keyhole, the phase transitions during melting and evaporating, the thermo-capillary convection, the natural convection, and the phase-specific and temperature-dependent material properties up to the evaporation temperature. The validity of the model was backed up by experimentally obtained data, including the drilling time, the weld pool length, the local temperature history outside the weld pool, the process efficiency, and a range of metallographic crosssections.
The model was applied for the cases of partial penetration laser beam welding of 8 mm and 12 mm thick unalloyed steel sheets. The obtained experimental and numerical results reveal that the bulging region forms transiently depending on the penetration depth of the weld, showing a tendency to transition from a slight bulging to a fully developed bulging region between penetration depths of 6 mm and 9 mm, respectively.
The performance of titanium alloy (Ti6Al4V) surfaces was investigated in lubricated reciprocating sliding tribological tests (RSTT). Special emphasis was laid on the effect of surface nanostructures in area of contact on the respective friction and wear behaviour. These so-called laser-induced periodic surface structures (LIPSS, ripples) were produced on the titanium alloy surface upon scan processing in air by an ultrashort pulsed femtosecond (fs) laser. As lubricant served two types of base oils, a pure polyalcylene-glycol, and an SAE 0W30 oil containing only antioxidants and temperature stabilizers. Tribological tests were carried out on polished as well as LIPSS covered areas using both types of base oil. A test metrics was established, combining the additive 2-ethylhexyl-zincdithiophosphate (ZDDP) or the ionic liquid [P6,6,6,14] [DEHP] (98% purity) with the respective base oils. The test metrics also considered the orientation of motion with respect to the orientation of the structures formed on the surface. Results are presented which show that the interplay between LIPSS and the local chemistry formed by the respective additives is beneficial for the tribological behaviour of the titanium alloy. Certain combinations of base oil, additive and LIPSS reduced friction and wear significantly in the tribological contact.
The amount of absorbed energy in the keyhole as well as its spatial and temporal distribution is essential to model the laser beam welding process. The recoil pressure, which develops because of the evaporation process induced by the absorbed laser energy at the keyhole wall, is a key determining factor for the macroscopic flow of the molten metal in the weld pool during high-power laser beam welding. Consequently, a realistic implementation of the effect of laser radiation on the weld metal is crucial to obtain reliable and accurate simulation results. In this paper, we discuss manyfold different improvements on the laser-material interaction, namely, the ray tracing method, in the numerical simulation of the laser beam welding process. The first improvement relates to locating the exact reflection points in the ray tracing method using a so-called cosine condition in the determination algorithm for the intersection of reflected rays and the keyhole surface. A second correction refers to the numerical treatment of the Gaussian distribution of the laser beam, whose beam width is defined by a decay of the laser intensity by a factor of 1/e2, thus ignoring around 14% of the total laser beam energy. In the third step, the changes in the laser radiation distribution in the vertical direction were adapted by using different approximations for the converging and the diverging regions of the laser beam, thus mimicking the beam caustic. Finally, a virtual mesh refinement was adopted in the ray tracing routine. The obtained numerical results were validated with experimental measurements.
The amount of absorbed energy in the keyhole as well as its spatial and temporal distribution is essential to model the laser beam welding process. The recoil pressure, which develops because of the evaporation process induced by the absorbed laser energy at the keyhole wall, is a key determining factor for the macroscopic flow of the molten metal in the weld pool during high-power laser beam welding. Consequently, a realistic implementation of the effect of laser radiation on the weld metal is crucial to obtain reliable and accurate simulation results. In this paper, we discuss manyfold different improvements on the laser-material interaction, namely, the ray tracing method, in the numerical simulation of the laser beam welding process. The first improvement relates to locating the exact reflection points in the ray tracing method using a so-called cosine condition in the determination algorithm for the intersection of reflected rays and the keyhole surface. A second correction refers to the numerical treatment of the Gaussian distribution of the laser beam, whose beam width is defined by a decay of the laser intensity by a factor of 1/e2, thus ignoring around 14% of the total laser beam energy. In the third step, the changes in the laser radiation distribution in the vertical direction were adapted by using different approximations for the converging and the diverging regions of the laser beam, thus mimicking the beam caustic. Finally, a virtual mesh refinement was adopted in the ray tracing routine. The obtained numerical results were validated with experimental measurements.
The amount of absorbed energy in the keyhole as well as its spatial and temporal distribution is essential to model the laser beam welding process. The recoil pressure, which develops because of the evaporation process induced by the absorbed laser energy at the keyhole wall, is a key determining factor for the macroscopic flow of the molten metal in the weld pool during high-power laser beam welding. Consequently, a realistic implementation of the effect of the laser radiation on the weld metal is crucial to obtain reliable and accurate simulation results.
In this paper, we discuss manyfold different improvements on the laser-material interaction, namely the ray-tracing method, in the numerical simulation of the laser beam welding process. The first improvement relates to locating the exact reflection points in the ray tracing method using a so-called cosine condition in the determination algorithm for the intersection of the reflected rays and the keyhole surface. A second correction refers to the numerical treatment of the Gaussian distribution of the laser beam, whose beam width is defined by a decay of the laser intensity by a factor of 1/e2 thus ignoring around 14 % of the total laser beam energy. In a third step, the changes in the laser radiation distribution in the vertical direction were adapted by using different approximations for the converging and the diverging regions of the laser beam thus mimicking the beam caustic. Finally, a virtual mesh refinement was adopted in the ray tracing routine. The obtained numerical results were validated with experimental measurements.
A steel pipeline segment of 2.5 m length was subjected to quasi-static four-point bending load in three steps for studying the initial cracking and damage accumulation based on the Acoustic Emission (AE) technique and by the direct current potential drop (DCPD) technique. For the latter, a new post-test analysis method was established.
AE is found more sensitive to crack initiation than DCPD. Formation of mesoscopic and macroscopic cracks as well as their closure and the resulting friction generate weighted peak frequencies below 400 kHz, whereas microscopic cracking produces AE with broad band spectra identifiable by weighted peak frequencies above 400 kHz. Critical states alike the maximum load level and the leak opening were accompanied by peak amplitudes above 85 dBAE. This rather fundamental study provides a data base for possibly developing advanced strategies of detection and alarm systems based on acoustic monitoring of pipelines, or at least, steel structures.
Since there is a continuously growing demand for complex, frequently heavy-sectioned spheroidal graphite cast iron (SGI) castings it is worth paying attention to the chunky graphite (CHG) degeneration which may occur under certain technological circumstances. Although a reference line for preventive actions in terms of general metallurgical and process measures could be drawn to avoid CHG in heavy-sectioned ferritic SGI castings, a broad majority of experts claim the avoidance of CHG in heavy sections cannot yet be rated a hundred percent process safe. A major reason may be seen in the fact that a universal, generally accepted explanation of CHG formation and growth has not yet been established, although several theories have been proposed. Nevertheless, metallurgical aspects are not in the focus of this paper.
This paper is about the current state of methods to detect CHG in SGI on the laboratory and component scales. Capabilities and limits of different metallographic, fractographic and non-destructive computer tomographic methods to recognize and quantify CHG are discussed. With respect to the characteristic fili-gree three-dimensional string-like, multi-branched CHG structure, which is non-isometric and non-dispersed, serious implications on the possibility to quantitatively characterize the amount of CHG must be considered.
In contrary to the metallurgical aspects, the knowledge about the impact of CHG on the materials and com-ponents properties is still surprisingly limited. Therefore, special emphasis of this paper is on the impact of CHG degeneration on the properties of ferritic SGI. Experimental results are reviewed to illustrate the effect of CHG on mechanical strength and ductility properties as well as fracture mechanics properties in terms of crack resistance and fracture toughness.
The present situation is characterized by discussions and uncertainty about the acceptance or rejection of SGI components containing CHG. Addressing this, conclusions from the materials engineering point of view are drawn for quality control, a safe operational strategy in the foundry and component safety.
Since there is a continuously growing demand for complex, frequently heavy-sectioned spheroidal graphite cast iron (SGI) castings it is worth paying attention to the chunky graphite (CHG) degeneration which may occur under certain technological circumstances. Although a reference line for preventive actions in terms of general metallurgical and process measures could be drawn to avoid CHG in heavy-sectioned ferritic SGI castings, a broad majority of experts claim the avoidance of CHG in heavy sections cannot yet be rated a hundred percent process safe. A major reason may be seen in the fact that a universal, generally accepted explanation of CHG formation and growth has not yet been established, although several theories have been proposed. Nevertheless, metallurgical aspects are not in the focus of this paper.
This paper is about the current state of methods to detect CHG in SGI on the laboratory and component scales. Capabilities and limits of different metallographic, fractographic and non-destructive computer tomographic methods to recognize and quantify CHG are discussed. With respect to the characteristic fili-gree three-dimensional string-like, multi-branched CHG structure, which is non-isometric and non-dispersed, serious implications on the possibility to quantitatively characterize the amount of CHG must be considered.
In contrary to the metallurgical aspects, the knowledge about the impact of CHG on the materials and com-ponents properties is still surprisingly limited. Therefore, special emphasis of this paper is on the impact of CHG degeneration on the properties of ferritic SGI. Experimental results are reviewed to illustrate the effect of CHG on mechanical strength and ductility properties as well as fracture mechanics properties in terms of crack resistance and fracture toughness.
The present situation is characterized by discussions and uncertainty about the acceptance or rejection of SGI components containing CHG. Addressing this, conclusions from the materials engineering point of view are drawn for quality control, a safe operational strategy in the foundry and component safety.
Based on state-of-the-art research and regulations, the application of the fracture mechanics master curve (MC) concept to ferritic ductile cast iron (DCI) is being investigated in a recently started German joint research project between BAM Berlin and MPA Stuttgart. This paper outlines the research approach and the planned investigations and provides first results.
According to the IAEA guidelines SSG 26, the safety assessment of DCI containers for transport as well as interim and final storage of radioactive materials is based on the fracture mechanics criterion of general crack initiation exclusion. Within this context, the focus of the current research project is on the further development of brittle fracture safety assessment methods under dynamic loading conditions. Within fracture mechanics safety assessments for steels in nuclear technology, the probabilistic MC concept according to ASTM E1921 is currently used for quasi-static loading conditions as a supplement to the established deterministic ASME reference curve concept. The MC concept allows for an effective statistical consideration of the scatter of the material toughness in the transition regime. Furthermore, the MC can also be used for elevated loading rates as they occur in accident or crash scenarios. However, for DCI, a systematic review of potential modifications to the MC assumptions and procedure according to ASTM E1921 and an associated validation are still lacking. Therefore, a corresponding methodology shall be established to determine and assess dynamic fracture toughness values of DCI in the ductile-to-brittle transition regime, using samples extracted from a component.
For the experimental program, a DCI material was produced as it is generally used for transport and storage containers. A basic mechanical-technological material characterization consisting of tensile, Charpy, and Pellini tests is planned. A comprehensive fracture mechanics test program was compiled covering dynamic testing of DC(T)9, C(T)25, C(T)50, SE(B)10, SE(B)25, and SE(B)140 specimens. Moreover, numerical analyses of different specimen geometries and test setups are planned to investigate the influences of stress triaxiality and loading rate. Throughout the experimental program, the microstructure-property relationship will be investigated based on quantitative metallographic and fractographic analyses. Finally, different MC assessment strategies will be considered, and modifications will be made if necessary.
Was Sie schon immer über Chunky-Graphit wissen w(s)ollten, aber bisher nicht zu fragen wagten
(2023)
Duktile Gusseisenwerkstoffe mit Kugelgraphit (GJS) haben ein erhebliches technisches Potenzial und sind von wirtschaftlicher Bedeutung. Nicht zuletzt daher ist es ökonomisch sinnvoll, gesellschaftlich nachhaltig und wissenschaftlich interessant, ihren Herstellungsprozess zu optimieren. Eine maßgebliche Rolle kommt hierbei der Vermeidung von Qualitätsabweichungen in Form von Gefügefehlern zu. Dieser Beitrag befasst sich mit der – leider vielfach nicht richtig oder zu wenig verstandenen, aber insbesondere bei kostenintensi-ven dickwandigen Gussteilen relevanten - Graphitentartung Chunky-Graphit (CG).
Die metallurgischen Ursachen von CG werden noch immer kontrovers diskutiert. Eine allgemein akzeptierte Theorie zur Bildung und dem Wachstumsmechanismus von CG existiert nicht, in der Gießereipraxis wird gleichwohl eine Fülle spezifischer technologischer Abhilfemaßnahmen praktiziert [1].
Der Schwerpunkt dieses Beitrages liegt jedoch nicht auf der metallurgischen Seite, sondern auf der Beschrei-bung der spezifischen Morphologie von CG (Bild 1), dessen Detektion im Werkstoff bzw. Bauteil sowie den Auswirkungen von CG auf die Werkstoffeigenschaften. Detailliert werden Möglichkeiten und Grenzen zer-störungsfreier und zerstörender Untersuchungsverfahren zur Identifikation und Quantifizierung von CG aufgezeigt. Ausgehend von der charakteristischen Morphologie von CG wird dessen Einfluss auf das Ver-formungs- und Bruchverhalten von GJS behandelt. Beispielhaft werden dabei die Eigenschaften Festigkeit, Verformbarkeit, das Risswachstumsverhalten und die Bruchzähigkeit diskutiert und Schlussfolgerungen für die Bewertung von mit CG behafteten GJS-Bauteilen abgeleitet.
Based on state-of-the-art research and regulations, the application of the fracture mechanics master curve (MC) concept to ferritic ductile cast iron (DCI) is being investigated in a recently started German joint research project between BAM Berlin and MPA Stuttgart. This paper outlines the research approach and the planned investigations and provides first results.
According to the IAEA guidelines SSG 26, the safety assessment of DCI containers for transport as well as interim and final storage of radioactive materials is based on the fracture mechanics criterion of general crack initiation exclusion. Within this context, the focus of the current research project is on the further development of brittle fracture safety assessment methods under dynamic loading conditions. Within fracture mechanics safety assessments for steels in nuclear technology, the probabilistic MC concept according to ASTM E1921 is currently used for quasi-static loading conditions as a supplement to the established deterministic ASME reference curve concept. The MC concept allows for an effective statistical consideration of the scatter of the material toughness in the transition regime. Furthermore, the MC can also be used for elevated loading rates as they occur in accident or crash scenarios. However, for DCI, a systematic review of potential modifications to the MC assumptions and procedure according to ASTM E1921 and an associated validation are still lacking. Therefore, a corresponding methodology shall be established to determine and assess dynamic fracture toughness values of DCI in the ductile-to-brittle transition regime, using samples extracted from a component.
For the experimental program, a DCI material was produced as it is generally used for transport and storage containers. A basic mechanical-technological material characterization consisting of tensile, Charpy, and Pellini tests is planned. A comprehensive fracture mechanics test program was compiled covering dynamic testing of DC(T)9, C(T)25, C(T)50, SE(B)10, SE(B)25, and SE(B)140 specimens. Moreover, numerical analyses of different specimen geometries and test setups are planned to investigate the influences of stress triaxiality and loading rate. Throughout the experimental program, the microstructure-property relationship will be investigated based on quantitative metallographic and fractographic analyses. Finally, different MC assessment strategies will be considered, and modifications will be made if necessary.
Photopolymer derived carbon grows in popularity, yet the range in available feature sizes is limited. Here we focus on expanding the field to low surface to volume ratio (SVR) structures. We describe a high temperature acrylic photopolymerizable precursor with FTIR and DSC and develop a thermal inert-gas treatment for producing architected carbon in the mm scale with SVR of 1.38 x10-3 μm-1. Based on TGA and MS, we distinguish two thermal regimes with activation energies of ~79 and 169 kJ mol-1, which we reason with mechanisms during the polymer’s morphologic conversion between 300 - 500 °C. The temperature range of the major dimensional shrinkage (300-440 °C, 50%) does not match the range of the largest alteration in elemental composition (440-600 °C, O/C 0.25-0.087%). The insights lead to an optimized thermal treatment with an initial ramp (2 °C min-1 to 350 °C), isothermal hold (14h), post hold ramp (0.5 °C min-1 to 440 °C) and final ramp (10 °C min-1 to 1000 °C). The resulting carbon structures are dimensionally stable, non-porous at the μm scale, and comprise an unprecedented variation in feature sizes (from mm to μm scale). The findings shall advance architected carbon to industrially relevant scales.
Cryoadsorption on the inner surface of porous materials is a promising solution for safe, fast, and reversible hydrogen storage. Within the class of highly porous metal−organic frameworks, zeolitic imidazolate frameworks (ZIFs) show high thermal, chemical, and mechanical stability. In this study, we selected ZIF-8 synthesized mechanochemically by twin-screw extrusion as powder and pellets. The hydrogen storage capacity at 77 K and up to 100 bar has been analyzed in two laboratories applying three different measurement setups showing a high reproducibility. Pelletizing ZIF-8 increases the packing density close to the corresponding value for a single crystal without loss of porosity, resulting in an improved volumetric hydrogen storage capacity close to the upper limit for a single crystal. The high volumetric uptake combined with a low and constant heat of adsorption provides ca. 31 g of usable hydrogen per liter of pellet assuming a temperature−pressure swing adsorption process between 77 K − 100 bar and 117 K − 5 bar. Cycling experiments do not indicate any degradation in storage capacity. The excellent stability during preparation, handling, and operation of ZIF-8 pellets demonstrates its potential as a robust adsorbent material for technical application in pilot- and full-scale adsorption vessel prototypes.
The main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration.
In dentistry it is of great interest to achieve good sealing interzones between tooth tissue and restoration materials to avoid, e. g. secondary caries. μXRF and CμXRF are suitable to investigate the elemental composition at these interzones in respect to diffusion of elements. Synchrotron X-ray refraction radiography (SXRR) and μCT measurements deliver highly resolved structural information and make structural changes such as micro cracks within the filling and the tooth tissue visible. The presented measurements are part of the DFG funded project IXdent (Integrative X-ray techniques for chemical and structural characterizations of dental interzones.)
The depth-resolved CμXRF measurements are affected by absorption effects, making a quantitative investigation of the interzone in depth difficult. Full 3D quantification of heterogenous samples requires a complete model including dark matrix and density for each voxel. The combination of different techniques paves the way for a quantitative analysis of dental interzones.
Towards interoperability: Digital representation of a material specific characterization method
(2023)
Certain metallic materials gain better mechanical properties through controlled heat treatments. In age-hardenable aluminum alloys, the strengthening mechanism is based on the controlled formation of nanometer sized precipitates, which hinder dislocation movement. Analysis of the microstructure and especially the precipitates by transmission electron microscopy allows identification of precipitate types and orientations. Dark-field imaging is often used to image the precipitates and quantify their relevant dimensions.
The present work aims at the digital representation of this material-specific characterization method. Instead of a time-consuming, manual image analysis, a digital approach is demonstrated. The integration of an exemplary digital workflow for quantitative precipitation analysis into a data pipeline concept is presented. Here ontologies enable linking of contextual information to the resulting output data in a triplestore. Publishing digital workflow and ontologies ensures the reproducibility of the data. The semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
This presentation provides a comprehensive overview of recent developments and the current status within the Semantic Interoperability work area, with a particular emphasis on the advancements related to the Platform MaterialDigital Core Ontology (PMDco). The presentation will delve into the collaborative and community-supported curation process that has been instrumental in shaping PMDco. Additionally, we will introduce the innovative Ontology Playground, showcasing its role in fostering experimentation and exploration within the realm of ontology development.
The PMD Core Ontology (PMDco) is a comprehensive set of building blocks produced via consensus building. The ontological building blocks provide a framework representing knowledge about fundamental concepts used in Materials Science and Engineering (MSE) today. The PMDco is a mid-level ontology that establishes connections between narrower MSE application ontologies and domain neutral concepts used in already established broader (top-level) ontologies. The primary goal of the PMDco design is to enable interoperability between various other MSE-related ontologies and other common ontologies.
PMDco’s class structure is both comprehensive and extensible, rendering it an efficient tool to structure MSE knowledge. The PMDco serves as a semantic middle-layer unifying common MSE concepts via semantic mapping to other semantic representations using well-known key terms used in the MSE domain. The PMDco enables straight-forward documentation and tracking of science data generation and in consequence enables high-quality FAIR data that allows for precise reproducibility of scientific experiments.
The design of PMDco is based on the W3C Provenance Ontology (PROV-O), which provides a standard framework for capturing the production, derivation, and attribution of resources. Via this foundation, the PMDco enables the integration of data from various data origins and the representation of complex workflows.
In summary, the PMDco is a valuable advancement for researchers and practitioners in MSE domains. It provides a common MSE vocabulary to represent and share knowledge, allowing for efficient collaboration and promoting interoperability between diverse domains. Its design allows for the systematic integration of data and metadata, enabling seamless tracing of science data. Overall, the PMDco is a crucial step towards a unified and comprehensive understanding of the MSE domain in general.
Many metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminium alloys, the strengthening mechanism is based on the controlled formation of nanometre-sized precipitates, which represent obstacles to dislocation movement and consequently increase the strength. Precise tuning of the material microstructure is thus crucial for optimal mechanical behaviour under service condition of a component. Therefore, analysis of the microstructure, especially the precipitates, is essential to determine the optimum parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in the first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and thereafter quantify their relevant dimensions. Often, these evaluations are still performed by manual image analysis, which is very time-consuming and to some extent also poses reproducibility problems.
Our work aims at a semantic representation of an automatable digital approach for this material specific characterization method under adaption of FAIR data practices. Based on DF-TEM images of different precipitation states of a wrought aluminium alloy, the modularizable, digital workflow of quantitative analysis of precipitate dimensions is described. The integration of this workflow into a data pipeline concept will also be discussed. Using ontologies, the raw image data, their respective contextual information, and the resulting output data of the quantitative image analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure data reproducibility. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was
found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism.
Laser powder bed fusion of metallic components (PBF-LB/M) is gaining acceptance in industry. However, the high costs and lengthy qualification processes required for printed components create the need for more effective in-situ monitoring and testing methods. This article proposes multispectral Optical Tomography (OT) as a new approach for monitoring the PBF-LB/M process. Compared to other methods, OT is a low-cost process monitoring method that uses long-time exposure imaging to observe the build process. However, it lacks time resolution compared to expensive thermographic sensor systems. Monochromatic OT (1C-OT) is already commercially available and observes the building process layer-wise using a single wavelength window in the NIR range. Multispectral OT (nC-OT) utilizes a similar setup but can measure multiple wavelength ranges per location simultaneously. By comparing the classical 1C-OT and nC-OT approaches, this article examines the advantages of nC-OT (two channel OT and RGB-OT) in reducing the false positive rate for process deviations and approximating maximum temperatures for a better comparison between different build processes and materials. This could ultimately reduce costs and time for part qualification. The main goal of this contribution is to assess the advantages of nC-OT compared to 1C-OT for in-situ process monitoring of PBF-LB/M.
Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results.
The role of defects in the fatigue strength of Wire Arc Additively Manufactured (WAAMed) Ti-6Al-4V is analysed by means of the IBESS model, a fracture mechanics short crack growth approach based on the cyclic R-curve. Pores and crack-like defects are analysed. Estimations of the role of pore shape and size agree well with published fatigue data of WAAM Ti-6Al-4V with pores. The model is also used to explain the effect of fabrication defects on the scatter of experimental data. This demonstrates that short crack growth models represent a suitable engineering tool for the fatigue assessment of defective AM materials.
In this article, we present two Coptic papyri, P 11934 and P 11935 from the Berlin collection excavated in Ashmunein (ancient Hermopolis) by Otto Rubensohn in 1906. We employ a multi-disciplinary approach that takes into account both their materiality – writing support as well as ink – and their content, as has become ‘best practice’. 1 Material aspects of written documents have traditionally been the purview of papyrologists. Recently developed methods of scientific analysis generate sets of archaeometric data with the potential to improve understanding of the materiality of ancient document production, as well as to yield new evidence for genuine papyrological research questions. To achieve this, a large corpus of comparative data needs to be built. Our contribution offers a first step in this direction. We aim at presenting the papyri, which were selected because of the ink corrosion during conservation work at the Berlin collection, in a format that is exhaustive both for material and textual aspects. The inks from both papyri were analysed using a combination of techniques, contributing to our better understanding of the development of ink technology in Late Antiquity.
The lattice enthalpies and monotropic relationship of two dehydroepiandrosterone (DEHA) polymorphs (forms I and II) were evaluated through a combination of differential scanning calorimetry (DSC), isothermal solution microcalorimetry, and drop-sublimation Calvet microcalorimetry experiments. The standard molar enthalpy of transition between both forms was determined as ΔtrsHom (II→I, 298.15 K) = - 0.90 ± 0.07 kJ mol-1 and ΔtrsHom (II→I, 417.8 K) = - 1.7 ± 1.0 kJ mol- 1, from measurements of standard molar enthalpies of solution in dimethyl sulfoxide and enthalpies of fusion, respectively. Drop-sublimation Calvet microcalorimetry experiments on form I led to ΔsubHom (cr I, 298.15 K) = 132.0±3.3 kJ mol - 1. This result, when combined with the more precise ΔtrsHom (II→I) value obtained by solution calorimetry, afforded ΔsubHom (cr II, 298.15 K) = 131.1±3.3 kJ mol - 1. The overall data indicate that on enthalpic grounds form I is more stable than form II from 298.15 K up to fusion. This conclusion, and the fact that DSC experiments indicated that form I has also a considerably higher temperature fusion, namely, Tfus(cr I)= 422.5±0.2 K and Tfus(cr II) = 413.1±0.2 K, suggest that the two polymorphs are monotropically related.
Comprehensive evaluation of peptide de novo sequencing tools for monoclonal antibody assembly
(2023)
Monoclonal antibodies are biotechnologically produced proteins with various applications in research, therapeutics and diagnostics. Their ability to recognize and bind to specific molecule structures makes them essential research tools and therapeutic agents. Sequence information of antibodies is helpful for understanding antibody–antigen interactions and ensuring their affinity and specificity. De novo protein sequencing based on mass spectrometry is a valuable method to obtain the amino acid sequence of peptides and proteins without a priori knowledge. In this study, we evaluated six recently developed de novo peptide sequencing algorithms (Novor, pNovo 3, DeepNovo, SMSNet, PointNovo and Casanovo), which were not specifically designed for antibody data. We validated their ability to identify and assemble antibody sequences on three multi-enzymatic data sets. The deep learning-based tools Casanovo and PointNovo showed an increased peptide recall across different enzymes and data sets compared with spectrum-graph-based approaches. We evaluated different error types of de novo peptide sequencing tools and their performance for different numbers of missing cleavage sites, noisy spectra and peptides of various lengths. We achieved a sequence coverage of 97.69–99.53% on the light chains of three different antibody data sets using the de Bruijn assembler ALPS and the predictions from Casanovo. However, low sequence coverage and accuracy on the heavy chains demonstrate that complete de novo protein sequencing remains a challenging issue in proteomics that requires improved de novo error correction, alternative digestion strategies and hybrid approaches such as homology search to achieve high accuracy on long protein sequences.
Komponenten von Fahrrädern werden im Betrieb vorwiegend schwingend beansprucht. Typische Werkstoffe sind Stahl, Aluminiumlegierungen, Messing, CFK und thermoplastische Kunststoffe. Da es sich, unabhängig von der Preiskategorie, um konstruktiven Leichtbau handelt, werden einige Bauteile betriebsfest mehr oder weniger weit oberhalb der Dauerfestigkeit ausgelegt. Die im normalen Betrieb auftretenden Schäden sind daher weit überwiegend Schwingbrüche. Andere Schadensmechanismen wie z.B. Korrosion spielen quantitativ eine untergeordnete Rolle. Schwingbrüche treten nach einer Periode unbemerkten Risswachstums oft ohne Vorwarnung und ohne makroskopische Verformung auf. Im Falle von sicherheitsrelevanten Komponenten wie Rahmen, Gabeln, Lenkern, Sattelstützen, Kurbelarmen oder Pedalen kann dies zu erheblichen Personenschäden führen, die den Wert des ursächlichen Bauteilschadens weit überschreiten.
Über einen langjährigen Zeitraum wurden gebrochene Komponenten aus dem Alltag und aus Gerichtsverfahren analysiert. Das Hauptaugenmerk lag hierbei auf der fraktographischen Analyse, teilweise wurden die zu Grunde liegenden Schadensursachen ermittelt. Einflussfaktoren sind beispielsweise konstruktive Kerben an ungünstigen Stellen, aber auch Werkstoffwahl und Fertigungsqualität spielen eine Rolle. In den meisten Fällen wurde jedoch die konstruktive Lebensdauer überschritten. Diese wird praktisch nie mitgeteilt, und eine wiederkehrende Prüfung sicherheitsrelevanter Bauteile findet nicht statt.
Im Sinne der Vermeidung von Schäden und Unfällen könnte darauf hingewirkt werden, für sicherheitsrelevante Komponenten Lebensdauern besser abzuschätzen und von der Laufleistung abhängige Sichtprüfungen zu empfehlen.
Die AG Fraktographie im DVM/DGM-Gemeinschaftsgremium „Elektronenmikroskopie in der Materialforschung“ betreibt seit 2013 eine fraktographische online-Datenbank („FractoDB“), die für das interessierte Fachpublikum kostenfrei zur Verfügung steht. Die Analyse und Bewertung von Bruchflächen und der darauf befindlichen Bruchmerkmale ist ein wichtiger Teilaspekt der Schadensanalyse bei der Suche nach Schadensmechanismen und Schadensursachen. Risse und Brüche an realen Bauteilen können nur dann bewertet werden, wenn gut dokumentierte Vergleichsbrüche aus Laborversuchen zur Verfügung stehen, sei es an Proben oder an Vergleichs-Bauteilen. Daher trägt die AG Fraktographie Bildmaterial zusammen, führt systematisch Laborversuche und Ringversuche durch und analysiert Brüche aus Schadensfällen. Die gewonnenen Daten werden zu Datensätzen zusammengestellt und über die Datenbank zugänglich gemacht. Derzeit ist ein Bestand von über 400 Datensätzen mit insgesamt über 4.500 Bildern verfügbar, welcher durchsucht werden kann und in Anlehnung an die VDI 3822 organisiert ist. Weitere Aktivitäten der AG Fraktographie, die in der FractoDB abgebildet werden, sind u.a. die Entwicklung einer fraktographischen Symbolik und die Analyse von Bruchmerkmalen mittels Machine Learning. Über die aktuellen Ergebnisse und Planungen wird berichtet.
Die Fraktographische Online-Datenbank der AG Fraktographie – Entwicklungsstand und weitere Planung
(2023)
Vortrag zum aktuellen Stand der fraktographischen online-Datenbank. Darstellung des AGM/DVM Gemeinschaftsausschusses REM in der Materialforschung und seiner Arbeitsgruppen Fraktographie, EBSD und 2D/3D-Prüfung. Ziele und Inhalte der fraktographischen Datenbank, Aufruf zum Mitmachen. Durchführung von Vergleichsversuchen, Entwicklung einer fraktographischen Symbolik, Ringversuch, Vorhaben iFrakto mit Entwicklung einer KI-gestützten Bruchflächenanalyse.
The materials mechanical testing ontology (MTO) was developed by collecting the mechanical testing vocabulary from ISO 23718 standard, as well as the standardized testing processes described for various mechanical testing of materials like tensile testing, Brinell hardness test, Vickers hardness test, stress relaxation test, and fatigue testing. Confirming the ISO/IEC 21838-2 standard, MTO utilizes the Basic Formal Ontology (BFO), Common Core Ontology (CCO), Industrial Ontologies Foundry (IOF), Quantities, Units, Dimensions, and data Types ontologies (QUDT), and Material Science and Engineering Ontology (MSEO) as the upper-level ontologies. Reusing these upper-level ontologies and materials testing standards not only makes MTO highly interoperable with other ontologies but also ensures its acceptance and applicability in the industry. MTO represents the mechanical testing entities in the 230 classes and four main parts: i) Mechanical testing experiments entities like tensile, hardness, creep, and fatigue tests as the subclasses of mseo:Experiment, ii) Mechanical testing quantity concepts such as toughness, elongation, and fatigue strength in the appropriate hierarchies of bfo:Disposition and bfo:Quality classes, iii) Mechanical testing artifacts like indenter as the subclasses of cco:Artifact, and iv) mechanical testing data like the stress-strain, S-N, or creep curves as the subclasses of cco:InformationContentEntity. MTO is publicly available via the KupferDigital GitLab repository.
The KupferDigital project aims to develop digital methods, tools, and data space infrastructures for digitalizing the entire life cycle of copper materials. The mechanical testing process is one of the main chains of such life cycles which generates lots of important testing data about the mechanical properties of the materials and their related materials and testing metadata. To train the digitalization of the mechanical testing process, different kinds of copper alloys were provided for this project, and their mechanical properties were measured by typical methods like Brinell and Vickers hardness and tensile testing. The primary raw testing data as well as the secondary datasets of these tests are provided. The detailed materials specifications, the utilized mechanical testing methods, and provided datasets are described in the content file. The test data files of heterogeneous structures are processed by the KupferDigital digital tools to be converted to standardized machine-readable data files.
This research deals with the development of the Vickers hardness knowledge graph, mapping the example dataset in them, and exporting the data-mapped knowledge graph as a machine-readable Resource Description Framework (RDF). Modeling the knowledge graph according to the standardized test procedure and using the appropriate upper-level ontologies were taken into consideration to develop the highly standardized, incorporable, and industrial applicable models. Furthermore, the Ontopanel approach was utilized for mapping the real experimental data in the developed knowledge graphs and the resulting RDF files were successfully evaluated through the SPARQL queries.
Mechanical testing ontology
(2023)
The materials mechanical testing ontology (MTO) was developed by collecting the mechanical testing vocabulary from ISO 23718 standard, as well as the standardized testing processes described for various mechanical testing of materials like tensile testing, Brinell hardness test, Vickers hardness test, stress relaxation test, and fatigue testing. Confirming the ISO/IEC 21838-2 standard, MTO utilizes the Basic Formal Ontology (BFO), Common Core Ontology (CCO), Industrial Ontologies Foundry (IOF), Quantities, Units, Dimensions, and data Types ontologies (QUDT), and Material Science and Engineering Ontology (MSEO) as the upper-level ontologies.
Nickel-based alloys have been widely used for gas turbine blades owing to their excellent mechanical properties and corrosion resistance at high temperatures. The operating temperatures of modern gas turbines have been increased in pursuit of increased thermal efficiency. Turbine blades are exposed to these high temperatures combined with mechanical stresses, resulting in material damage through creep, fatigue, and other mechanisms. These turbine blades must be regularly inspected and replaced as needed, to prevent the loss of efficiency, breakdown, and catastrophic failure. Repair of the damaged turbine blades is often a more practical and cost-effective option than replacement, as replacement is associated with high costs and loss of material resources. To this end, state-of-the-art repair technologies including different additive manufacturing and brazing processes are considered to ensure efficient repair and optimum properties of repaired components.
In any repaired part, materials property-mismatches and/or inner defects may facilitate the crack initiation and propagation and thus reduce the number of load cycles to failure. Therefore, a fundamental understanding of the fatigue crack growth and fracture mechanisms in joining zones is required to enable the prediction of the remaining life of repaired components and to further improve and adapt the repair technologies.
Fatigue crack growth experiments have been conducted on SEN (Single Edge Notch) specimens joined via brazing, and pre-sintered Preform (PSP) and multi-materials (casted/printed) specimens layered via additive manufacturing (AM). The experiments were performed at 950 °C and various stress ratios. The crack growth was measured using DCPD (Direct Current Potential Drop) method. The stress intensity factors for joined SEN specimens were calculated using the finite element method and then used to derive the fatigue crack growth curves. Metallographic and fractographic analyses were conducted to get insight into the fracture mechanism.
Results show that the experimental technique for fatigue crack growth was successfully adapted and applied for testing joined specimens. Furthermore, the initial tests indicate that the investigated braze filler material provides a lower resistance to crack growth, and bonding defects cause a crack to deviate to the interface of the base material and joining zone. In AM-sandwich specimens, the crack growth rates are significantly reduced when the crack reaches the interface of printed material and casted material. The obtained crack growth data can be used to calibrate a crack growth model, which will further be utilized to predict the remaining life of repaired components.
Proton exchange membrane fuel cells (PEMFCs) are one of the most promising alternative green energy technologies that deliver high energy density without CO2 emissions. The proton conductivity of proton exchange membranes (PEM) contributes to the overall efficiency of a PEMFC. Materials being used as PEMs must exhibit high proton conductivity at the working conditions of the targeted PEMFC. To date, Nafion and Nafion-like polymers with acidic functionality are widely used as membrane materials due to their high proton conductivity in the range of 10-1 to 10-2 Scm-1 at higher relative humidity. However, these materials suffer from high costs, hazardous production process, and poor performance at high temperatures, limiting their versatility.
In this context, crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology, owing to their tunable framework structure. However, it is still challenging bulk synthesis for real-world applications of these materials. Herein, we present mechanochemical gram-scale synthesis of series of mixed ligand metal organic frameworks (MOFs) and metal hydrogen‐bonded organic frameworks (MHOFs) using phenylene diphosphonic acid and 1-hydroxyethylidene-1,1-diphosphonic acid with different bipyridyl type of ligands, respectively. In all cases, the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, the frameworks exhibited high proton conductivity. The study demonstrates the potential of green mechanosynthesis for preparations of framework-based proton conducting materials in bulk scale for green energy generation.
Mechanically flexible single crystals of molecular materials offer potential for a multitude of new directions in advanced materials design. Before the full potential of such materials can be exploited, insight into their mechanisms of action must be better understood. Such insight can be only obtained through synergistic use of advanced experimentation and simulation. We herein report the first detailed mechanistic study of elasto-plastic flexibility in a molecular solid. An atomistic origin for this mechanical behaviour is proposed through a combination of atomic force microscopy, μ-focus synchrotron X-ray diffraction, Raman spectroscopy, ab initio simulation, and computed elastic tensors. Our findings suggest that elastic and plastic bending are intimately linked and result from extensions of the same molecular deformations. The proposed mechanism bridges the gap between contested mechanisms, suggesting its applicability as a general mechanism for elastic and plastic bending in organic molecular crystals.
To evaluate the durability of new alternative cement compositions, it is important to examine the internal transport of moisture through these materials. For this purpose, mortars were prepared from different types of cement and capillary suction experiments were carried out. The moisture transport was studied with an NMR tomograph and compared with weight easurements. With the tomograph, the total moisture input could be determined, as well as the moisture content within the samples non-destructively and spatially resolved. This allows precise observation of the moisture fronts. The tomograph was also used to determine the capillary transport
coefficient.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
In this presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
AbstractViscous healing of cracks induced by the Vickers indentation in a soda lime magnesium silicate, a soda borosilicate, and a soda aluminosilicate glass (NAS) was studied by laser scanning microscopy. Plots of the crack length, width, and depth normalized to the initial crack length versus time over viscosity merge into single master curves of each of these quantities for each glass. Despite glass properties do not differ strikingly from each other, however, these master curves strongly differ among the glasses. This finding was attributed to a different interplay of various crack healing phenomena. Lateral cracks were found to be responsible for the bulging of the sample surface around the Vickers imprint, which in turn promotes radial crack widening as the main cause of healing delay. The most rapid healing of lateral cracks was observed in NAS in which bulging and crack widening were least pronounced.
Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any type of solid upon irradiation with intense laser pulses. They represent a (quasi-)periodic modulation of the surface topography in the form of a linear grating and are typically formed in a “self-ordered” way in the focus of a laser beam. Thus, they are often accompanying laser material processing applications. The structural sizes of LIPSS typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation.
From a theoretical point of view, a controversial debate has emerged during the last decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter-reorganization processes (distinctly after the laser irradiation). From a practical point of view, however, LIPSS represent a simple and robust way for the nanostructuring of solids that allows creating a wide range of different surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc.
This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas behind the LIPSS, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches.
Fourth generation light sources, namely short wavelength, short pulse free electron lasers (FELs) are offering new and fascinating possibilities to resolve laser-induced structure formation at surfaces on the sub-micrometer to nanometer length scale and in temporal regimes ranging from picoseconds to several nanoseconds with sub-picosecond resolution. This unique spatio-temporal resolution allows to reveal early signatures of coherent/plasmonic electromagnetic scattering effects followed by the excitation of hydrodynamic capillary waves – providing new insights to the above-mentioned debate.
Finally, some unsolved scientific problems related to LIPSS are identified and the pending technological limitations are discussed. While the currently available laser and scanner technology already allows large area surface processing with rates at the m2/min level, industrial applications of LIPSS are sometimes limited by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. Strategies for overcoming such limitations are outlined.
Laser-induced periodic surface structures (LIPSS) have gained remarkable attention as they represent a universal phenomenon that is often accompanying laser-processing. Such LIPSS enable a large variety of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Moreover, so-called “high spatial frequency LIPSS” (HSFL) provide an appealing and straightforward way for surface nanostructuring featuring spatial periods even below 100 nm – far beyond the optical diffraction limit. However, the imposed surface functionalities are usually caused by both, topographic and chemical surface alterations. For exploring these effects in detail, multi-method characterizations were performed here for HSFL on processed Ti- 6Al- 4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 1 – 400 kHz pulse repetition rate) under different laser and scan processing conditions. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), stylus profilometry (SP), and white light interference microscopy (WLIM), as well as near-surface chemical analyses by X-ray photoelectron spectroscopy (XPS), hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results allow to qualify the laser ablation depth, the geometrical HSFL characteristics and provide detailed insights into the depth extent and the nature of the ps-laser-induced near-surface oxidation. Significance for medical applications will be outlined.
Laser-induced periodic surface structures (LIPSS) and their combination with self-ordered microstructures forming hierarchical Spikes enable a large variety of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Moreover, high spatial frequency LIPSS (HSFL) provide an appealing and straightforward way for surface nanostructuring featuring spatial periods even below 100 nm – far beyond the optical diffraction limit. However, the imposed surface functionalities are usually caused by both, topographic and chemical surface alterations. For exploring these effects in detail, multi-method characterizations were performed here for HSFL and hierarchical Spikes processed on Ti-6Al-4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 1 – 400 kHz pulse repetition rate) under different laser and scan processing conditions. The following sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), stylus profilometry (SP), and white light interference microscopy (WLIM), as well as near-surface chemical analyses by X-ray photoelectron spectroscopy (XPS), hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results allow to qualify the laser ablation depth, the geometrical HSFL/Spikes characteristics and provide detailed insights into the depth extent and the nature of the ps-laser-induced near-surface oxidation arising from the laser-processing in ambient air and into the relevance of heat-accumulation effects at high pulse repetition rates. Moreover, the direct comparison of the HAXPES and XPS data reveals the role of surface-covering organic contaminants adsorbed from the ambient atmosphere without the uncertainties and potential sputter reduction potentially caused by ion-sputter depth profiling.
Irradiation of solid surfaces with intense ultrashort laser pulses represents a unique way of depositing energy into materials. It allows to realize states of extreme electronic excitation and/or very high temperature and pressure and to drive materials close to and beyond fundamental stability limits. As a consequence, structural changes and phase transitions often occur along unusual pathways and under strongly nonequilibrium conditions. Due to the inherent multiscale nature — both temporally and spatially—of these irreversible processes, their direct experimental observation requires techniques that combine high temporal resolution with the appropriate spatial resolution and the capability to obtain good quality data on a single pulse/event basis. In this respect, fourth-generation light sources, namely, short wavelength and short pulse free electron lasers (FELs), are offering new and fascinating possibilities. As an example, this talk will discuss the results of scattering experiments carried out at the FLASH free electron laser at DESY (Hamburg, Germany), which allowed us to resolve laser-induced structure formation at surfaces on the nanometer to submicron length scale and in temporal regimes ranging from picoseconds to several nanoseconds with sub-picosecond resolution. The current status and future perspectives in this field via exploiting the unique possibilities of these 4th-generation light sources will be discussed.
Laser-induced periodic surface structures (LIPSS) have gained remarkable attention as they represent a universal phenomenon that is often accompanying laser-processing. Such LIPSS enable a plethora of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Due to the inherent multiscale nature of processes involved in LIPSS formation, their in-situ observation requires experimental techniques that combine high temporal resolution with the appropriate spatial resolution. In this respect fourth generation light sources, namely short wavelength, short pulse free electron lasers (FELs) are offering new and fascinating possibilities. This work contribution will discuss the results of scattering experiments carried at the FLASH free electron laser at DESY (Hamburg, Germany), which allowed us to resolve laser-induced structure formation at surfaces on the nm to sub-µm length scale and in temporal regimes ranging from ps to several ns with sub-ps resolution. A ps-optical pump / fs-XUV scattering probe scheme was employed to 100 nm thick laser-excited silicon films, while recording snapshots of the transmitted XUV scattering patterns at various delay times after the laser pulse impact. On timescales ranging from hundred ps until several ns almost quantitative agreement was observed between certain features of the recorded scattering patterns and predictions of the first-principles theory of J.E. Sipe and coworkers. Other scattering features appearing with a delay of ~100 ps and lasting for ~1 ns are attributed to capillary surface waves being excited at the laser-melted film material while ablation proceeds. Our superior spatio-temporal resolution experiments allow to uniquely reveal and distinguish early signatures of coherent/plasmonic electromagnetic scattering effects, separately followed by hydrodynamic matter reorganization.
Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications.
Defects are still common in metal components built with Additive Manufacturing (AM). Process monitoring methods for laser powder bed fusion (PBF-LB/M) are used in industry, but relationships between monitoring data and defect formation are not fully understood yet. Additionally, defects and deformations may develop with a time delay to the laser energy input. Thus, currently, the component quality is only determinable after the finished process.
Here, active laser thermography, a non-destructive testing method, is adapted to PBF-LB/M, using the defocused process laser as heat source. The testing can be performed layer by layer throughout the manufacturing process. The results of the defect detection using infrared cameras are presented for a custom research PBF-LB/M machine. Our work enables a shift from post-process testing of components towards in-situ testing during the AM process. The actual component quality is evaluated in the process chamber and defects can be detected between layers.
Great complexity characterizes Additive Manufacturing (AM) of metallic components via laser powder bed fusion (PBF-LB/M). Due to this, defects in the printed components (like cracks and pores) are still common. Monitoring methods are commercially used, but the relationship between process data and defect formation is not well understood yet. Furthermore, defects and deformations might develop with a temporal delay to the laser energy input. The component’s actual quality is consequently only determinable after the finished process.
To overcome this drawback, thermographic in-situ testing is introduced. The defocused process laser is utilized for nondestructive testing performed layer by layer throughout the build process. The results of the defect detection via infrared cameras are shown for a research PBF-LB/M machine.
This creates the basis for a shift from in-situ monitoring towards in-situ testing during the AM process. Defects are detected immediately inside the process chamber, and the actual component quality is determined.
OECD Prüfrichtlinie 125
(2023)
Diese Präsentation ist eine Einführung in die OECD TG 125 zur Bestimmung der Partikelgrößen von Nanomaterialien. Es wird auf die verchiedenen Probleme der Partikelgrößenbestimmung eingegangen wie z.B. verschiedene Oberflächenschichten, Äquivalenzdurchmesser und Verteilungsfunktionen. Gleichzeitig werden die neuen Begrifflichkeiten eingeführt, die in der TG 125 definiert neu werden.
Die Bestimmung der Nanopartikelgrößen- und -formverteilung nach OECD TG 125 mit einem Differentiellen Mobilitäts Analyse System (DMAS), auch bekannt als SMPS, wird vorgestellt:
- Generelles Messprinzip
- Welchen Durchmesser misst die Methode?
- Welche Partikel kann diese Methode messen?
- Welche Informationen kann diese Methode liefern?
- Wo stößt die Methode an ihre Grenzen?
- Implementierung und Datenauswertung,
- Reporting.
Anschließend wurde eine Q&A-Session für DMAS/SMPS organisiert.
Low-temperature co-fired ceramics (LTCC) are used to fabricate robust multilayer circuits. Typically, thick-film technology is applied for metallization. For specific sensor applications, thin films are deposited directly on the as-fired LTCC-surface. These deposited thin films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it.
200 nm Ni-thin films were deposited on three different commercial constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The thin-films were structured by covering corresponding sections with a UV-curable photo resisn and subsequent etching of the uncovered surface, leaving behind the desired structure. The etched Ni-thin film showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas the CT800 had a failure rate of 40 %. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. To address this phenomenon, the chemical resistance of the three different commercial LTCC (CT708, CT800 and DP951) against four different commonly used etching media (sulphuric acid, phosphoric acid, aqua regia, and hydrofluoric acid) is investigated. The dissolved ions are analyzed by ICP-OES to correlate the LTCC-composition and its chemical resistance.
Low-temperature co-fired ceramics (LTCC) are used to fabricate multilayer circuits which are robust in harsh environments. Thick-film technology is well established for the metallization of circuit boards and microsystems. For specific sensor applications, the combination of LTCC and thin-film technology is advantageous to reach higher structure resolutions. Due to the high roughness of as-fired LTCC surfaces compared with silicon-wafers, the deposition of low-defect- films with narrowly specified properties is challenging. The deposited thin-films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it. There is spare literature about thin films on commercial LTCC comparing different material systems or sintering techniques. For developing thin-film sensors on multilayer circuits it is crucial to identify thin-film-compatible commercial LTCC material as well as the crucial surface properties. In this work we evaluate the thin-film capability of different LTCC compositions and surface qualities.
To evaluate the influence of the material composition on the thin film capability, 200 nm Ni-thin films were deposited on three different constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The effect of surface quality was assessed by thin-film deposition on free-sintered, pressure-assisted sintered, and polished DP951. The thin-films were structured by covering corresponding sections with a UV-curable photo resin and subsequent etching of the uncovered surface, leaving behind the desired structure.
The etched Ni-thin films showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas CT800 had a high sheet resistance and a failure rate of 40 %. These results are correlated with surface roughness of the LTCC, scanning electron micrographs of the deposited thin-films, and the chemical resistance of the LTCC against commonly used etching media. Contrary to the expectations, no correlation between roughness and thin-film capability was found. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. Additionally, the adhesion of thin-films on DP951 is better than on CT708 and CT800.
Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design.
The mechanical properties of unstabilised earthen building materials are distinctively influenced by changes in material moisture content. However, this moisture-dependency often remains unconsidered in the calculation of the load-bearing capacity of earth constructions. This paper aims to derive a convenient way to sufficiently consider the impact of different material moisture contents on the mechanical properties of unstabilised earth masonry. Therefore, the influence of relative humidity and temperature on the strength and deformation characteristics of unstabilised earth blocks, earth mortar and earth masonry is evaluated by conducting compression tests under various climate conditions. The results show that the compressive strength and the modulus of elasticity are linearly correlated with the relative humidity, whereas changes in temperature at constant relative humidity have no significant influence. To account the distinct moisture-dependency, a general applicable modification factor for unstabilised earthen materials is provided, which enables the adjustment of the compressive strength and the modulus of elasticity in dependency of arbitrary hygroscopic material moisture contents.
Lehmmauerwerk bietet sich aufgrund seiner zahlreichen ökologischen Vorteile für die Errichtung klimafreundlicher und ressourcenschonender Gebäude an. Um den Anwendungsbereich tragenden Lehmmauerwerks durch eine zeitgemäße Nachweisführung zu erweitern, werden in diesem Beitrag Grundlagen für die Entwicklung eines eurocodekonformen Bemessungskonzepts erarbeitet. Hierzu werden die Ergebnisse umfangreicher experimenteller Untersuchungen an Lehmmauerwerk sowie Lehmsteinen und -mörteln nach Konditionierung bei unterschiedlichen Klimata vorgestellt. Darauf aufbauend erfolgt eine Traglastanalyse druckbeanspruchter Lehmmauerwerkswände mittels numerischer und analytischer Methoden. Die daraus gewonnenen Erkenntnisse werden abschließend in einen an DIN~EN~1996-3/NA angelehnten Bemessungsvorschlag überführt, welcher die materialspezifischen Besonderheiten von Lehmmauerwerk berücksichtigt und eine fundierte Grundlage für eine wirtschaftliche und zuverlässige Nachweisführung darstellt.
We discuss the non-linear stress–strain behavior of microcracked polycrystalline ceramics under uniaxial tension and compression (displacement control).
Micromechanics explanation and modeling of its basic features, such as non-linearity and hysteresis in stress–strain curves, are developed, with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles in tension and crack sliding playing a critical role in compression. Experiments involving complex loading histories are explained, and themodel is shown to reproduce the basic features of the observed stress–strain curves.
We report about a joint project aiming at the digitalization of a lab course in materials testing. The undergraduate students were asked to prepare samples of a precipitation hardened aluminum alloy and characterize them using hardness and tensile tests. In a first step, we developed the frames for the digital labor notebook using eLabFTW. The primary data and the relevant metadata of each run were saved in a central database and made available for analysis and report issues. The whole set of results produced in a course was made available in the database. This database can be improved and serve as an open repository for data on this specific alloy.
The logical frame for the joint project was provided by the PMD Core Ontology (PMDco), a mid-level ontology that enables the representation and description of processes and process chains in an MSE-specific manner, ensuring full traceability of generated data. For the digitalization of this lab course, the tensile test ontology (TTO) was applied which is designed as a module of the PMDco using strongly related semantic concepts.
The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes.
Ananion-dopedaluminiumchlorofluoride AlCl0.1F2.8(OTeF5)0.1(ACF-teflate) was synthesized.The material contains pentafluor-oorthotellurate(teflate)groups, which mimic fluoride ions electronically, but are sterically more demanding. They are embedded into the amorphous structure. The latter was studied by PDF analysis, EXAFS data and MAS NMR spectroscopy. The mesoporous powder is a Lewis superacid, and ATR-IR spectra of adsorbed CD3CN reveal a blue-shift of the adsorption band by73 cm-1, which is larger than the shift for SbF5. Remarkably,ACF-teflate catalyzes dehydrofluorination reactions of mono-fluoroalkanes to yield olefins in C6D6. In these cases,no Friedel-Crafts products were formed.
Anhand der Wirksumme ist eine Abschätzung des legierungsabhängigen Einflusses auf den Korrosionswiderstand gegen chloridhaltige Medien möglich. Die berechneten Werte sind nur bei optimaler Wärmebehandlung und Verarbeitung zutreffend.
Die Anwendung einer einfachen Formel unter Berücksichtigung von Chrom, Molybdän und Stickstoff ist in der Regel völlig ausreichend. Das daraus abgeleitete Ranking von Werkstoffen ist für diverse technische Regelwerke und zur Unterstützung der Werkstoffauswahl geeignet.
Für die Warenein-/Ausgangskontrolle ist die alleinige Feststellung der Wirksumme unzureichend. Ergänzende Korrosionsuntersuchungen/-prüfungen zur Beschreibung des Korrosionswiderstandes sind dafür notwendig. Gleiches gilt für die Beurteilung von Schadensfällen. Hier sind Verarbeitung, Einsatzbedingungen und die Konstruktion von ausschlaggebender Bedeutung.
Die Bedingungen für den schadensfreien Einsatz nichtrostender Stähle, nicht nur bei Schweißverbindungen, sind:
1) Die Passivschicht muss sich vollständig ausbilden können.
Voraussetzung dafür sind glatte, blanke, saubere Oberfläche, eine gleichmäßige Elementverteilung, wenig Ausscheidungen und Verunreinigungen. Eine mögliche Beeinflussung der Gefügeausbildung durch Warmumformung und durch die
schweißtechnische Verarbeitung sind zu beachten. Anlauffarben
müssen durch geeignete geeignete chemische bzw. mechanische Nachbehandlung entfernt werden.
2) Die Repassivierung von Defektstellen unter Einsatzbedingungen muss möglich sein, was durch geeignete Werkstoffauswahl und die Legierungszusammensetzung sicherzustellen ist. Unplanmäßige Betriebszustände oder Störungen können kritische Systemzustände hervorrufen, die die Repassivierung beeinträchtigen oder verhindern.
Eine geeignete Unterhaltsreinigung ist sicherzustellen.
Neubewertung von metallenen Dach- und Fassadenmaterialien unter Dauerhaftigkeits- und Umweltaspekten
(2023)
Metallene Dach- und Fassadenmaterialien unterliegen nach ihrer Installation infolge von Korrosions- und Abschwemmprozessen einem Abtrag von Metallionen. Durch Regenereignisse gelangen diese in umliegende Gewässer und Böden. Die verwendeten metallenen Werkstoffe, wie z.B. Kupfer und Zink bilden zeitabhängig schützende Deckschichten aus, die die Dauerhaftigkeit der Werkstoffe gewährleisten und damit den Austrag von Metallionen signifikant begrenzen. Die Geschwindigkeit der Deckschichtbildung sowie die erreichte Schutzwirkung sind von verschiedenen Umwelteinflüssen und klimatischen Bedingungen abhängig. Diese haben sich in den letzten Jahrzehnten in Europa stark verändert, so dass es einer aktuellen Datenbasis für die Bewertung der Dauerhaftigkeit und der Umweltauswirkungen bedarf. Im Rahmen eines Forschungsvorhabens werden aktuell Feldstudien zur Ermittlung des Runoffs und der Schutzwirkung der gebildeten Deckschichten durchgeführt. Ergänzt werden diese durch Laborversuche mit künstlicher Beregnung.
Bedingung für den schadensfreien Einsatz nichtrostender Stähle ist die vollständige Ausbildung der Passivschicht. Voraussetzung dafür sind glatte, blanke, saubere Oberfläche, eine gleichmäßige Elementverteilung, wenig Ausscheidungen und Verunreinigungen. Eine mögliche Beeinflussung der Gefügeausbildung durch Warmumformung und durch die schweißtechnische Verarbeitung sind zu beachten. Anlauffarben müssen durch geeignete geeignete chemische bzw. mechanische Nachbehandlung entfernt werden. Eine ausreichende Nachbehandlung kann durch elektrochemische Prüfverfahren ebenso sichergestellt werden wie mittels der KorroPad-Prüfmethode. Letzte ist einfach und schnell in der Anwendung und ermöglicht es dem Verarbeiter, die Geeignetheit einer Nachbehandlung zu überprüfen.
Im Vortrag werden die wesentlichen Grundlagen zum Verständnis der Korrosion metallener Werkstoffe in komprimierter Form vorgestellt. Der Schwerpunkt liegt auf der Betrachtung der atmosphärischen Korrosion und den sich daraus ergebenden Anforderungen an den Korrosionsschutz insbesondere für den Bereich Verpackungen.
Anhand der Wirksumme ist eine Abschätzung des legierungsabhängigen Einflusses auf den Korrosionswiderstand gegen chloridhaltige Medien möglich. Die berechneten Werte sind nur bei optimaler Wärmebehandlung und Verarbeitung zutreffend.
Die Anwendung einer einfachen Formel unter Berücksichtigung von Chrom, Molybdän und Stickstoff ist in der Regel völlig ausreichend. Das daraus abgeleitete Ranking von Werkstoffen ist für diverse technische Regelwerke und zur Unterstützung der Werkstoffauswahl geeignet.
Für die Warenein-/Ausgangskontrolle ist die alleinige Feststellung der Wirksumme unzureichend. Ergänzende Korrosionsuntersuchungen/-prüfungen zur Beschreibung des Korrosionswiderstandes sind dafür notwendig. Gleiches gilt für die Beurteilung von Schadensfällen. Hier sind Verarbeitung, Einsatzbedingungen und die Konstruktion von ausschlaggebender Bedeutung.
Argyrodite-type materials have lately sparked a lot of research interest due to their thermoelectric properties.One promising candidate is canfieldite (Ag8SnS6), which has a Pna21 orthorhombic crystal structure at room temperature (RT). Recently, a new low-temperature (LT) phase transition of canfieldite at 120K has been found. Here, we investigate structural, vibrational and thermodynamic properties of Ag8SnS6 at room- and low-temperature employing density functional theory (DFT) and lattice dynamics computations. Thermal properties calculations were based on the quasi-harmonic approximation (QHA) as implemented in phonopy. We achieve good agreement with experiments. Thermal properties such as the constant-pressure heat capacity (Cp) and thermal conductivity are very close to experimental measurements. Furthermore, we compared RT and LT Ag8SnS6 Grüneisen parameters with argyrodites analogues, Ag8XS6 (X = Sn, Si, Ge), to arrive at an improved
Argyrodite-type materials have lately sparked a lot of research interest due to their thermoelectric properties. One promising candidate is canfieldite (Ag8SnS6), which has a Pna21 orthorhombic crystal structure at room temperature (RT). Recently, Slade group found a new low-temperature (LT) phase transition of canfieldite at 120K. Therefore, we investigate structural, vibrational and thermodynamic properties of Ag8SnS6 at room- and low-temperature employing density-functional theory (DFT) and lattice dynamics computations. Thermal properties calculations were based on the quasi-harmonic approximation (QHA) as implemented in phonopy. We achieve good agreement with experiments. Lattice parameters were overestimated by 2%, and thermal properties such as the constant-pressure heat capacity Cp are very close to experimental measurements. Our simulations also reveal a possible new phase transition at around 312 K. Furthermore, we compared RT and LT Ag8SnS6 Grüneisen parameters with some argyrodites analogues, Ag8TS6 (T = Si, Ge, Ti and Sn), finding a relationship between the anharmonicity and low thermal conductivity.
Argyrodite-type materials have lately sparked a lot of research interest due to their thermoelectric properties. One promising candidate is canfieldite (Ag8SnS6), which has a Pna21 orthorhombic crystal structure at room temperature (RT). Recently, experimentalists have found a new low-temperature (LT) phase transition of canfieldite at 120K. Therefore, we investigate structural, vibrational and thermodynamic properties of Ag8SnS6 at room- and low-temperature employing density-functional theory (DFT) and lattice dynamics computations. Thermal properties calculations were based on the quasi-harmonic approximation (QHA) as implemented in phonopy. We achieve good agreement with experiments. Lattice parameters were overestimated by 2%, and thermal properties such as the constant-pressure heat capacity Cp are very close to experimental measurements. Our simulations also reveal a possible new phase transition at around 312 K. Furthermore, we compared RT and LT Ag8SnS6 Grüneisen parameters with some argyrodites analogues, Ag8TQ6 (T = Si, Ge, Ti and Sn; Q = S, Se), finding a relationship between the anharmonicity and low thermal conductivity.
This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy.
This work investigates the microstructure formed in friction stir welds of FCC alloys, focused on two multiprincipal alloys: a CoCrFeMnNi high-entropy alloy (HEA) and a CoCrNi medium-entropy alloy (MEA). A commercial stainless steel AISI 304 is used for comparison. The largest nugget was formed in the MEA, while the smallest was formed in the HEA. Grain refinement occurs in the stirred zone in all welds. Discontinuous dynamic recrystallisation is the predominant restoration mechanism during friction stir welding of the three investigated alloys. A sharp decrement in the Σ3 boundary fraction occurs in the stirred zone of the AISI 304 and HEA welds, while comparable values with the base metal are found for the MEA weld. The peak in the maximum index of crystallographic texture is observed on the advancing side of the stirred zone of the AISI 304 weld. A strong <001> θ-fibre texture is formed in the advancing side of the nugget in the AISI 304 from a well-established {123} <634> S-type texture in the base metal. Multiple crystallographic texture components without specific fibres are identified in most regions of the welds, indicating the complex shear path history during friction stir welding.