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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.
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.
Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. However, the “what is my material” barrier hinders further commercialization. X-ray photoelectron spectroscopy (XPS) is considered as a method of choice for the determination of the elemental and chemical composition. In this work the influence of the morphology of graphene particles on the XPS results is studied and investigated as a function of X-ray energy, using conventional XPS with Al K𝜶 radiation and hard X-ray photoemission spectroscopy (HAXPES) using Cr K𝜶 radiation. Thereby, the information depth is varied between 10 and 30 nm. For this purpose, two commercial powders containing graphene nanoplatelets with lateral dimensions of either ≈100 nm or in the micrometer range are compared. These larger ones exist as stack of graphene layers which is inspected with scanning electron microscopy. Both kinds of particles are then functionalized with either oxygen or fluorine. The size of the graphene particles is found to influence the degree of functionalization. Only the combination of XPS and HAXPES allows to detect the functionalization at the outermost surface of the particles or even of the stacks and to provide new insights into the functionalization process.
Creep-resistant steels such as the 13CrMoV9-10, used in the construction of thick-walled pressure vessels, are most commonly submerged arc welded (SAW). These steels can develop stress relief cracks (SRC) if the mandatory post weld heat treatment (PWHT) is performed improperly. Current PWHT parameters, such as heating rate and holding time at a specific holding temperature, are based on both empirical experience and conventional free shrinking welding experiments to characterize the SRC-susceptibility of the weld. These cannot adequately depict the higher residual stresses caused by the structurally induced stiffness of the surrounding construction. This study discusses the development of a repeatable, precise, and time-efficient methodology to study the effects of different stress levels and heating rates on the SRC susceptibility of the coarse grain heat-affected zone (CGHAZ). For that purpose, samples were thermically treated to simulate a coarse grain heat-affected zone (CGHAZ) and subsequently exposed to representative levels of stress during the heating phase of a PWHT. The recorded stress and heating rate–dependent strains were mathematically analyzed via curve tracing/calculus to identify interdependent effects. This procedure facilitates the measurement of material characteristics such as carbide growth on grain boundaries at the µm-scale via an integrated value over the entire sample volume. The first and second derivatives show a slight, precipitate-dependent, increase in hardness of the sample, depending on the heating rate and applied stress. This new methodology generates an improved assessment of the SRC susceptibility of SAW microstructures of creep-resistant CrMoV steels.
Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure
(2023)
The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure, and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. In this work, a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves is proposed to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. To demonstrate this effect, the generalized law of the hydrogen solubility is parameterized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments.
A systematic study on a face‐centered cubic‐based compositionally complex alloy system Al–Co–Cr–Cu–Fe–Ni in its single‐phase state is carried out, where a mother senary compound Al₈Co₁₇Cr₁₇Cu₈Fe₁₇Ni₃₃ and five of its suballoys, obtained by removing one element at a time, are investigated and exhaustively analyzed determining the contribution of each alloying element in the solid solution. The senary and the quinaries are compared using experimental techniques including X‐ray absorption spectroscopy, X‐ray diffraction, transmission electron microscopy, and first principles hybrid Monte Carlo/molecular dynamics simulations. Chemical short‐range order and bond length distances have been determined both at the experimental and computational level. Electronic structure and local atomic distortions up to 5.2 Å have been correlated to the microhardness values. A linear regression model connecting hardness with local lattice distortions is presented.
Prolonging structural integrity—Fatigue of scarf repairs for wind turbine blade shell applications
(2023)
The influence of scarf repair variables on the mechanical properties of glass fiber reinforced polymer sandwich structures is examined for the application of wind turbine blade shell repairs. Reference shell specimens are tested under fully-reversed cyclic loading to understand the fatigue behavior of the sub-component structure within a range of in-service loads, to which shell specimens with a scarf joint repair are compared. A fatiguesuperior repair material is shown to improve the fatigue behavior of the repaired structures compared to the reference specimens. In separating layup and geometry, damage development is examined on the subcomponent scale for a structural understanding of a scarf repair using in-situ digital image correlation-based strain field measurements as well as passive thermography. Within scarf repair variables, the geometry is shown to play a larger role than layup in the fatigue performance of the repaired structure.
Laser melting manufacturing of large elements of lunar regolith simulant for paving on the Moon
(2023)
The next steps for the expansion of the human presence in the solar system will be taken on the Moon. However, due to the low lunar gravity, the suspended dust generated when lunar rovers move across the lunar soil is a significant risk for lunar missions as it can affect the systems of the exploration vehicles. One solution to mitigate this problem is the construction of roads and landing pads on the Moon. In addition, to increase the sustainability of future lunar missions, in-situ resource utilization (ISRU) techniques must be developed. In this paper, the use of concentrated light for paving on the Moon by melting the lunar regolith is investigated. As a substitute of the concentrated sunlight, a high-power CO2 laser is used in the experiments. With this set-up, a maximum laser spot diameter of 100 mm can be achieved, which translates in high thicknesses of the consolidated layers. Furthermore, the lunar regolith simulant EAC-1A is used as a substitute of the actual lunar soil. At the end of the study, large samples (approximately 250 × 250 mm) with interlocking capabilities were fabricated by melting the lunar simulant with the laser directly on the powder bed. Large areas of lunar soil can be covered with these samples and serve as roads and landing pads, decreasing the propagation of lunar dust. These manufactured samples were analysed regarding their ineralogical composition, internal structure and mechanical properties.
Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy
(2023)
We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production.
Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies.
Aqueous Dispersions of Polypropylene: Toward Reference Materials for Characterizing Nanoplastics
(2023)
Microplastics and nanoplastics pollute the natural environment all over the world, but the full extent of the hazards posed by this waste is unclear. While research on microplastics is well advanced, little work has been done on nanoplastics. This discrepancy is mainly due to the lacking ability to detect nanoplastics in biologically and environmentally relevant matrices. Nanoplastics reference materials can help the development of suitable methods for identifying and quantifying nanoplastics in nature. The aim is to synthesize nanoplastics made from one of the most commonly used plastics, namely polypropylene. An easy way to produce long-term stable aqueous dispersions of polypropylene nanoparticles (nano polypropylene) is reported. The nanoplastic particles, prepared by mechanical breakdown, show a mean hydrodynamic diameter of D h = 180.5 ± 5.8 nm and a polydispersity index of PDI = 0.084 ± 0.02. No surfactant is needed to obtain dispersion which is stable for more than 6 months. The colloidal stability of the surfactant-free nano polypropylene dispersions is explained by their low zeta potential of 𝜻 = −43 ± 2 mV.
We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves a transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1-x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms while degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed with in-situ and ex-situ scattering and diffraction, as well as X -ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on a metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1-x-struvites exhibit high surface areas and pore volumes (240 m²g-1 and 0.32 cm-3 g-1 for Mg and 90 m²g-1 and 0.13 cm-3 g-1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further applications, for instance, in (electro)catalysis.
Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects.
The rational design of next generation molecular and nanoscale reporters and the comparison of different emitter classes require the determination of the fluorometric key performance parameter fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. Main prerequisites for reliable Φf measurements, which are for transparent luminophore solutions commonly done relative to a reference, i.e., a fluorescence quantum yield standard of known Φf, are reliable and validated instrument calibration procedures to consider wavelength-, polarization-, and time-dependent instrument specific signal contributions, and sufficiently well characterized fluorescence quantum yield standards. As the standard’s Φf value directly contributes to the calculation of the sample’s Φf, its accuracy presents one of the main sources of uncertainty of relative Φf measurements. To close this gap, we developed a first set of 12 fluorescence quantum yield standards, which absorb and emit in the wavelength region of 330−1000 nm and absolutely determined their Φf values with two independently calibrated integrating sphere setups.
Criteria for standard selection and the configuration of these novel fluorescence reference materials are given, and the certification procedure is presented including homogeneity and stability studies and the calculation of complete uncertainty budgets for the certified Φf values. The ultimate goal is to provide the community of fluorescence users with available reference materials as a basis for an improved comparability and reliability of quantum yield data since the measurement of this spectroscopic key property is an essential part of the characterization of any new emitter.
Outer membrane lipopolysaccharides (LPS) play a crucial role in determining attachment behavior and pathogenicity of bacteria. The aim of this study was to develop a simple procedure for anchoring bacterial lipopolysaccharides to polystyrene (PS) microparticles as a model system for in situ attachment studies. By using a swellcapture methodology, commercially available LPS of Pseudomonas aeruginosa (strain ATCC 27316 serotype 10.22) was anchored onto PS microparticles in a proof-of-concept study. A detailed chemical and morphological characterization has proven the success of LPS incorporation. It was shown that the coverage and structure of the LPS film was concentration dependent. The procedure can easily be adapted to LPS of other bacterial strains to generate a synthetic model toolkit for attachment studies.
Bacterial biofilms pose serious problems in medical and industrial settings. One of the major societal challenges lies in the increasing resistance of bacteria against biocides used in antimicrobial treatments, e.g., via overabundant use in medicine, industry, and agriculture or cleaning and disinfection in private households. Hence, new efficient bacteria-repellent strategies avoiding the use of biocides are strongly desired. One promising route to achieve bacteria-repellent surfaces lies in the contactless and aseptic large-area laser-processing of technical surfaces. Tailored surface textures, enabled by different laser-processing strategies that result in topographic scales ranging from nanometers to micrometers may provide a solution to this challenge. This article presents a current state-of-the-art review of laser-surface subtractive texturing approaches for controlling the biofilm formation for different bacterial strains and in different environments. Based on specific properties of bacteria and laser-processed surfaces, the challenges of anti-microbial surface designs are discussed, and future directions will be outlined.
Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability.
Materials that support natural biodiversity on their surfaces can compensate for human activities that have a negative impact on nature and thus contribute to a carbon-neutral and nature-positive world. Specifically designing bioreceptive materials which favor the growth of biofilms on their surface is an approach complementing conventional, macroscopic green façades. But what exactly characterizes a bioreceptive substrate and how do biofilm and substrate interact? How and why does a spontaneous colonization and the formation of biofilms take place? What are biofilms and how can they be established in a laboratory setting? How can this existing knowledge be transferred to the artificial stone concrete so that this material can be tuned to increase (or decrease) its bioreceptivity?
This review paper aims at summarizing the existing state of knowledge on bioreceptive concrete and pointing out inconsistencies and contradictions which can only be removed by more interdisciplinary research in the field.
Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys.
Fused filament fabrication (FFF) is a material extrusion-based technique often used in desktop 3D printers. Polymeric filaments are melted and are extruded through a heated nozzle to form a 3D object in layers. The extruder temperature is therefore a key parameter for a successful print job but also one of the main emission driving factors as harmful pollutants (e.g., ultrafine particles) are formed by thermal polymer degradation. The awareness of potential health risks has increased the number of emission studies in the past years. However, studies usually refer their calculated emission data to the printer set extruder temperature for comparison purposes. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperature and found significant temperature deviations to the displayed set temperature among printer models. Our result shows that printing the same filament feedstocks with three different printer models and with identical printer set temperature resulted in a variation in particle emission of around two orders of magnitude. A temperature adjustment has reduced the variation to approx. one order of magnitude. Thus, it is necessary to refer the measured emission data to the actual extruder temperature as it poses a more accurate comparison parameter for evaluation of the indoor air quality in user scenarios or for health risk assessments.
AbstractThis work addresses the critical need for multifunctional materials and substrate‐independent high‐precision surface modification techniques that are essential for advancing microdevices and sensing elements. To overcome existing limitations, the versatility of mussel‐inspired materials (MIMs) is combined with state‐of‐the‐art multiphoton direct laser writing (DLW) microfabrication. In this way, 2D and 3D MIM microstructures of complex designs are demonstrated with sub‐micron to micron resolution and extensive post‐functionalization capabilities. This study includes polydopamine (PDA), mussel‐inspired linear, and dendritic polyglycerols (MI‐lPG and MI‐dPG), allowing their direct microstructure on the substrate of choice with the option to tailor the patterned topography and morphology in a controllable manner. The functionality potential of MIMs is demonstrated by successfully immobilizing and detecting single‐stranded DNA on MIM micropattern and nanoarray surfaces. In addition, easy modification of MIM microstructure with silver nanoparticles without the need of any reducing agent is shown. The methodology developed here enables the integration of MIMs in advanced applications where precise surface functionalization is essential.
The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
This paper presents a novel approach for developing sustainable building materials through Sequential Learning. Data sets with a total of 1367 formulations of different types of alkali-activated building materials, including fly ash and blast furnace slag-based concrete and their respective compressive strength and CO2-footprint, were compiled from the literature to develop and evaluate this approach. Utilizing this data, a comprehensive computational study was undertaken to evaluate the efficacy of the proposed material design methodologies, simulating laboratory conditions reflective of real-world scenarios. The results indicate a significant reduction in development time and lower research costs enabled through predictions with machine learning. This work challenges common practices in data-driven materials development for building materials. Our results show, training data required for data-driven design may be much less than commonly suggested. Further, it is more important to establish a practical design framework than to choose more accurate models. This approach can be immediately implemented into practical applications and can be translated into significant advances in sustainable building materials development.
Wire arc additive manufacturing (WAAM) enables the efficient production of weight-optimized modern engineering structures. Further increases in efficiency can be achieved by using high-strength structural steels. Commercial welding consumables for WAAM are already available on the market. Lack of knowledge and guidelines regarding welding residual stress and component safety during production and operation leads to severely limited use for industry applications. The sensitive microstructure of high-strength steels carries a high risk of cold cracking; therefore, residual stresses play a crucial role. For this reason, the influences of the material, the WAAM process, and the design on the formation of residual stresses and the risk of cold cracking are being investigated. The material used has a yield strength of over 800 MPa. This strength is adjusted via solid solution strengthening and a martensitic phase transformation. The volume expansion associated with martensite formation has a significant influence on the residual stresses. The focus of the present investigation is on the additive welding parameters and component design on their influence on hardness and residual stresses, which are analyzed by means of X-ray diffraction (XRD). Reference specimens (hollow cuboids) are welded fully automated with a systematic variation of heat control and design. Welding parameters and AM geometry are correlated with the resulting microstructure, hardness, and residual stress state. Increased heat input leads to lower tensile residual stresses which causes unfavorable microstructure and mechanical properties. The component design affects heat dissipation conditions and the intensity of restraint during welding and has a significant influence on the residual stress.
Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement.
Aero-engine turbine disks are safety-relevant components which are operated under high thermal and mechanical stress conditions. The actual part qualification and certification procedures make use of spin-tests conducted on production-similar disks. While these tests provide, on the one hand, a reliable definition of the critical conditions for real components, on the other hand they represent a relevant cost item for engine manufacturers. The aim of this work is to present two alternative burst speed assessment methods under development based on the Failure Assessment Diagram (FAD) and a global stability criterion, respectively. In the scope of the fracture mechanics assessment, the failure modes hoop-burst and rim-peeling are investigated with semicircular surface cracks modelled at the critical regions on the turbine disk. The comparison of the predicted critical rotational speed shows good agreement between the assessment methods.
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.