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Paper des Monats
- ja (1)
Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables.
Recent publications indicate that the order of electrochemical anodization (before or after the laser processing step) plays an important role for the response of bone-forming osteoblasts—an effect that can be utilized for improving permanent dental or removable bone implants. For exploring these different surface functionalities, multimethod morphological, structural, and chemical characterizations are performed in combination with electrochemical pre- and postanodization for two different characteristic microspikes covered by nanometric laser-induced periodic surface structures on Ti–6Al–4V upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ≈1 ps pulse duration, 67 and 80 kHz pulse repetition frequency) at two distinct sets of laser fluence and beam scanning parameters. This work involves morphological and topographical investigations by scanning electron microscopy and white light interference microscopy, structural material examinations via X-ray diffraction, and micro-Raman spectroscopy, as well as near-surface chemical analyses by X-ray photoelectron spectroscopy and hard X-ray photoelectron spectroscopy. The results allow to qualify the mean laser ablation depth, assess the spike geometry and surface roughness parameters, and provide new detailed insights into the near-surface oxidation that may affect the different cell growth behavior for pre- or postanodized medical implants.
The current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis.
In this study, we investigated the diverse range of materials used for sizing in Iranian paper manuscripts during the Timurid (fifteenth century) to Safavid (sixteenth century) and Qajar (nineteenth century) periods. Our approach combined historical analysis with scientific examination of reconstructed sizings. We reconstructed 15 sizing materials based on identified Persian historical recipes and analysed their physical, optical, and spectral characteristics. Additionally, we assessed their behaviour against the mould fungus Aspergillus flavus. The results revealed distinctive properties for each sizing material, shedding light on their potential applications in paper preservation. Furthermore, our investigation demonstrated variations in hygroscopicity, thickness, grammage, and ash content post-sizing. The sizing materials also exhibited different effects on paper reflectance properties. Additionally, our study revealed insights into the impact of sizing on burnished papers, indicating that the mechanical process of burnishing did not significantly alter the chemical composition or spectral properties of the paper, with only minor changes in brightness observed in specific cases. All tested sizing materials supported varying levels of mould growth, indicating potential implications for paper conservation. Our findings provide valuable insights into the historical practices of Iranian paper sizing and offer practical considerations for the preservation of paper manuscripts.
Abstract. In power electronics, compound semiconductors with large bandgaps, like silicon carbide (SiC), are increasingly being used as material instead of silicon. They have a lot of advantages over silicon but are also intolerant of nanoscale material defects, so that a defect inspection with high accuracy is needed. The different defect types on SiC samples are measured with various measurement methods, including optical and tactile methods. The defect types investigated include carrots, particles, polytype inclusions and threading dislocations, and they are analysed with imaging ellipsometry, coherent Fourier scatterometry (CFS), white light interference microscopy (WLIM) and atomic force microscopy (AFM). These different measurement methods are used to investigate which method is most sensitive for which type of defect to be able to use the measurement methods more effectively. It is important to be able to identify the defects to classify them as critical or non-critical for the functionality of the end product. Once these investigations have been completed, the measurement systems can be optimally distributed to the relevant defects in further work to realize a hybrid analysis of the defects. In addition to the identification and classification of defects, such a future hybrid analysis could also include characterizations, e.g. further evaluation of ellipsometric data by using numerical simulations.
Rotational rheometry test of Portland cement-based materials - A systematic literature review
(2024)
This study systematically reviews 62 papers on the use of rotational rheometry to assess the fresh state behavior of Portland cement-based materials. The research highlights the wide variation in test methods and aims to provide a comprehensive overview. Findings reveal that 50.0% of studies employed vane geometry, despite its limitations in providing transformation equations. Regarding dynamic shearing tests, 67.0% followed a consensus using a pre-shearing step and a step-wise routine with stabilization times ≥ 10 s. While the Bingham model is commonly used, the study emphasizes the importance of considering shear-thinning behavior in cementitious materials. Models like Herschel-Bulkley and modified Bingham may be more appropriate. This review offers insights into testing conditions for rotational rheometry of cementitious materials, serving as a foundation for future research in the field.
For the hydrogen-based energy economy of tomorrow, the construction of the necessary infrastructure will play a central role. Most materials used to date, such as welded steels, can be prone to hydrogen embrittlement under certain conditions. This includes the classic delayed cold cracking during welding as well as degradation phenomena during service of components in hydrogen-containing environment. For the evaluation of any hydrogen effect, for example, on the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. In the case of weld seams, the carrier gas hot extraction (CGHE) according to ISO 3690 is meanwhile state-of-the-art. CGHE is based on accelerated hydrogen degassing due to the thermal activation of hydrogen at elevated temperatures. In addition to the quantification of hydrogen, thermal desorption analysis (TDA) with varying heating rates can be used to determine and evaluate the hydrogen trapping at microstructural defects in the material. For both techniques, experimental and metrological influences must be considered, which have a major effect on the result. For example, ISO 3690 suggests different sample geometries and minimum extraction times for CGHE. This study summarizes the results and experiences of numerous investigations at the Federal Institute for Materials Research and Testing (BAM) with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding the influence of the sample surface (polished/welded), measurement accuracy depending on the sample volume and the insufficient monitoring of the effect of PI control on the extraction temperature. A deviating extraction temperature from the target temperature can significantly falsify the measurement results. Based on the results, methods are shown which allow the desired extraction temperature to be reached quickly without physically interfering with the measuring equipment. This serves to significantly improve the reliability of the hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples is recommended for the heating procedure of choice to exclude possible undesired temperature influences before the measurement. The methods described can be transferred directly to industrial applications
Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering.
In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF.
Durch Auslagerungs- und elektrochemische Tests im Labor kann das Korrosionsverhalten verschiedener metallener Werkstoffe beurteilt werden. Aus den Versuchsergebnissen, die in verschiedenen synthetischen Geothermalwässern im Labor erzielt wurden, lassen sich die folgenden Schlussfolgerungen ziehen:
• Die Anfälligkeit für Spaltkorrosion wurde als wichtigster Aspekt für die Werkstoffqualifizierung ermittelt.
• Der niedriglegierte Stahl 25CrMo4 zeigte bei niedrigem Salzgehalt in MB-Geothermalwasser eine gleichmäßige Korrosion unterhalb der akzeptierten Schwelle von 0,3 mm/Jahr. Daher kann er als geeignet für geothermische Bedingungen mit niedrigem Salzgehalt angesehen werden, wie sie für MB getestet wurden. Es besteht keine Notwendigkeit, auf höherlegierte (teurere) Werkstoffe auszuweichen. Ein niedrigerer pH-Wert (wie bei LHD) führt zu Korrosionsraten oberhalb der akzeptablen Grenzwerte, so dass die niedriglegierten Werkstoffe nicht für Flüssigkeiten mit niedrigem pH-Wert geeignet sind.
• Stark salzhaltige Geothermalwässer erfordern höherlegierte Werkstoffe, da die Korrosionsrate von niedriglegiertem Stahl zu hoch ist.
• Der Duplexstahl X2CrNiMo22-5-3 und der Superduplexstahl X2CrNiMoCuWN25-7-4 wurden aufgrund ihrer kritischen Anfälligkeit für örtliche Korrosion in Form von Loch- und Spaltkorrosion unter Betriebsbedingungen nicht als geeignet für geothermische Anwendungen in Geothermalwässern mit einer mit NDB und ORG vergleichbaren Zusammensetzung angesehen.
• Der superaustenitische Stahl X1CrNiMoCu32-28-7 eignet sich für ORG und salzarme Wässer. In NDB-Geothermalwasser wurde er bei 100 °C als geeignet angesehen. Jedoch schränkt seine Anfälligkeit für Spaltkorrosion seine Anwendbarkeit ein. Neben seiner guten Korrosionsbeständigkeit ist sein Repassivierungsverhalten für seine begrenzte Anwendbarkeit in Geothermalwässern mit niedrigem pH-Wert verantwortlich.
• Die Nickelbasislegierung NiCr23Mo16Al wurde als geeignet erachtet und stellt eine sichere Option für den Einsatz in geothermischen Anlagen dar, selbst wenn mit stark salzhaltigem Geothermalwasser gearbeitet wird.
Durch Auslagerungs- und elektrochemische Tests im Labor kann das Korrosionsverhalten verschiedener metallener Werkstoffe beurteilt werden. Aus den Versuchsergebnissen, die in verschiedenen synthetischen Geothermalwässern im Labor erzielt wurden, lassen sich die folgenden Schlussfolgerungen ziehen:
• Die Anfälligkeit für Spaltkorrosion wurde als wichtigster Aspekt für die Werkstoffqualifizierung ermittelt.
• Der niedriglegierte Stahl 25CrMo4 zeigte bei niedrigem Salzgehalt in MB-Geothermalwasser eine gleichmäßige Korrosion unterhalb der akzeptierten Schwelle von 0,3 mm/Jahr. Daher kann er als geeignet für geothermische Bedingungen mit niedrigem Salzgehalt angesehen werden, wie sie für MB getestet wurden. Es besteht keine Notwendigkeit, auf höherlegierte (teurere) Werkstoffe auszuweichen. Ein niedrigerer pH-Wert (wie bei LHD) führt zu Korrosionsraten oberhalb der akzeptablen Grenzwerte, so dass die niedriglegierten Werkstoffe nicht für Flüssigkeiten mit niedrigem pH-Wert geeignet sind.
• Stark salzhaltige Geothermalwässer erfordern höherlegierte Werkstoffe, da die Korrosionsrate von niedriglegiertem Stahl zu hoch ist.
• Der Duplexstahl X2CrNiMo22-5-3 und der Superduplexstahl X2CrNiMoCuWN25-7-4 wurden aufgrund ihrer kritischen Anfälligkeit für örtliche Korrosion in Form von Loch- und Spaltkorrosion unter Betriebsbedingungen nicht als geeignet für geothermische Anwendungen in Geothermalwässern mit einer mit NDB und ORG vergleichbaren Zusammensetzung angesehen.
• Der superaustenitische Stahl X1CrNiMoCu32-28-7 eignet sich für ORG und salzarme Wässer. In NDB-Geothermalwasser wurde er bei 100 °C als geeignet angesehen. Jedoch schränkt seine Anfälligkeit für Spaltkorrosion seine Anwendbarkeit ein. Neben seiner guten Korrosionsbeständigkeit ist sein Repassivierungsverhalten für seine begrenzte Anwendbarkeit in Geothermalwässern mit niedrigem pH-Wert verantwortlich.
• Die Nickelbasislegierung NiCr23Mo16Al wurde als geeignet erachtet und stellt eine sichere Option für den Einsatz in geothermischen Anlagen dar, selbst wenn mit stark salzhaltigem Geothermalwasser gearbeitet wird.
The stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation can provide a certain degree of plasticity to Ceria-stabilized (Ce-TZP) zirconia-based composites. Characterizing and monitoring this phase transition on a millimeter-size range, within the bulk and in-situ remains a challenge. In this work, the mechanical behavior of Ce-TZP based composite was studied in tension, combining microscopy and synchrotron Xray refraction techniques. In contrast with microscopy methods, which only provide surface information, X-ray refraction radiography (SXRR) allowed the visualization of all the transformation bands, over the entire length and thickness of tested specimens, opening up new avenues for in-situ stress-induced t-m transformation studies.
Glycolide was polymerized in bulk by means of four different ROPPOC catalysts: tin(II) 2-ethylhexanoate (SnOct2), dibutyltin bis(pentafluoro-phenoxide) (BuSnOPF),zinc biscaproate (ZnCap), and zinc bis(pentafluoro-phenyl sulfide) (ZnSPF). The temperature was varied between 110 and 180°C and the time between 3 h and 7 days. For the few polyglycolides (PGAs) that were soluble extremely high molecular masses were obtained. The MALDI TOF mass spectra had all a low signal-to-noise ration and displayed the peaks of cyclic PGAs with a“saw-tooth pattern ”indicating formation of extended-ring crystallites in the mass range below m/z 2500. The shape of DSC curves varied considerably with catalyst and reaction conditions, whereas the long-distance values measured by SAXS were small and varied little with the polymeriza-tion conditions.
Thermal transient problems, essential for modeling applications like welding and additive metal manufacturing, are characterized by a dynamic evolution of temperature. Accurately simulating these phenomena is often computationally expensive, thus limiting their applications, for example for model parameter estimation or online process control. Model order reduction, a solution to preserve the accuracy while reducing the computation time, is explored. This article addresses challenges in developing reduced order models using the proper generalized decomposition (PGD) for transient thermal problems with a specific treatment of the moving heat source within the reduced model. Factors affecting accuracy, convergence, and computational cost, such as discretization methods (finite element and finite difference), a dimensionless formulation, the size of the heat source, and the inclusion of material parameters as additional PGD variables are examined across progressively complex examples. The results demonstrate the influence of these factors on the PGD model’s performance and emphasize the importance of their consideration when implementing such models. For thermal example, it is demonstrated that a PGD model with a finite difference discretization in time, a dimensionless representation, a mapping for a moving heat source, and a spatial domain non-separation yields the best approximation to the full order model.
A corrosion study is performed on six variations of titanium grade 5 (Ti6Al4V) samples. Samples are prepared in different conditions by variation of preanodization, postanodization, and picosecond-laser (ps-laser) surface treatment, while polished and anodized samples serve as reference. Microcones and nanosized periodic surface features are successfully produced on Ti6Al4V samples. The morphology and topography of the structures are visualized by scanning electron microscopy and white light interference microscopy. Furthermore, the relative electrochemically active surface area (ECSA) is determined for the ps-laser-treated samples. It is determined that the preanodized and laser-treated sample has 3.5 times larger ECSA than a polished sample, and that the laser-treated sample has 4.1 times larger area. Moreover, Tafel analysis is performed to determine the corrosion properties of the samples. It is shown that the corrosion resistance improves for both laser-structured samples after the anodization. To further study the surface of the samples, electrochemical impedance spectroscopy measurements are conducted. The study indicates that the ps-laser-treated and anodized Ti6Al4V is suitable to be used for the fabrication of bone screws and plates due to its improved corrosion resistance as compared to nonanodized samples.
AbstractIn this study, we compare the residual stress state in a laser powder bed fusion (PBF‐LB/M) AlSi10Mg alloy in the as‐built (AB) condition with that after two different heat treatments (265 °C for 1 h, HT1; and 300 °C for 2 h, HT2). The bulk residual stress (RS) is determined using synchrotron X‐ray diffraction (SXRD), and near‐surface profiles are determined using laboratory energy‐dispersive X‐ray diffraction (EDXRD). The EDXRD results do not reveal any notable difference between the conditions at a depth of 350 μm, suggesting that the machining process yields a comparable residual stress state in the near‐surface regions. On the other hand, the SXRD results show that HT1 is more effective in relieving the bulk RS. It is observed that HT1 reduces the RS state in both the aluminium matrix and the silicon network. In addtion, HT2 does not have a significant impact on relaxing the RS as‐built state of the matrix, although it does induce a reduction in the RS magnitudes of the Si phase. It is concluded that the heat treatment stress relieving is effective as long as the Si‐network is not disaggregated.
AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small.
It is proposed to model the experimentally observed weld pool boundary with superellipses (Lamé curves) and to find the unknown parameters of the curves using optimization methods. It has been shown experimentally that during laser welding of austenitic stainless steel with a thickness of 2 mm at a speed of 20 mm/s, the rear weld pool part has a shape close to triangular which can be accurately approximated by a superellipse. Analytical dependences of the trajectory and growth rate of the crystal and its cross-sectional area on the geometry of the rear weld pool part are obtained.
A method of solving the thermo-fluid dynamics problem is presented, enabling the prediction of the shape and dimensions of the weld pool during keyhole laser welding of thick plates. It is shown that the rear weld pool boundary can be satisfactorily approximated by a set of superellipses (Lamé curves). The presence of a convex rear weld pool boundary in the mid-plane has been observed experimentally and reproduced numerically. It was shown that in this zone the concentration of liquating impurities increases and the local solidification temperature decreases, contributing to the susceptibility to hot cracking.
The LOBSTER (Deringer et al., 2011;Maintz et al., 2013 ,2016 ;Nelson et al., 2020 ) software aids in extracting quantum-chemical bonding information from materials by projecting the plane-wave based wave functions from density functional theory (DFT) onto an atomic orbital basis. LobsterEnv, a module implemented in pymatgen (Ong et al., 2013) by some of the authors of this package, facilitates the use of quantum-chemical bonding information obtained from LOBSTER calculations to identify neighbors and coordination environments. LobsterPy is a Python package that offers a set of convenient tools to further analyze and summarize the LobsterEnv outputs in the form of JSONs that are easy to interpret and process. These tools enable the estimation of (anti) bonding contributions, generation of textual descriptions, and visualization of LOBSTER computation results. Since its first release, both LobsterPy and LobsterEnv capabilities have been extended significantly. Unlike earlier versions, which could only automatically analyze Crystal Orbital Hamilton Populations (COHPs) (Dronskowski & Blöchl, 1993), both can now also analyze Crystal Orbital Overlap Populations (COOP) (Hughbanks & Hoffmann, 1983) and Crystal Orbital Bond Index (COBI) (Müller et al., 2021). Extracting the information about the most important orbitals contributing to the bonds is optional, and users can enable it as needed. Additionally, bonding-based features for machinelearning (ML) studies can be engineered via the sub-packages “featurize” and “structuregraphs”. Alongside its Python interface, it also provides an easy-to-use command line interface (CLI) that runs automatic analysis of the computations and generates a summary of results and publication-ready figures. LobsterPy has been used to produce the results in Ngo et al. (2023), Chen et al. (2024), Naik et al. (2023), and it is also part of Atomate2 (2023) bonding analysis workflow for generating bonding analysis data in a format compatible with the Materials Project (Jain et al., 2013) API.
Beim Unterpulverschweißen sind die Prozessgeräusche ein Indikator für eine gute Fügequalität. Diese Beurteilung kann i.d.R. nur von einer erfahrenen Fachkraft durchgeführt werden. Eine kürzlich entwickelte künstliche Intelligenz kann automatisch das akustische Prozesssignal anhand vortrainierter Merkmale klassifizieren und die Fügequalität anhand des Geräuschs beurteilen. Der Algorithmus, einmal richtig trainiert, kann den Prüfaufwand beim Unterpulverschweißen deutlich reduzieren.
Die additive Fertigung mittels Schweißverfahren bietet große ökonomische Vorteile für eine ressourceneffiziente Bauteilherstellung. Offene Fragen bezüglich Homogenität, Anisotropie der Schweißgefüge und den damit verbundenen Bauteileigenschaften stehen einer wirtschaftlichen Verarbeitung oftmals im Wege. Finale Bauteilgeometrie und Oberflächengüte erfordern meist komplementäre subtraktive Fertigungsschritte. Werkstoffe für hochbelastbare Komponenten sind oftmals schwer spanbar. In einem Vorhaben der BAM und des ISAF wurde untersucht, wie die Modifikation der AM-Schweißzusätze und das ultraschallunterstützte Fräsen (US) die Zerspanungssituation verbessern. Der vorliegende Artikel stellt wesentliche Zusammenhänge zwischen Legierung, Gefüge und Zerspanung zweier schwer spanbarer Hochleistungslegierungen (FeNi und CoCr) dar. Großes Potenzial zeigte neben dem US die Modifikation mit Zr und Hf bei Zulegierung in das Schweißgut mittels Beschichtung von Massivdrähten bzw. Herstellung von Fülldrähten.
Abstract
In the post-processing of large maritime components, a considerable amount of waste in the form of milling and grinding chips is produced. At the same time, additive manufacturing technologies have shown great potential in producing high-volume parts for maritime applications, allowing novel design approaches and short lead times. In this context, this study presents a sustainable approach to recycle and use aluminium bronze waste material, generated during post-processing of large cast ship propellers, as feedstock for laser-powder directed energy deposition. The recycling technology used to produce powder batches is inductive re-melting in combination with ultrasonic atomization. The derived metal powders are characterized using digital image analysis, powder flowability tests, scanning electron microscopy as well as energy dispersive X-ray spectroscopy. Compared to conventional metal powders produced by gas atomization, the recycled material shows excellent sphericity and a powder size distribution with a higher content of finer and coarser particles. Metallographic sections of deposited additively produced specimens show an increased hardness and reduced ductility, but also competitive densities and higher yield and ultimate tensile strength compared to cast material. The process chain shows high potential for the maritime sector to enable circular and sustainable manufacturing.
Die neue Generation von bainitischen Schmiedestählen bietet auf der einen Seite ein erhebliches Festigkeitspotenzial, das es im Sinne des Leichtbaus auch für zyklisch belastete Sicherheitsbauteile zu heben gilt. Auf der anderen Seite geht mit dieser Festigkeitssteigerung im Vergleich zu Vergütungsstählen ein Verlust an Duktilität und Zähigkeit einher. Am Beispiel des Demonstratorbauteils Achsschenkel ging das Forschungsvorhaben der Frage nach, wie ein Freigabeprozess zu gestalten ist, damit das Festigkeitspotenzial der neuen Stähle zuverlässig ausgenutzt werden kann. Als Ergebnis wird eine Vorgehensweise dargestellt, die den Eigenschaften der neuen Generation von Schmiedestählen Rechnung trägt, um den sicheren Betrieb der Komponenten zu gewährleisten.
AbstractThe high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations.
The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles.
We present Jobflow, a domain-agnostic Python package for writing computational workflows tailored for high-throughput computing applications. With its simple decorator-based approach, functions and class methods can be transformed into compute jobs that can be stitched together into complex workflows. Jobflow fully supports dynamic workflows where the full acyclic graph of compute jobs is not known until runtime, such as compute jobs that launch
other jobs based on the results of previous steps in the workflow. The results of all Jobflow compute jobs can be easily stored in a variety of filesystem- and cloud-based databases without the data storage process being part of the underlying workflow logic itself. Jobflow has been intentionally designed to be fully independent of the choice of workflow manager used to dispatch the calculations on remote computing resources. At the time of writing, Jobflow
workflows can be executed either locally or across distributed compute environments via an adapter to the FireWorks package, and Jobflow fully supports the integration of additional workflow execution adapters in the future.
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.
Die Fourier-Transformations-Infrarot-Spektroskopie (FTIR-Spektroskopie) stellt eine innovative und wirkungsvolle Methode zur Charakterisierung von Bitumen und bitumenhaltigen Bindemitteln dar. So erlaubt die FTIRCharakterisierung nicht nur eine Bewertung des Alterungsfortschritts eines Bindemittels, sondern zudem auch die Identifizierung von im Bitumen enthaltenen Additiven und Schadstoffen wie z. B. polyzyklischen aromatischen Kohlenwasserstoffen (PAK), die Ableitung verschiedener physikalischer und chemischer Kennwerte sowie weiterhin eine Klassifizierung von Bindemitteln nach verschiedenen übergeordneten Eigenschaften wie der Raffinerie, dem Alterungszustand und auch der Alterungsempfindlichkeit.
In recent decades, the number of components in concrete has grown, particularly in formulations aimed at reducing carbon footprints. Innovations include diverse binders, supplementary cementitious materials, activators, concrete admixtures, and recycled aggregates. These developments target not only the enhancement of material properties but also the mitigation of the ecological and economic impacts of concrete — the most extensively used material by humankind. However, these advancements also introduce a greater variability in the composition of raw materials. The material’s behavior is significantly influenced by its nanoscale properties, which can pose challenges in accurate characterization. Consequently, there’s an increasing need for experimental tuning of formulations. This is accompanied by a more inconsistent composition of raw materials, which makes an experimental tuning of formulations more and more necessary. However, the increased complexity in composition presents a challenge in finding the ideal formulation through trial and error. Inverse design (ID) techniques offer a solution to this challenge by allowing for a comprehensive search of the entire design space to create new and improved concrete formulations. In this publication, we introduce the concept of ID and demonstrate how our open-source app “SLAMD” provides all necessary steps of the workflow to adapt it in the laboratory, lowering the application barriers. The intelligent screening process, guided by a predictive model, leads to a more efficient and effective data-driven material design process resulting in reduced carbon footprint and improved material quality while considering socio-economic factors in the materials design.
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 process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down.
Black writing materials of different types and compositions have varied in use over time and different geographical regions. With this paper, we would like to contribute to their study by listing and reviewing recipes for black writing inks that were in circulation in the Carolingian Empire as well as by referencing the archaeometric analyses of the black inks used in the manuscripts. The studies presented here that involved the humanities and natural sciences provide new insights into how the scholars of the early Medieval Ages organized manuscripts.
Die heute in der Anwendung befindlichen Bemessungskonzepte für Ermüdung von Beton stammen zum Teil noch aus den 1990er Jahren und sind speziell hinsichtlich hochfester Betone konservativ ausgelegt. Um die Vorteile von Türmen für Windkraftanlagen, vor allem auch aus hochfesten Betonen, im Zuge des geplanten Ausbaus der Windenergieversorgung in Deutschland wirtschaftlich nutzbar zu machen, müssen diese Bemessungskonzepte weiterentwickelt werden. Dafür sind umfangreiche Untersuchungen zur Ermittlung von Bruchlastwechselzahlen und zur Charakterisierung der Schädigungsentwicklung unter Ermüdungsbeanspruchung erforderlich. Allgemein anerkannte bzw. verbindliche Regelwerke oder Verfahren zur experimentellen Bestimmung der Ermüdungsfestigkeit (Bruchlastwechselzahlen) an Betonproben gibt es zurzeit aber nicht und die bisher durchgeführten Untersuchungen variieren in Parametern wie Probengeometrie, Probengröße und Prüffrequenz. Eine vergleichende Analyse der Ergebnisse der Studien und insbesondere die Übertragbarkeit auf bauteilrelevante Abmessungen ist auf dieser Grundlage nur sehr eingeschränkt möglich.
Admixtures are important constituents to enhance the performance of concrete. They allow for more efficient use of binders which can mitigate negative environmental impacts from producing cement-based materials. Commonly used rheology modifying agents like polycarboxylate ethers or cellulose ethers are synthetic or semi-synthetic, respectively. This requires additional energy consumption for their production and global supply chains particularly for many developing regions, which will be large consumers of concrete in the future. However, many locally available bio-based polysaccharides could be effectively used instead. These polymers are often overlooked by engineers and scientists due to their limited distribution and inherent complexity, yet they represent an underleveraged source of precursors for admixtures. This study investigates the action mechanisms of some bio-based rheology modifying agents, i.e., acacia gum and miscanthus gum, and provides a comparison to a conventionally modified starch. The results show that the mechanism of action of these polymers is closely related to the composition of the mixture, mixing regime, and the composition of the aqueous phase. Depending on the agent, either plasticizing or stabilizing effects on rheology can be revealed.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
Im Additive Manufacturing Verfahren Directed Energy Deposition (DED) wird bei der Verarbeitung von Werkzeugstahl in der Regel reines Argon als Schutzgas verwendet. Dabei kann die Verwendung von speziellen Schutzgasgemischen, auch bei geringen Anteilen zugemischter Gase, durchaus die Bauteilqualität positiv beeinflussen.
In Vorarbeiten der Messer SE & Co. KGaA zeigte ein gewisser Sauerstoffanteil im Schutzgas die Tendenz, den Flankenwinkel von Schweißspuren beim DED zu verbessern. In der vorliegenden Studie wurde daher detailliert untersucht in wie weit unterschiedliche Schutzgasgemische einen Einfluss auf die Qualität sowie die geometrischen Eigenschaften der additiv gefertigten Strukturen des Werkzeugstahls 1.2709 beim Laser-DED ausüben. Es erfolgten zunächst Testschweißungen in Form von Einzelspuren mit unterschiedlichen Gemischen aus dem Basisschutzgas Argon mit geringen Anteilen verschiedener Gase. Dabei wurde der Einfluss der Zusätze auf die Spurgeometrie und Aufbauqualität untersucht. Auf Basis dieser Vorversuche wurde eine Auswahl vielversprechender Gasgemische getroffen und Detailuntersuchungen in Form von Spuren, Flächen und Quadern unter Zugabe verschiedener Mengen an Zusätzen durchgeführt. Zur Bewertung des Einflusses der Schutzgasbeimengungen wurden der Flankenwinkel, die Porosität und das Gefüge der Proben anhand metallografischer Schliffe untersucht. Es zeigte sich, dass eine Zugabe von geringen Anteilen an Zusätzen zunächst zu einer Vergrößerung des Flankenwinkels im Vergleich zu reinem Argon führt. Mit steigendem Anteil der Gase nimmt dieser Winkel jedoch ab. So kann je nach Menge des zugesetzten Gases eine individuelle Benetzung des aufgetragenen Materials an der Oberfläche erreicht werden. Auch die Porosität ließ sich durch Schutzgasgemische beeinflussen und zeigt ein abweichendes Verhalten im Vergleich zu reinem Argon.
In this study, a wound dressing composed of an alginate dialdehyde−gelatin (ADA-GEL) hydrogel incorporated by astaxanthin (ASX) and 70B (70:30 B2O3/CaO in mol %) borate bioactive glass (BBG) microparticles was developed through 3D printing. ASX and BBG particles sti.ened the composite hydrogel construct and delayed its in vitro degradation compared to the pristine hydrogel construct, mainly due to their cross-linking role, likely arising from hydrogen bonding between the ASX/BBG particles and ADA-GEL chains. Additionally, the composite hydrogel construct could hold and deliver ASX steadily. The composite hydrogel constructs codelivered biologically active ions (Ca and B) and ASX, which should lead to a faster, more e.ective wound-healing process. As shown through in vitro tests, the ASX-containing composite hydrogel promoted fibroblast (NIH 3T3) cell adhesion, proliferation, and vascular endothelial growth factor expression, as well as keratinocyte (HaCaT) migration, thanks to the antioxidant activity of ASX, the release of cell-supportive Ca2+ and B3+ ions, and the biocompatibility of ADA-GEL. Taken together, the results show that the ADA-GEL/BBG/ASX composite is an attractive biomaterial to develop multipurposed wound-healing constructs through 3D printing.
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.
A giant Zn segregation transition is revealed using CALPHAD-integrated density-based modeling of segregation into Fe grain boundaries (GBs). The results show that above a threshold of only a few atomic percent Zn in the alloy, a substantial amount of up to 60 at.% Zn can segregate to the GB. We found that the amount of segregation abruptly increases with decreasing temperature, while the Zn content in the alloy required for triggering the segregation transition decreases. Direct evidence of the Zn segregation transition is obtained using high-resolution scanning transmission electron microscopy. Base on the model, we trace the origin of the segregation transition back to the low cohesive energy of Zn and a miscibility gap in Fe-Zn GB, arising from the magnetic ordering effect, which is confirmed by ab-initio calculations. We also show that the massive Zn segregation resulting from the segregation transition greatly assists with liquid wetting and reduces the work of separation along the GB. The current predictions suggest that control over Zn segregation, by both alloy design and optimizing the galvanization and welding processes, may offer preventive strategies against liquid metal embrittlement.
Viscosity modifying agents: Key components of advanced cement-based materials with adapted rheology
(2022)
Viscosity modifying agents (VMAs) are essential ingredients for the production of flowable cement-based materials. This paper presents an overview of commonly used VMAs and attempts to shed some light on the underlying physics at the origin of their mechanisms of action. The main molecular parameters of VMA controlling the rheological properties of the cement pore solution are highlighted. As the mechanisms of action of VMAs in cement-based materials are closely related to their affinity with the surface of cement particles, the adsorption of the main VMA types is discussed. The effect of VMAs on flow properties and stability of cement-based materials is presented for VMAs added without any superplasticizer, and then in systems incorporating both VMAs and superplasticizers. Finally, the effect of VMAs in enhancing concrete properties to secure adequate performance of different construction applications, and perspectives for future developments of novel cement-based materials made with VMAs are showcased.
FAIR (findable, accessible, interoperable and reusable) data usage is one of the main principals that many of the research and funding organizations include in their strategic plans, which means that following the main principals of FAIR data is required in many research projects. The definition of data being FAIR is very general. When implementing that for a specific application or project or even setting a standardized procedure within a working group, a company or a research community, many challenges arise. In this contribution, an overview about our experience with different methods and tools is outlined.
We begin with a motivation on potential use cases for the application of FAIR data with increasing complexity starting from a reproducible research paper over collaborative projects with multiple participants such as Round-Robin tests up to data-based models within standardization codes, applications in machine learning or parameter estimation of physics-based simulation models.
In a second part, different options for structuring the data (including metadata schema) are discussed. The first one is the openBIS system, which is an open-source lab notebook and PostgreSQL based data management system. A second option is a semantic representation using RDF based on ontologies for the domain of interest.
In a third section, requirements for workflow tools to automate data processing are discussed and their integration into reproducible data analysis is presented with an outlook on required information to be stored as metadata in the database.
Finally, the presented procedures are exemplarily demonstrated for the calibration of a temperature dependent constitutive model for additively manufactured mortar. A metadata schema for a rheological measurement setup is derived and implemented in an openBIS database. After a short review of a potential numerical model predicting the structural build-up behavior, the automatic workflow to use the stored data for model parameter estimation is demonstrated.
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.
Die Begriffe gefährlicher Stoff und Gefahrstoff werden häufig nicht unterschieden – in vielen Fällen resultieren aber durch den Kontext auch keine Missverständnisse. Tatsächlich bestehen aber Unterschiede – sowohl inhaltlich als auch bezüglich des Rechtsbereichs, der jeweils für sie gilt.
Stoffe sind gefährlich, wenn sie den Kriterien der CLP-Verordnung für physikalische Gefahren, Gesundheitsgefahren oder Umweltgefahren entsprechen. Sie werden dann im Sinne der CLP-Verordnung entsprechend eingestuft und es ergeben sich Pflichten bezüglich des Inverkehrbringens innerhalb der EU.
Gefahrstoffe sind in der Gefahrstoffverordnung definiert. Sie beinhalten die gefährlichen Stoffe und weitere nicht notwendigerweise als gefährlich eingestufte Stoffe. Das Ziel ist vor allem der Schutz von Beschäftigten bei Tätigkeiten mit Gefahrstoffen – es handelt sich also um eine Arbeitsschutzvorschrift.
Dieser Aufsatz stellt gefährliche Stoffe in ihrem Kontext vor, gibt einen Überblick über die Prinzipien und Rechtsfolgen sowie Hinweise auf weiterführende Informationen und stellt ihnen die Gefahrstoffe gegenüber.
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
Ring-expansion polymerizations (REPs) catalyzed by two cyclic tin catalysts (2-stanna-1.3-dioxa-4,5,6,7-dibenzazepine [SnBiph] and
2,2-dibutyl-2-stanna-1,3-dithiolane [DSTL]) are performed at 140 °C in bulk.
Small amounts (4 vol%) of chlorobenzene or other solvents are added to
facilitate transesterification reactions (ring–ring equilibration) in the solid poly(l-lactide)s. In the mass range up to m/z 13 000 crystalline PLAs displaying a so-called saw-tooth pattern in the MALDI-TOF mass spectra are obtained indicating the formation of extended-ring crystals. The characteristics of extended-ring crystallites and folded-ring crystallites are discussed. Furthermore, extremely high melting temperatures (Tm’s up to 201.2 °C) and melting enthalpies (𝚫Hm’s up to 106 J g−1)) are found confirming that 𝚫Hm max, the 𝚫Hm of a perfect crystal, is around or above 115 J g−1 in contrast to literature data.
We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is on the same scale as the scattering intensity, may offer a novel pathway for determining the degree of crystallinity.
The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from Q < 0.01 1/nm up to Q < 150 1/nm, with a resolution of 0.16 Angstrom. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to 8000^3 voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-Q behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts.
Microplastic particles with sizes between 1 to 1000 μm are widely distributed worldwide. Origin, transport pathways and fate are poorly known, as sampling, sample preparation and detection methods are major challenges. In addition, reference materials that mimic environmental particles are lacking. Most challenging is the yield of MP particle production and the need for resource-intensive grinding with liquid nitrogen. In this paper, a machine is designed to produce aged microplastic particles as reference material candidates with high yield. The machine is based on ultraviolet aging of a thin foil and mechanical fragmentation using clean air. An example of aging and fragmentation of high density polyethylene with additional physical and chemical characterization of shape, size, aging state by carbonyl index and density is presented.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process.
Optical Thermometry is popular among researchers because of its non-contact, high sensitivity, and fast measurement properties. In the present experiment, Er3+/Yb3+/K+ co-doped NaYF4 nanoparticles with different K+ concentrations were synthesized by solvothermal method, and the samples showed bright upconversion green emission under the excitation of a 980 nm laser. The powder X-ray diffractometer and transmission electron microscope were used to characterize the crystal structure and its surface morphology, respectively. The spectral characteristics of nanoparticles with K+ doping concentration from 10% to 30% (Molar ratio) were investigated by fluorescence spectroscopy, and it was observed that the fluorescence intensity reached the maximum at the K+ concentration of 20%, after which the intensity weakened when the K+ content continued to increase. According to the dependence between the luminescence intensity of the sample and the laser power density and fluorescence lifetime, the intrinsic mechanism was carefully investigated. Temperature-dependent spectra of the samples were recorded in the temperature range of 315–495 K, and the maximum values of absolute sensitivity (Sa) and relative sensitivity (Sr) were measured at 0.0041 K−1 (455 K) and 0.9220%K−1 (315 K). The experimental results show that K+/Er3+/Yb3+ triple-doped NaYF4 green fluorescent nanoparticles (GFNs) have good prospects for applications in display devices, temperature sensing, and other fields.