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L-Lactide (LA) was polymerized with neat tin(II) 2-ethylhexanoate (SnOct2) in toluene at 115 °C at low concentration with variation of the LA/Cat ratio. Cyclic polylactides (cPLAs) with number average molecular weights (Mn) between 7 000 and 17 000 were obtained. MALDI-TOF mass spectrometry also revealed the formation of a few percent of linear chains. Crystalline cPLAs with Mn around 9 000 and 14 000 were annealed at 140 °C in the presence of ScOct2 or dibutyl-2-stanna-1,3-dithiolane (DSTL). Simultaneously, crystallites of extended linear chains and crystallites of extended cycles were formed regardless of the catalyst, indicating that transesterification reaction proceeded different for linear chains and for cycles, governed by thermodynamic control. The formation of extended chain crystallites with low dispersity indicates the existence of symproportionation of short and long chains. A complementary experiment was carried out with a PLA ethyl ester composed mainly of linear chains with a small fraction of cycles
Ceramic additive manufacturing (AM) requires a complex process chain with various post-processing steps that require expensive machines and special expertise. The key to further market penetration is AM that makes it possible to integrate into an already established ceramic process chain. Most successful AM technologies for ceramics are, however, based on processes that initially have been developed for polymeric materials. For ceramics AM, polymers or precursors are loaded with ceramic particles. This strategy facilitates the entry into AM, however the introduction of organic additives into the ceramic process chain represents a considerable technological challenge to ultimately obtain a ceramic component after additive shaping. In the present communication, two technologies based on ceramic suspensions will be introduced, the “layerwise slurry deposition” (LSD) and “laser induced slip casting” (LIS) technology. Both technologies take advantage of the high packing densities reached by conventional slip casting and moreover enable the processing of fines, even nanoparticles.
A key aspect in the development of multilayer inductors is the magnetic permeability of the ferrite layers. Here, the effects of different processing steps on the permeability of a NiCuZn ferrite is investigated. Dry pressed, tape cast, and co‐fired multilayer samples are analyzed. An automated data pipeline is applied to structure the acquired experimental data according to a domain ontology based on PMDco (Platform MaterialDigital core ontology). Example queries to the ontology show how the determined process‐property correlations are accessible to non‐experts and thus how suitable data for component design can be identified. It is demonstrated how the inductance of co‐fired multilayer inductors is reliably predicted by simulations if the appropriate input data corresponding to the manufacturing process is used.This article is protected by copyright. All rights reserved.
This data article presents a set of primary, analyzed, and digitalized mechanical testing datasets for nine copper alloys. The mechanical testing methods including the Brinell and Vickers hardness, tensile, stress relaxation, and low-cycle fatigue (LCF) testing were performed according to the DIN/ISO standards. The obtained primary testing data (84 files) mainly contain the raw measured data along with the testing metadata of the processes, materials, and testing machines. Five secondary datasets were also provided for each testing method by collecting the main meta- and measurement data from the primary data and the outputs of data analyses. These datasets give materials scientists beneficial data for comparative material selection analyses by clarifying the wide range of mechanical properties of copper alloys, including Brinell and Vickers hardness, yield and tensile strengths, elongation, reduction of area, relaxed and residual stresses, and LCF fatigue life. Furthermore, both the primary and secondary datasets were digitalized by the approach introduced in the research article entitled “Toward a digital materials mechanical testing lab” [1]. The resulting open-linked data are the machine-processable semantic descriptions of data and their generation processes and can be easily queried by semantic searches to enable advanced data-driven materials research.
AbstractTwo‐photon polymerization (2PP) additive manufacturing (AM) utilizes feedstocks of ceramic nanoparticles of a few nanometers in diameter, enabling the fabrication of highly accurate technical ceramic design with structural details as small as 500 nm. The performance of these materials is expected to differ from conventional AM ceramics, as nanoparticles and three‐dimensional printing at high resolution introduce new microstructural aspects. This study applies 2PP‐AM of yttria‐stabilized zirconia to investigate the mechanical response behavior under compressive load, probing the influence of smallest structural units induced by the line packing during the printing process, design of sintered microblocks, and sintering temperature and thereby microstructure. We find a dissipative mechanical response enhanced by sintering at lower temperatures than conventional. The pursued 2PP‐AM approach yields a microstructured material with an increased number of grain boundaries that proposedly play a major role in facilitating energy dissipation within the here printed ceramic material. This microplastic response is further triggered by the filigree structures induced by hollow line packing at the order of the critical defect size of ceramics. Together, these unique aspects made accessible by the 2PP‐AM approach contribute to a heterogeneous nano‐ and microstructure, and hint toward opportunities for tailoring the mechanical response in future ceramic applications.
Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks.
Quantum dots (QDs) are remarkable semiconductor nanoparticles, whose optical properties are strongly size-dependent. Therefore, the real-time monitoring of crystal growth pathway during synthesis gives an excellent opportunity to a smart design of the QDs luminescence. In this work, we present a new approach for monitoring the formation of QDs in aqueous solution up to 90 °C, through in situ luminescence analysis, using CdTe as a model system. This technique allows a detailed examination of the evolution of their light emission. In contrast to in situ absorbance analysis, the in situ luminescence measurements in reflection geometry are particularly advantageous once they are not hindered by the concentration increase of the colloidal suspension. The synthesized particles were additionally characterized using X-ray diffraction analysis, transition electron microscopy, UV-Vis absorption and infrared spectroscopy. The infrared spectra showed that 3-mercaptopropionic acid (MPA)-based thiols are covalently bound on the surface of QDs and microscopy revealed the formation of CdS. Setting a total of 3 h of reaction time, for instance, the QDs synthesized at 70, 80 and 90 °C exhibit emission maxima centered at 550, 600 and 655 nm. The in situ monitoring approach opens doors for a more precise achievement of the desired emission wavelength of QDs.
The glass system (50NaPO3–20BaF2–10CaF2–20GdF3)-xTbCl3 with x = 0.3, 1, 3, 5, and 10 wt % was investigated. We successfully produced transparent glass ceramic (GC) scintillators with x = 1 through a melt-quenching process followed by thermal treatment. The luminescence and crystallization characteristics of these materials were thoroughly examined using various analytical methods. The nanocrystallization of Tb3+-doped Na5Gd9F32 within the doped fluoride-phosphate glasses resulted in enhanced photoluminescence (PL) and radioluminescence (RL) of the Tb3+ ions. The GC exhibited an internal PL quantum yield of 33 % and the integrated RL intensity across the UV-visible range was 36 % of that reported for the commercial BGO powder scintillator. This research showcases that Tb-doped fluoridephosphate GCs containing nanocrystalline Na5Gd9F32 have the potential to serve as efficient scintillators while having lower melting temperature compared to traditional silicate and germanate glasses.
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.
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.
This research deals with the development of the Vickers hardness knowledge graph, mapping the example dataset in them, and exporting the data-mapped knowledge graph as a machine-readable Resource Description Framework (RDF). Modeling the knowledge graph according to the standardized test procedure and using the appropriate upper-level ontologies were taken into consideration to develop the highly standardized, incorporable, and industrial applicable models. Furthermore, the Ontopanel approach was utilized for mapping the real experimental data in the developed knowledge graphs and the resulting RDF files were successfully evaluated through the SPARQL queries.
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.