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Paper des Monats
- ja (68)
A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
The development of hydrogen technologies entails high safety requirements in distribution and dispensing infrastructure. Therefore, it is necessary to pursue research on material compatibility in hydrogen, especially for critical parts with tribological issues.
The focus of this study is to evaluate the influence of hydrogen on a wider range of commercially available polymer materials. Thereby, the friction and wear behavior of different grades of TPE, POM, PA66, PA12, PPA, PEEK, PPS, PTFE, PAI, PI and PBI were investigated against a rotating steel disk (AISI 304). Filled and unfilled polymers from different suppliers were evaluated at room temperature in air, vacuum and hydrogen gas (H2) as well as in liquid hydrogen at - 253°C (LH2).
The sliding behavior of the polymer materials is discussed by means of surface analyses, whereby special attention is paid to the formation of a transfer film.
According to the results at ambient temperature, the effect of hydrogen environment on the tribological behavior of neat polymers may be related to lack of moisture, but also to saturated hydrocarbons in gaseous hydrogen. In liquid hydrogen, the best tribological performances were achieved with neat PA polymers as well as PPS and PI composites.
Effect of high-pressure hydrogen environment on the physical and mechanical properties of elastomers
(2024)
Theiler, Géraldine ; Cano Murillo, Natalia ; Halder, Karabi ; Balasooriya, Winoj ; Hausberger, Andreas ; Kaiser, Andreas
This study presents the influence of high-pressure hydrogen environment on the physical and mechanical properties of two types of cross-linked hydrogenated acrylonitrile butadiene rubbers. Based on the CSA/ANSI standard, static exposures in hydrogen experiments were performed up to 100 MPa at 120 °C. Characterization before and after exposure was conducted by means of density and hardness measurements, dynamic mechanical analysis (DMA), tensile tests, compression set, FT-IR and AFM analyses to assess effects after decompression. While the effect of high-pressure exposure is significant immediately after exposure, most of the physical and mechanical properties recover after 48 hours. FT-IR, AFM, SEM and compression set results indicate, however, permanent effects.
Wetzel, Annica ; Morell, Daniel ; von der Au, Marcus ; Wittstock, Gunther ; Ozcan, Ozlem ; Witt, Julia
Multi-principal element alloys (MPEAs) are gaining interest in corrosion and electrocatalysis research due to their electrochemical stability across a broad pH range and the design flexibility they offer. Using the equimolar CrCoNi alloy, we observe significant metal dissolution in a corrosive electrolyte (0.1 M NaCl, pH 2) concurrently with the oxygen evolution reaction (OER) in the transpassive region despite the absence of hysteresis in polarization curves or other obvious corrosion indicators. We present a characterization scheme to delineate the contribution of OER and alloy dissolution, using scanning electrochemical microscopy (SECM) for OER-onset detection, and quantitative chemical analysis with inductively coupled-mass spectrometry (ICP-MS) and ultraviolet visible light (UV-Vis) spectroscopy to elucidate metal dissolution processes. In-situ electrochemical atomic force microscopy (EC-AFM) revealed that the transpassive metal dissolution on CrCoNi is dominated by intergranular corrosion. These results have significant implications for the stability of MPEAs in corrosion systems, emphasizing the necessity of analytically determining metal ions released from MPEA electrodes into the electrolyte when evaluating Faradaic efficiencies of OER catalysts. The release of transition metal ions not only reduces the Faradaic efficiency of electrolyzers but may also cause poisoning and degradation of membranes in electrochemical reactors.
The Na salt of chloroacetic acid is condensed in suspension. Furthermore,glycolic acid is condensed in bulk or in concentrated solution by means of SnCl2 or 4-toluene sulfonic acid (TSA) as catalysts. The temperatures are varied from 160 to 200°C and the time from 1 to 5 days. Low molar mass cyclic poly(glycolic acid) (PGA) is detected by means of matrix-assisted laser desorption ionization time-of-flight (MALDI TOF) mass spectrometry in most PGAs. A predominance of certain cycles having an even number of repeat units is observed suggesting a thermodynamically favored formation of extended-ring crystals. Extremely high melting temperatures (up to 237.5°C)and high melting enthalpies are found for polycondensations with TSA in 1,2-dichlorobenzene.
Kapoor, M. ; Overgaard Christensen, Ch. ; Wittrup Schmidt, J. ; Dalsgaard Sørensen, J. ; Thöns, Sebastian
Reclassification of bridges, i.e., a change in load rating, using reliability-based methods and a direct update with proof load information has been presented by many authors. However, bridge reclassification has hardly been studied from a decision analytic perspective, i.e., with quantification of the risks and benefits of different classification choices, and the expected benefit gain from proof loading. We derive, explain and exemplify a decision analytic approach for bridge reclassification along with models for (1) elastic and ultimate capacity and their adaptation with proof load information, (2) proof load information with classification outcomes accounting for target reliabilities and, (3) utilities including socio-economic benefits from reclassification. The approach and models are exemplified with a case study based on reclassification of bridges with a low existing classification. Decision rules, for practical use by a highway authority to find the optimal classification, are identified and documented based on: (1) the measurement of the capacity at elastic limit by proof loading, (2) the bridge reclassification benefits, and, (3) the required annual reliability level. From a Value of Information analysis, it is concluded that the proof load information is highly valuable for reclassification in cases of high socio-economic benefits and high reliability requirements.
Emamverdi, Farnaz ; Huang, J. ; Szymoniak, Paulina ; Bojdys, M. J. ; Böhning, Martin ; Schönhals, Andreas
Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy.
Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials.
Glienke, R. ; Kalkowsky, F. ; Hobbacher, A. F. ; Holch, A. ; Thiele, Marc ; Marten, F. ; Kersten, R. ; Henkel, K.-M.
Wind turbines are exposed to a high number of load cycles during their service lifetime. Therefore, the fatigue strength verification plays an important role in their design. In general, the nominal stress method is used for the fatigue verification of the most common used butt-welded joints. The Eurocode 3 part 1–9 is the current design standard for this field of application. This paper presents recent results of fatigue tests on small-scaled specimens and large components with transverse butt welds to discuss the validity of the FAT-class. Furthermore, results from numerical simulations for the verification with the effective notch stress and the crack propagation approach are used for comparison. Based on the consistency between the numerical results and the fatigue tests, the influence of the seam geometry on the fatigue resistance was investigated. Finally, a prediction of the fatigue strength of butt-welded joints with plate thicknesses up to 80 mm was carried out.
Trogadas, P. ; Cho, J. I. S. ; Rasha, L. ; Lu, X. ; Kardjilov, N. ; Markötter, Henning ; Manke, I. ; Shearing, P. R. ; Brett, D. J. L. ; Coppens, M. O.
A systematic, nature-inspired chemical engineering approach is employed to solve the issue of flooding in electrochemical devices. The mechanism of passive water transport utilized by lizards living in arid environments is leveraged to design flow-fields with a microchannel structure on their surface, through which capillary pressure rapidly removes the water generated in the electrochemical device. This water management strategy is implemented in proton exchange membrane fuel cells (PEMFCs) with a lunginspired flow-field, which ensures uniform distribution of reactants across the catalyst layer. Jointly, this nature-inspired approach results in flood-free, stable operation at 100% RH and a B60% increase in current (B1.9 A cm-2) and peak power density (B650 mW cm−2) compared to current PEMFCs with a flood-prone, serpentine flow-field (B0.8 A cm-2 and 280 mW cm-2, respectively). This significant advance allows for PEMFC operation at fully humidified conditions.
Strobl, Dominic ; Unger, Jörg F. ; Ghnatios, C. ; Klawoon, Alexander ; Pittner, Andreas ; Rethmeier, Michael ; Robens-Radermacher, Annika
Despite the advances in hardware and software techniques, standard numerical methods fail in providing real-time simulations, especially for complex processes such as additive manufacturing applications. A real-time simulation enables process control through the combination of process monitoring and automated feedback, which increases the flexibility and quality of a process. Typically, before producing a whole additive manufacturing structure, a simplified experiment in the form of a beadon-plate experiment is performed to get a first insight into the process and to set parameters suitably. In this work, a reduced order model for the transient thermal problem of the bead-on-plate weld simulation is developed, allowing an efficient model calibration and control of the process. The proposed approach applies the proper generalized decomposition (PGD) method, a popular model order reduction technique, to decrease the computational effort of each model evaluation required multiple times in parameter estimation, control, and optimization. The welding torch is modeled by a moving heat source, which leads to difficulties separating space and time, a key ingredient in PGD simulations. A novel approach for separating space and time is applied and extended to 3D problems allowing the derivation of an efficient separated representation of the temperature.
The results are verified against a standard finite element model showing excellent agreement. The reduced order model is also leveraged in a Bayesian model parameter estimation setup, speeding up calibrations and ultimately leading to an optimized real-time simulation approach for welding experiment using synthetic as well as real measurement data.
Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design.
Distributed fiber optic sensors for structural health monitoring of composite pressure vessels
(2024)
In diesem Beitrag geben wir einen umfassenden Überblick über unsere Forschung auf dem Gebiet der verteilten faseroptischen Sensorik für die strukturelle Zustandsüberwachung von Wasserstoffdruckbehältern aus Verbundwerkstoffen. Insbesondere zeigen wir, wie die Integration von faseroptischen Sensoren in Druckbehälter aus Verbundwerkstoffen die Sicherheit erhöht und gleichzeitig die Wartungskosten senkt. Die geringe Größe von Lichtwellenleitern ermöglicht ihre Integration in Verbundwerkstoffstrukturen während des Herstellungsprozesses, wodurch eine kontinuierliche Überwachung sowie eine präzise Erkennung und Lokalisierung von Strukturschäden während des Betriebs der Druckbehälter ermöglicht wird. Wir erörtern auch das Potenzial modernster Signalverarbeitungsmethoden und des maschinellen Lernens für die Weiterentwicklung der vorausschauenden Instandhaltung. Die von uns vorgestellten Anwendungen von faseroptischen Sensoren zeigen, dass sie einen wichtigen Beitrag zur Energiewende hin zu erneuerbaren Energien leisten können.
A novel distributed acoustic sensing technique is proposed that exploits both phase and amplitude of the Rayleigh backscattered light to quantify the environmental variation. The system employs a wavelength-scanning laser and an imbalanced Mach-Zehnder interferometer to acquire the reflection spectra and the phase of the detected light, respectively. Fading-free and low-frequency measurements are realized via the crosscorrelation of the reflection spectra. The discrete crosscorrelation is used to circumvent the nonlinear frequency sweeping of the laser. Based on the phase of the backscattered light, it is possible to quantify fast environmental variations. The whole system requires no hardware modification of the existing system and its functionality is experimentally validated. The proposed system has the potential to monitor ground motion/movement at very low frequency band like subsidence around mining areas and at high frequency band like earthquakes and vibrations induced by avalanches.
The BAM Data Store
(2023)
As a partner in several NFDI consortia, the Bundesanstalt für Materialforschung und -prüfung (BAM, German federal institute for materials science and testing) contributes to research data standardization efforts in various domains of materials science and engineering (MSE). To implement a central research data management (RDM) infrastructure that meets the requirements of MSE groups at BAM, we initiated the Data Store pilot project in 2021. The resulting infrastructure should enable researchers to digitally document research processes and store related data in a standardized and interoperable manner. As a software solution, we chose openBIS, an open-source framework that is increasingly being used for RDM in MSE communities.
The pilot project was conducted for one year with five research groups across different organizational units and MSE disciplines. The main results are presented for the use case “nanoPlattform”. The group registered experimental steps and linked associated instruments and chemicals in the Data Store to ensure full traceability of data related to the synthesis of ~400 nanomaterials. The system also supported researchers in implementing RDM practices in their workflows, e.g., by automating data import and documentation and by integrating infrastructure for data analysis.
Based on the promising results of the pilot phase, we will roll out the Data Store as the central RDM infrastructure of BAM starting in 2023. We further aim to develop openBIS plugins, metadata standards, and RDM workflows to contribute to the openBIS community and to foster RDM in MSE.
The plant secondary metabolite families of coumarin and 4-hydroxy coumarin have a broad pharmacological spectrum ranging from antibacterial to anticancer properties. One prominent member of this substance class is the synthetic but naturally inspired anticoagulant drug and rodenticide warfarin (coumadin). A vast number of publications focus on the identification of warfarin and its major cytochrome P450-mediated phase I metabolites by liquid chromatography (LC) with mass spectrometry (MS) and tandem mass spectrometric (MS/MS) detection techniques. For the first time, electron ionization (EI) induced high-resolution quadrupole time-of-flight mass spectrometric (HR-qToF-MS) data of in-liner derivatized warfarin and selected hydroxylated species is provided in this study as an alternative to LC-MS/MS approaches. Furthermore, the characteristic fragments and fragmentation pathways of the analyzed methyl ethers are concluded. The obtained data of analytical standards, specific deuterated and 13C-labeled compounds prove inductive cleavage of the acyl or acetonyl side chain, methyl migration, and H-migration, along with consequential inductive cleavage as predominant fragmentation routes. Based on the HR-spectral data, commonalities and differences between the analyzed compounds and fragment groups were evaluated with future applicability in structure elucidation and spectra prediction of related compounds.
The emission of ultrafine particles from small desktop Fused Filament Fabrication (FFF) 3D printers has been frequently investigated in the past years. However, the vast majority of FFF emission and exposure studies have not considered the possible occurrence of particles below the typical detection limit of Condensation Particle Counters and could have systematically underestimated the total particle emission as well as the related exposure risks. Therefore, we comparatively measured particle number concentrations and size distributions of sub-4 nm particles with two commercially available diethylene glycol-based instruments – the TSI 3757 Nano Enhancer and the Airmodus A10 Particle Size Magnifier. Both instruments were evaluated for their suitability of measuring FFF-3D printing emissions in the sub-4 nm size range while operated as a particle counter or as a particle size spectrometer. For particle counting, both instruments match best when the Airmodus system was adjusted to a cut-off of 1.5 nm. For size spectroscopy, both instruments show limitations due to either the fast dynamics or rather low levels of particle emissions from FFF-3D printing in this range. The effects are discussed in detail in this article. The findings could be used to implement sub-4 nm particle measurement in future emission or exposure studies, but also for the development of standard test protocols for FFF-3D printing emissions.
Konert, Florian ; Campari, Alessandro ; Nietzke, Jonathan ; Sobol, Oded ; Paltrinieri, Nicola ; Alvaro, Antonio
Hydrogen has great potential on the path towards decarbonization of the energy and transport sectors and can mitigate the urgent issue of global warming. It can be sustainably produced through water electrolysis with potentially zero emissions, and efficiently used (e.g., in fuel cell systems). Despite its environmental advantages, hydrogen-metal interactions could result in the degradation of the mechanical properties of several structural materials. In order to determine the magnitude of the material degradation in relation to hydrogen exposure, extensive material testing is required. The standardized procedure for in-situ testing for the quantification of the impact of compressed gaseous hydrogen (CGH2) relies on the utilization of an autoclave around the tested specimen. Such test set-up is complex, expensive, time-consuming and requires special equipment, trained personnel, and strict safety procedures. A relatively recent method to circumvent these issues and provide affordable results consists of using hollow specimens, thus applying the hydrogen pressure inside rather than outside the specimen. It allows to reduce the volume of hydrogen by several orders of magnitude and to perform the tests more efficiently and in a safer manner. This study focuses on evaluating the tensile properties of X65 vintage pipeline steel tested in a high-pressure hydrogen environment using hollow specimens. Tests are performed in 6 MPa H2 and Ar at the nominal strain rate of 10−6 s−1 to evaluate the reduced area at fracture and the elongation loss. The effect of surface finishing on crack initiation and propagation is investigated by comparing two different manufacturing techniques. In this way, this study provides insights into the applicability of a novel, reliable, and safe testing method which can be used to assess the hydrogen-assisted ductility loss in metallic materials.
Andreoli, A. F. ; Fantin, Andrea ; Kasatikov, S. ; Bacurau, V. P. ; Widom, M. ; Gargarella, P. ; Mazzer, E. M. ; Woodcock, T. G. ; Nielsch, K. ; Coury, F. G.
The unusual behavior observed in the coefficient of thermal expansion and specific heat capacity of CrFeNi, CoCrNi, and CoCrFeNi medium/high-entropy alloys is commonly referred to as the K-state effect. It is shown to be independent of the Curie temperature, as demonstrated by temperature-dependent magnetic moment measurements. CoCrFeNi alloy is chosen for detailed characterization; potential reasons for the K-state effect such as texture, recrystallization, and second-phase precipitation are ruled out. An examination of the electronic structure indicates the formation of a pseudo-gap in the Density of States, which suggests a specific chemical interaction between Ni and Cr atoms upon alloying. Hybrid Monte Carlo/Molecular Dynamic (MC/MD) simulations indicate the presence of non-negligible chemical short-range order (CSRO). Local lattice distortions are shown to be negligible, although deviations around Cr and Ni elements from those expected in a fully disordered structure are experimentally observed by X-ray absorption spectroscopy. The determined bonding distances are in good agreement with MC/MD calculations. A mechanism is proposed to explain the anomalies and calorimetric experiments and their results are used to validate the mechanism.
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.
Rhode, Michael ; Erxleben, Kjell ; Richter, Tim ; Schroepfer, Dirk ; Mente, Tobias ; Michael, Thomas
Multiple principal element alloys encompass the well-known high entropy alloys (HEA). The alloy system represents a new class of materials consisting of at least three alloying elements, each containing 5 to 35 at.%. Thus, this alloying concept differs fundamentally from conventional materials such as steel or nickel alloys. For this purpose, the alloying elements are specifically selected, the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. In particular, conflicting goals, such as the trade-off between strength and ductility in conventional steels, are overcome. However, in the last 20 years, the focus has been on material synthesis. With the increase in available material quantities, the focus is now on processing issues such as joining and welding processes. The weldability of HEAs has received very little attention so far. The experience with dissimilar metal welds is completely lacking but is essential for the application of these materials in combination with conventional materials. The present study presents comprehensive experimental results on the weldability of an equimolar CoCrFeMnNi-HEA in cold-rolled and heat-treated condition, which was joined by tungsten inert gas welding to an austenitic steel AISI 304. The mechanical properties of the dissimilar metal welds were characterized by cross-weld tensile samples, whereas the local deformation in the weld of the different welding zones was measured by digital image correlation. In accordance with the respective initial HEA condition (cold-rolled vs. heat-treated), the local strain behavior was divergent and influenced the global mechanical properties of both DMW types. Nonetheless, the experiments provided proof in principle of the weldability for dissimilar joints of the CoCrFeMnNi-HEA welded to conventional materials like austenitic stainless steels ensuring a corresponding capability for mechanical loading. This allows further considerations on the application of these innovative materials.