BAM-Publica - Publikationsserver der Bundesanstalt für Materialforschung und -prüfung
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H2O-Initiated Polymerization of L-Lactide
Water-initiated ring-opening polymerizations (ROPs) of L-lactide (LA) were performed in bulk at 140 °C, whereupon 11 different salts or complexes of low-toxic metal ions such as tin (II), Zn(II), Zr(IV), and Bi(III) were used as catalysts. Only four catalysts gave satisfactory results despite a long reaction time (24 h). The influence of the temperature was studied with tin (II) 2-ethylhexanoate (SnOct2), dibutyltin oxide (Bu2SnO), and zinc bis-acetylacetonate (Zn(acac)2) and zirconium acetylacetonate (Zr(acac)4). With SnOct2, Bu2SnO and Zr(acac)4 the time was varied at 140 °C to compare their reactivity. Furthermore, two series of ROPs were carried out with variation of the LA/H2O ratio to verify the control of the molecular weight by the monomer-initiator ratio. Bi- or tri-modal molecular weight distributions (MWD) were found for most of the ROPs and bimodal melting endotherms in the differential scanning calorimetry (DSC) heating traces. The thickness and dependence of the 3D packing of the crystallites were monitored by small-angle X-ray scattering (SAXS) measurements
Artistlib - remote control the radiographic simulator aRTist from Python
The software aRTist is a simulation tool for the generation of realistic radiographs of virtual radiographic superstructures. With radiographic simulations, virtual component models can be scanned as in a computed-tomography scanner. In modern radiography, simulation has become an important tool to minimize cost- and time-intensive measurements. It is increasingly used to optimize techniques for complex applications, to support the method developments, and for educational purposes. With Artistlib, we have started the development of a programming interface to support use cases where the interactive use of the graphical user interface is not suitable. The open-source Python library is intended to remote control and automate the radiographic simulator aRTist
Optical and Spectroscopic Properties of Glasses
Optical glasses have given us the eyes to unveil the microscopic and the macroscopic worlds through microscope and telescope lenses, they have revolutionized the way we communicate through fiber optics and portable device screens, as well as given us new perspectives for sustainable energy harvesting conversion and generation. To meet the demands of ever-growing markets, the compositional design of new glasses requires full characterization of thermal, mechanical, electric, and optical properties. Particularly, the characterization of optical properties is not only relevant for optical/luminescent applications but is also essential for the tailored design of some medical and dental materials such as restorative resins, implants and prothesis. In this seminar we will introduce the fundaments on the optical properties of materials, with particular focus on glasses, and the techniques to characterize them
Perspective article: Multisectoral considerations to enable a circular economy for plastics
Plastics are widely used but improper disposal and release lead to increasing global pollution, threatening environmental and human health. To address this issue, we suggest intersectoral collaboration to achieve zero plastic pollution. The outcomes of the project P-LEACH demonstrated the enormous complexity and range of potential toxic effects of plastic-associated chemicals and micro-/nanoplastics released into water from UV-weathered plastics. We initiated an intersectoral dialogue amongst scientists, manufacturers, regulators and representatives of civil society about how to alleviate the negative impacts of plastic pollution. Circular economy offers a framework for selecting non-toxic chemicals, extending product (re)use, and waste reduction, which act to alleviate pollution when applied to plastics. We suggest three measures to advance a circular economy of plastics: 1.) Increase simplicity of chemicals in virgin plastics combined with transparent information on the contents; 2.) Consider recyclability already in plastic material and product design; 3.) Foster communication through intersectoral dialogue. Major cornerstones are the provision of standardized, easy-to-use tools to characterize plastics and plastic leachates chemically and (eco)toxicologically, the enhancement of citizen awareness enabling them to make informed choices, the creation of economic incentives for manufacturers, and sector-specific regulations to provide products that safeguard environmental and human health
Quantifying Damage Evolution in Concrete: Combining Acoustic Emission and Ultrasonic Testing under Uniaxial Loading
Active-source ultrasonic monitoring using ultrasonic pulse velocity measurements and coda wave interferometry (CWI) can provide information about the evolution elastic properties of concrete with increasing damage. The acoustic emission (AE), a passive method based on "listening” to the radiation of elastic waves in solids caused by irreversible changes within the material structure, gives the first indications of microstructural changes and microcracking. The question is: how the registered microcracking activity alters the elastic properties of concrete?
Our study aims to quantify the connection between the evolution of AE events and the overall elastic properties of concrete, assessed via active-source ultrasonic testing. We analyze the spatiotemporal evolution of AE events, changes in wave propagation speed, and nonlinear effects during stepwise quasi-static loading/unloading of concrete specimens. By integrating CWI with AE analysis, we achieve a comprehensive assessment of the evolution of the sample's damage throughout the entire loading process. Our findings underscore the complementary nature of these methods, revealing that a singular approach may not provide a complete picture of the extent of damage
CO2-based matrix-independent carbon quantification approach for single microplastic-ICP-MS analysis
This study presents a new CO2-based, matrix-independent calibration approach for size determination of microplastic (MP) particles using single particle inductively coupled plasma-mass spectrometry (sp-ICP-MS). By incorporating a CO2 gas calibration approach and upon adjusting the flow rates, an accurate size determination of MPs between 2 and 7 μm was enabled. Scanning electron microscopy (SEM) was successfully applied for method validation. The CO2 gas calibration curves exhibited excellent linearity and reproducibility, with minimal matrix effects across different sample types and matrices, including river water and saline solutions. This CO2-based approach eliminates the limitations of matrix- and size-dependent calibrations, enabling robust and accurate size determinations of MPs. This advancement represents a significant step forward in the analytical capabilities for MPs, paving the way for improved environmental monitoring and assessment of plastic pollution
Recycling nickel aluminium bronze grinding chips to feedstock for directed energy deposition via impact whirl milling: Investigation on processability, microstructure and mechanical properties
During the production of ship propellers, considerable quantities of grinding chips from nickel aluminium bronze are produced. This paper examines the mechanical comminution of such chips via impact whirl milling and the utilization of two chip-powder batches as feedstock for a laser-based directed energy deposition process. The materials are characterized via digital image analysis, standardized flowability tests, scanning electron microscopy and energy dispersive X-ray spectroscopy and are compared to conventional, gas atomized powder. The specimens deposited via directed energy deposition are analyzed for density, hardness and microstructure and tensile properties for vertical and horizontal build up directions are compared. At elevated mill rotation speeds, the comminution with impact whirl milling produced rounded particles, favorable flow properties and particle size distribution, making them suitable to deposit additive specimens. The microstructure exhibited characteristic martensitic phases due to the high cooling rates of the additive manufacturing process. The presence of ceramic inclusions was observed in both the powder and on the tensile fracture surfaces, partly impairing the mechanical properties. However, specimens in the vertical build-up direction (Z) showed competitive tensile results, with 775 MPa in tensile strength, 455 MPa in yield strength and 12.6 % elongation at break. The findings of this study indicate that recycling of machining chips to additive manufacturing feedstock can be a viable option for reducing material costs and environmental impact
Batterien und Elektrolyseure der nächsten Generation
Übersichtvortrag zu Batterien und Elektrolyseuren. Ausgehend vom Funktionsprinzip von klassischen Lithium-Ionen-Zellen wurde deren Aufbau und die verwendeten Aktivmaterialien eingeführt. Im Anschluss wurde auf nachhaltigere Alternativtechnologien wie Natrium-Ionen und Natrium-Schwefel eingegangen. Immer mit dem Fokus auf den verwendeten Materialien und den umweltrelevanten Aspekten
Reimagining user-driven science
The materials scientists we work with do not want (or need) to learn the ways of the scatterer; they are primarily interested in obtaining trustworthy, authoritative answers. In particular, they need structural understanding in light of the wider framework of their experiment(s). Our interest, therefore, lies in helping them attain this this interconnected understanding, while using such investigations to further hone our methodology to approximate perfection.
While perfection is by definition an unattainable goal, we have spent the last 15+ years exploring and expanding on many of its constituent aspects (often together with likeminded people) [1]. These aspects include:
developing various visualization and simulation tools,
deconstructing data corrections and uncertainty estimation,
advancing analysis methods,
quantifying questions on traceability, documentation,
reproducible automation of synthesis-, measurement- and data pipelines,
data visualization, exploration and education,
and many more…
As we explored these individual aspects, it has become clear that high quality output demands involving ourselves in the entire experimental workflow, with all associated aspects. This allows you to establish trustworthy links between parameters, structure, and performance. Through multiple cross-checks and validations, we can furthermore assign a degree of confidence to our findings. This is what we call the holistic approach.
This talk will briefly define perfection in scattering experiments, expand on the holistic approach, and show examples to demonstrate its benefits
Homochiral versus racemic 2D covalent organic frameworks
The synthesis of homochiral two-dimensional covalent organic frameworks (2D COFs) from chiral π-conjugated building blocks is challenging, as chiral units often lead to misaligned stacking interactions. In this work, we introduce helical chirality into 2D COFs using configurationally stable enantiopure and racemic [5]helicenes as linkers in the backbone of 2D [5]HeliCOFs as powders and films. Through condensation with 1,3,5-triformylbenzene (TFB) or 1,3,5-triformylphloroglucinol (TFP), our approach enables the efficient formation of a set of homochiral and racemic 2D [5]HeliCOFs. The resulting carbon-based crystalline and porous frameworks exhibit distinct structural features and different properties between homochiral and racemic counterparts. Propagation of helical chirality into the backbone of the crystalline frameworks leads to the observation of advanced chiroptical properties in the far-red visible spectrum, along with a less compact structure compared with the racemic frameworks. Homogeneous thin films of [5]HeliCOFs disclosed photoluminescent properties arising from the controlled growth of highly ordered π-conjugated lattices. The present study offers insight into general chiral framework formation and extends the Liebisch−Wallach rule to 2D COFs