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Eingeladener Vortrag
- nein (145) (entfernen)
Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorspar has been named among the 30 critical raw materials in the EU. 1 However, the sustainable transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. Herein, we present the heterogeneous catalyst zirconium chloro fluoride (ZCF) that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
The use of a dedicated approach: DoE for synthesis + characterization + Chemometric Analysis, is a valuable method for the safe-by-design synthesis of several types of materials for large-scale application in catalysis, energy harvesting, biomedical and environmental applications, etc. This approach is not only related to the material synthesis, but can be expanded to any type of molecules/material, with relevant saving of solvents, energy and times.
The principles of (Hard) X-ray photoelectron spectroscopy and some application in the field of (core-shell) nanoparticles will be presented. The presentation should answer hoe to get reliable results. Furthermore, examples of the correlation between physical-chemical measurments and toxicological results are given which are crucial for the risk assessment of nanoparticles.
Climate change and increasing demand for electricity require the use of power electronics based on new wide bandgap (WBG) compound semiconductors. Power electronics devices are used in numerous application areas to control and convert electric energy. These may include generation and distribution of renewable energy for green hydrogen, electrification of transport or 5G communication. WBG electronics have much higher efficiency than the silicon-based ones and can operate at higher power densities, voltages, temperatures and switching frequencies with low energy losses. However, defects in the semiconductors can considerably affect the performance of power electronic devices or make their operation even impossible. The presentation will show the application of spectroscopic and imaging ellipsometry as well as white light interference microscopy for defect characterisation in SiC, GaN and Ga2O3 over a wide wavelength range.
We used parameterized modelling of ellipsometric transfer parameters to determine the dielectric properties of bulk materials and thin layers. Imaging ellipsometry offers more information and is an advanced variant of optical microscopy, combining the lateral resolution of optical microscopy with the extreme sensitivity to surface and interface effects of ellipsometry. Surface topography and morphology of different types of defects were additionally investigated with imaging white light interference microscopy. Modern electronic thin film components require complex surface analysis methodologies and hybrid metrology. Hybrid measurement techniques enable fast and non-destructive traceable characterisation of thin film compound semiconductors as well as accurate detection and identification of defects. This methodical approach leads to a better understanding of the materials themselves and of the defect formation mechanisms during manufacturing.
This work aims to enable highly reproducible manufacturing of compound semiconductor power electronics as well as operation monitoring to ensure failure-safety of electronic systems in power electronic devices.
Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein.
Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein.
Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein.
The efficient exploration of novel alloy compositions is crucial for advancing the development of new materials. One widely utilized approach for creating phase diagrams is the use of diffusion-controlled synthesis for gradient alloys. This method is also an effective means for rapidly identifying potential material combinations.
The present study focusses on the exploration of quaternary multi-principle-element alloys (MPEAs) using diffusion multiples. We established a diffusion system by combining an equimolar ternary alloy (FeNiCr) with single diffusing elements Mn and Mo. Using ThermoCalc simulations, we determined suitable temperature ranges where we can expect the formation of single-phase alloys. Depending on the diffusion constants of the selected metals, diffusion times were adjusted to obtain diffusion zones with a depth of greater than 50 μm. Microstructural and compositional information was gathered via scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) and correlated to local mechanical properties evaluated by means of nanoindentation. Local corrosion properties were examined using Atomic Force Microscopy (AFM) and Scanning Electrochemical Microscopy (SECM).
Our results indicate that the ThermoCalc simulations have a good predictive power for crystallographic phases. However, especially with the Mn-FeNiCr system, formation of Cr-rich secondary phases were observed, which led to Cr-depletion and thus to localized corrosion processes in the matrix at the vicinity of the secondary phases. Based on the results of the local electrochemical tests, we have selected single-phase compositions along the diffusion zone and synthesized these alloys in bulk for corrosion studies by means of potentiodynamic polarization and SECM.
The presentation will summarize our methodology using diffusion couples as an
efficient tool for exploring compositional spaces of MPEAs in the search for novel single-phase alloys and the results of our correlative study on the mechanical and corrosion properties of these materials.
The efficient exploration of novel alloy chemistries is crucial for advancing the development of new materials. Diffusion-controlled synthesis of gradient alloys is an intelligent approach for creating phase diagrams and to effectively identify potential material combinations with tailored properties.
This project focusses on the design of quaternary multi-principle-element alloys (MPEAs) using diffusion couples. Our diffusion system contains an equimolar ternary alloy (FeNiCr) and additional single diffusing elements e.g. Mn and Mo. We determined the optimal temperature ranges for the diffusion thermal treatment by means of ThermoCalc simulations with the aim to form single-phase MPEAs. Microstructure and chemical characterization of the diffusion couples were performed by means of scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). For most alloy couples, the diffusion zone contained a single-phase alloy matrix with diffusion-induced compositional gradient as well as precipitation phases. This heterogeneity makes the diffusion couples interesting materials to investigate local mechanical and corrosion properties. Thus, local corrosion properties were examined using Atomic Force Microscopy (AFM) and Scanning Electrochemical Microscopy (SECM). Nanoindentation was used for the analysis of local mechanical properties.
Based on the results of the local corrosion analysis, we have selected single-phase alloy chemistries along the diffusion zone and reproducibly synthesized these alloys in bulk for detailed corrosion studies by means of potentiodynamic polarization and SECM.
The presentation will briefly summarize our methodology and motivation for using diffusion couples as an efficient tool for exploring phase diagrams of MPEAs in the search for new alloy chemistries and the results of our correlative study on the mechanical and corrosion properties of these materials.
Old materials, new life: Using diffusion-controlled synthesis for discovery of novel alloy systems
(2023)
Multi principal element alloy (MPEAs) concept allows us to rethink how we develop application-tailored, sustainable materials. The vast composition space leads to nearly indefinite material combinations and will facilitate finding Pareto optimal materials with lower CO2 footprint and avoidance of critical minerals as design criteria. To probe this large compositional space efficiently, the use high-throughput screening methods is inevitable. Diffusion-controlled synthesis of gradient materials is the optimal technique for screening complex compositional materials that would otherwise require comprehensive modelling or experimental efforts.
In this study, we have used a series of diffusion couples of pure metals and alloys with the aim to create a materials library with correlated data on composition and microstructure. With future recycling prospects in mind, and possible applications of Cu containing alloys in electrocatalytic carbon dioxide reduction and antimicrobial alloys we have generated diffusion couples of brass (Cu63Zn37) and bronze (Cu89Sn11) with either pure metals (Fe, Ni, etc.) or with binary or ternary alloys (FeNi, FeNiCr etc.). For different diffusion times and temperatures, we calculated diffusion constants for the material combinations. Following a detailed characterisation of the gradient materials, we have investigated general and local corrosion properties, electrocatalytic activity for oxygen evolution reaction (OER) and carbon dioxide reduction reaction (CRR) as well as mechanical properties (hardness, elastic modulus) on single-phase alloys synthesized in bulk by means of vacuum arc-melting based on the selected local compositions.
In most cases, due to the short diffusion times, the contact between the diffusion couples lead to two separate diffusion zones and thus, different alloy families on both sides. Especially with ternary alloys, interesting selective diffusion processes and unexpected repulsion effects were observed. The presentation will provide an overview of the gradient materials with a focus on the functional properties of single-phase alloy families derived from them.
Due to their favorable mechanical and anti-corrosion properties, medium entropy alloys (MEA) are of high academic and industrial interest as novel materials for engineering and catalytic applications. Previous studies on general corrosion behavior indicate high current densities at high anodic potentials for MEAs. Further investigations of the underlying transpassive dissolution and local corrosion behavior remain scarce.
To understand the passivation behavior of MEAs CrCoNi and FeCrNi at high anodic potentials, the mechanisms of transpassive dissolution and the oxygen evolution reaction were investigated in this project. Scanning electrochemical microscopy (SECM) was applied in the interrogative mode for the detection of evolving metal species and oxygen. By means of ICP-MS analysis, dissolved metal species were quantified to provide a fundamental understanding on the transpassive dissolution. As the oxygen evolution reaction (OER) may contribute a large percentile to the observed current at high anodic potentials, SECM measurements were employed to analyze the onset of the OER. Potentiodynamic, potentiostatic and chronoamperometric techniques as well as different electrolytes were used to induce precisely controlled corrosion loads during the SECM experiments and for the ICP-MS analysis. Macroscopic corrosion properties of the alloys, electrical and chemical properties of the passive films were studied by means of potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and X-Ray Photoelectron Spectroscopy (XPS), respectively.
Finally, the analysis of the corrosion morphology and the potential of the surface before, during and after passivity breakdown was carried out by means of in-situ atomic force microscopy (AFM) and scanning Kelvin probe force microscopy (SKPFM). The presentation will summarize our results on the interplay of anodic passivation and oxygen evolution of MEAs in aqueous NaCl electrolytes.
The high-throughput synthesis and characterization of potential material combinations plays an important role in accelerating the development of new materials. Diffusion controlled synthesis of gradient alloys is widely used to create phase diagrams, and it is also one of the most effective combinatorial approaches for rapid realization of potential material combinations.
This study focuses on the synthesis and investigation of the quaternary multi-principle-element alloy (MPEA) FeNiCrMn by means of diffusion multiples, the correlation of their microstructural and chemical characterization data with their application relevant properties like local mechanical and corrosion properties. A diffusion system was set up by combining an equimolar ternary alloy (FeNiCr) with a single diffusing metallic component (Mn) with the highest interdiffusion coefficient. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to collect microstructural and compositional information which were correlated to local mechanical properties studied with nanoindentation. Local corrosion properties were investigated by means of Atomic Force Microscopy (AFM) and Scanning Electrochemical Microscopy (SECM). We have observed that a >50 μm deep homogeneous diffusion zone was formed the thickness of which scales with the duration of the thermal treatment. Beyond the Mn-concentration gradient in the FeNiCr matrix, a distinct Cr-rich secondary phase, characterized by high hardness and elastic modulus values appeared. We synthesized MPEAs with selected compositions from the diffusion zone as well as the Cr-rich phase as bulk alloys for electrochemical corrosion studies under different environmental conditions. The presentation will summarize the results of our correlative study on the mechanical properties and corrosion resistance of the quaternary multi-principle-element alloy (MPEA) FeNiCrMn family.
Multiphoton lithography (MPL) has recently attracted significant research interest as a versatile tool capable of fabricating 2D and 3D micro- and nanoscopic features with high spatial resolution. The integrity of MPL microstructures, or their ability to respond to external stimuli, is of critical importance. Often, the mechanically flexible micro-objects are expected to be capable of shape morphing, bending, or other motion to ensure their functionality. However, achieving the desired properties of MPL-manufactured micro components for a specific application still remains challenging.
In this work, we present new MPL materials based on epoxy-acrylate interpenetrating networks (IPNs). We aim at fabrication 3D microstructures, whose properties can be easily tuned by varying the ratio of the IPN components and fabrication parameters. The studied mixtures consist of polyethylene glycol diacrylate (PEGDA) and cycloaliphatic epoxide functional groups. Consequently, tryarylsylfonium salt and cyclopentanone photoinitiator tailored for MPL were used to ensure cationic and radical polymerization, respectively. The resulting library of 3D microstructures was investigated for their thermal and mechanical properties using highly sensitive space-resolved methods. For the first time, we were able to evaluate the glass transition behavior of 3D MPL microstructures using fast scanning calorimetry. The influence of both IPN composition and fabrication parameters on glass transition temperature and material fragility was demonstrated. AFM force-distance curve and intermodulation methods were used to characterize the micromechanical properties with lateral resolution of the techniques in the range of 1 micron and 4 nm, respectively. The elastic-plastic behavior of the microarchitectures was evaluated and explained in terms of IPN morphology and thermal properties. The fabricated 3D IPN microstructures exhibit higher structural strength and integrity compared to PEGDA. In addition, IPNs exhibit high to full elastic recovery (up to 100%) with bulk modulus in the range of 4 to 6 MPa. This makes IPNs a good base material for modeling microstructures with intricate 3D designs for biomimetics and scaffold engineering.
The effects of composition and MPL microfabrication parameters on the resulting IPN properties give us a better understanding of the underlying mechanisms and microfabrication-structure-property relationships. Moreover, our funding supports the further development of IPN systems as versatile and easily tunable MPL materials.
Ellipsometry is a very powerful tool used for accurate material investigation in a wide wavelength range. It is a non-destructive and fast method. Imaging ellipsometry as a combination of optical microscopy and ellipsometry enables spatially resolved measurements when determining the layer thickness and dielectric properties of thin layers. It is known for its high polarisation sensitivity and high contrast for the surface structures. In this contribution we show the application of the imaging ellipsometry for detection of defects in energy materials and quality validation of possible reference materials for nano-electronics.
Defects in wide bandgap semiconductors, in homoepitaxial SiC and heteroepitaxial GaN layers on transparent SiC substrates, can be successfully detected and classified by means of imaging ellipsometry. Correlation of imaging ellipsometry results with results from complementary techniques such as white light interference microscopy as well as atomic force microscopy contribute to understanding of surface topography and defect formation mechanisms. We discuss the potential of different methods for analysing ellipsometric map data for monitoring the defect densities.
Electric properties of materials at the nanoscale can be investigated by means of scanning probe microscopy methods such as scanning microwave microscopy and conductive atomic force microscopy. However, development of new robust and easy-to-use calibration methods and calibration standards is essential to increase the traceability of these methods and allow their broad application in industry. We show how imaging spectroscopic ellipsometry can be used for development and monitoring of processing quality of patterned reference samples based on indium tin oxide (ITO) layer with different thickness and conductivity.
There is an urgent demand for reliable data on microplastic analysis, particularly on its physico-chemical properties as well as validated methodology to obtain such data. Through interlaboratory comparisons (ILCs) it becomes possible to assess accuracy and precision of methods by involving many laboratories around the world. At BAM, my tasks focused around organisation of an ILC on physico-chemical characterisation of microplastic detection methods under the international pre-standardisation platform VAMAS (www.vamas.org/twa45/) as Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods” under the Technical Working Area TWA 45 “Micro and Nano Plastics in the Environment”.
With a proud number of 84 participants this ILC is able to provide superior statistical results. Thermoanalytical (Py-GC/MS and TED-GC/MS) and vibrational (µ-IR and µ-Raman) methods were asked for identification and quantification of microplastic test samples according to mass or particle number. Preliminary results indicate which methods show a higher accuracy and precision and reveal some sample preparation ideas which work best for microplastics characterisation. At the end of the ILC an overall plausibility of the results will be assessed.
Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. These polymers are characterized by a high permeability and reasonable permselectivity. The latter point is somehow surprising because for microporous systems a more Knudson-like diffusion is expected then a size dependent temperature activated sieving process. It was argued in the framework of a random gate model that molecular fluctuations on a time scale from ps to ns are responsible for the permselectivity.
Here series of polymers of intrinsic microporosity (PIMs) as well as microporous polynorbornenes with bulky Si side groups and a rigid backbone are considered. The polymers have different microporosity characterized by high BET surface area values.
First inelastic time-of-flight neutron scattering measurements were carried out to investigate the low frequency density of state (VDOS). The measured data show the characteristic low frequency excess contribution to the VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. It was found that the frequency of the maximum position of the Boson peak correlates with the BET surface area value.
Secondly elastic scans as well as quasielastic neutron scattering measurements by a combination of neutron time-of-flight and backscattering have been out. A low temperature relaxation process was found for both polymers. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized.
The neutron scattering experiments were accompanied by fast scanning calorimetry and broadband dielectric investigations as well as atomistic molecular dynamic simulations.
This talk explores the intricate connections between scientists, focusing on the networking dynamics within the realm of metal-organic frameworks (MOFs). The study delves into the collaborative networks formed among scientists, shedding light on the synergistic relationships that contribute to advancements in MOF research.