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Applied and Technical Mineralogy:� high-throughput automated platform for in-situ monitoring of CaSO4 formation
No full textIn this project we investigate nucleation pathways by utilizing synchrotron-XRD and running a case-study on calcium sulfate and its polymorphs. To accomplish this, we developed a modular automation setup for reactions in solution to run synthesis and control reaction conditions. So far we successfully characterized the recycling process of gypsum (CaSO4*2H2O) and are now investigating the formation of anhydrite (CaSO4*0H2O) as well as possible applications for the automation setup and analysis
Influence of laser power on the melt pool shape of handheld laser beam welding of 1.5 mm thick micro alloyed steel
No full textManual welding of structures requires highly skilled welders due to the large heat-affected zone of arc-based processes, that can negatively impact microstructure and cause distortion. Handheld laser beam welding is a promising alternative with high welding velocity and a concentrated heat input. However, its current use in industry is limited to parts with aesthetic requirements, often made of high-alloyed steel. To extend the use of handheld laser beam welding to low-cost steels with good mechanical properties, this study investigates the influence of laser power on the melt pool shape for micro-alloyed steel with a thickness of 1.5 mm. Tested joint geometries are T-joints welded with filler wire as well as butt joints and overlap joints without filler wire, which are typically found in assemblies under mechanical load. Weld quality is assessed by weld porosity analysis. The results show that the handheld laser beam welding with filler wire produces T-joints with a very good external appearance, but with porosity between level C and D in the cross sections according to DIN EN ISO 13919-1. By increasing the laser power, a deep penetration of the T-joint zone can be achieved without increasing the actual throat thickness. For handheld laser beam welding of butt joints a full penetration weld of the highest quality class can be reached. Overlap joints can be welded with full or partial penetration depending on the laser power selected, with quality classes between B and C in terms of porosity
Electron Beam Bonding: A novel method for joining additively manufactured carbon fiber thermoplastic composites with aluminum to produce multi-material joints for lightweight applications
No full textIn recent years, new solutions have been explored to reduce the weight of components for the automotive, railway, and aerospace industries. For this reason, Carbon Fiber Composites (CFCs) have increasingly replaced metals in products that need to be lightweight. However, due to their poor thermal conductivity, CFCs have limited use in applications requiring efficient heat dissipation. In such applications, conventionally manufactured metal alloys are typically utilized. To address these limitations, a novel approach using a combination of additively manufactured aluminum and CFCs is proposed to exploit the distinct advantages of both materials. These innovative hybrid structures aim to combine good structural and thermal management properties with reduced weight compared to conventionally produced metal products. In this study, additively manufactured aluminum alloy (AlSi10Mg) and short carbon fiber Polyamide 6 composite (sCF-PA6) are utilized to produce metal–polymer pairs using electron beam energy to bond the two materials. Direct irradiation of short CFCs with electron beam leads to polymer degradation. Thus, a novel method “Electron Beam Bonding” for joining CFCs with aluminum alloy in various joint configurations using electron beam technology is demonstrated. This innovative approach presents a promising solution for creating metal–polymer multi-materials for lightweight applications
Quantifying the total and accessible amount of surface functionalities and ligands on nanomaterials
No full textEngineered nanomaterials (NMs) of various chemical composition and surface functionalization are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NM dispersibility, stability, processability, and function as well as the interaction with biological species and environmental fate are largely determined by NM surface functionalities, i.e., functional groups (FGs) and ligands. Therefore, reliable, reproducible, and eventually standardized surface characterization methods are vital for quality control of NMs, and mandatory to meet increasing concerns regarding their safety.
Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods.[1] The latter less costly and fast methods, which can be automated, are often used by NM producers for process and quality control.[1,2] To validate methods, establish measurement uncertain-ties, test reference materials, and produce reference data, multi-method characterization studies are needed.[3,4] as well as interlaboratory comparisons (ILC) on determining NM surface chemistry and well characterized test and reference NMs providing benchmark values.[5,6] Here, we present examples for quantifying common surface FGs such as amino and carboxyl groups on functional NMs of different chemical composition such as silica, polymer, iron oxide, and lanthanide-based upconversion nanoparticles with optical assays, electrochemical titration methods, qNMR, and chromatographic separation techniques. In addition, ongoing interlaboratory comparisons will be presented
Sustainable Synthesis of Na+ and Bi3+ - doped Cs₂AgInCl₆ Double Perovskites for Efficient White-Light Emission
No full textDouble halide perovskites have emerged as promising, less-toxic alternatives to lead-based perovskites for diverse photochemical applications. Among them, Cs₂AgInCl₆ has attracted significant attention, particularly when doped with various elements, which induce self-trapped exciton (STE) states within the bandgap, resulting in efficient white-light emission and a remarkable enhancement of photoluminescence quantum yield (PL QY). While several solid-state and solution-based methods have been employed for the synthesis of double halide perovskites, many rely on toxic solvents and complex procedures, hindering scalability. In this study, we present two environmentally friendly synthesis approaches for the preparation of Cs₂AgInCl₆ doped with monovalent (Na⁺) and trivalent (Bi³⁺) cations:
1. Green solution-based method: Utilizes mild reagents and entirely replaces harsh chemicals, enabling synthesis at ambient conditions.
2. Mechanochemical approach: Employs high-energy ball milling for 62 minutes at room temperature to obtain the desired crystalline phase.
These green methodologies provide sustainable and scalable alternatives to conventional routes, minimizing the environmental footprint. We systematically compare the structural and optical properties of the doped perovskites synthesized via both approaches. The resulting materials exhibit strong UV absorption, broadband white-light emission, high PL QY (up to 85%, Fig. 1), long PL lifetimes, and good thermal and environmental stability (up to 300 °C in air). These results highlight the potential of doped Cs₂AgInCl₆ double perovskites as an eco-friendly material with possible photonic applications as in white-light devices
Recipe‐Free Synthesis of Optimal Operation Trajectories for Batch Processes Based on Process Models
No full textAbstractBatch processes are usually operated following recipes, which are based on experience and expert knowledge. This ensures feasible and safe operation, because process constraints are indirectly included in the recipe. However, the recipe structure itself constrains the solution space and might exclude other more efficient trajectories. Therefore, the hidden constraints are explicitly formulated, and the arising optimization problem is solved without using prior knowledge in the form of recipes. Case studies are performed on rigorous models of a batch reactor and a batch distillation column. It is demonstrated that the optimization problem formulated as a smoothed dynamic nonlinear programming problem outperforms a mixed‐integer formulation. Finally, a multi‐objective case is investigated that strongly outperforms a recipe‐based benchmark
Automated in situ monitoring and analysis of process signatures and build profiles during wire arc directed energy deposition
No full textWire arc directed energy deposition (DED-Arc) is an emerging metal additive manufacturing process to build near-net shaped metallic parts in a layer-by-layer with minimal material wastage. Automated in situ monitoring and fast-responsive analyses of process signatures and deposit profiles during DED-Arc are in ever demand to print dimensionally consistent parts and reduce post-deposition machining. A comprehensive experimental investigation is presented here involving real-time synchronous measurement of arc current, voltage, and the deposit profile using a novel multi-sensor monitoring framework integrated with the DED-Arc set-up. The recorded current–voltage transients are used to estimate the time-averaged arc power, and energy input in real time for an insight of the influence of wire feed rate and printing travel speed on the deposit characteristics. A unique attempt is made to represent the geometric profiles of the single-track deposits in a generalized mathematical form corresponding to a segmented ellipse, which has exhibited the minimum root-mean-square error of 0.03 mm. The dimensional inconsistency of multi-track deposits is evaluated quantitatively in terms of waviness using build profile monitoring and automated estimation, which is found to increase with an increase in step-over ratio and energy input. For the multi-track mild steel deposits, the suitable range of step-over ratio for the minimum surface waviness is observed to lie between 0.6 and 0.65. Collectively, the proposed framework of synchronized process monitoring and real-time analysis provides a pathway to achieve dimensionally consistent and defect-free parts, and highlights the potential for closed-loop control systems for a wider industrial application of DED-Arc
Acoustic Ion Manipulation: Electric-field-free Approach to Gate, Focus, and Separate Ions at Atmospheric Pressure
No full textApproaches to control the motion and direction of ionized particles and mole-cules are an essential aspect of ion-based spectrometries, such as mass spec-trometry (MS) and ion mobility spectrometry (IMS). A wide variety of ion optics exist to reflect, focus, separate, gate, and filter ions based on physical proper-ties. Notably all rely on electric and magnetic fields to alter the trajectory of ionized atoms and molecules. While these optics are quite efficient at low pressures due to the large mean free path, diffusion and electrostatic repulsion between ions dominate at higher pressures. Conventional ion optics, that use electric or magnetic fields, can guide ions at atmospheric pressure (AP), but require high field strengths to overcome the dominating aerodynamic effects.
Here, we describe a remarkable phenomenon whereby low-power acoustic fields are used to move, shape, gate, and separate beams of gaseous ions at atmospheric pressure. We refer to this approach as Acoustic Ion Manipulation (AIM). Gaseous ions at AP are directed towards and separated by the presence of the acoustic field. To better understand the phenomenon, an ion-detector array provided a measure of bulk ion movement, while mass spectrometry (MS) offered chemical-specific information. As one example of an AIM setup, a standing acoustic wave was formed with two ultrasonic speakers and placed between an ionization source and ion detector. Ion beams preferentially travel through regions of stable pressure gradients (i.e. nodes) and deflect from un-stable regions (i.e. antinodes). Shadowgraphy revealed that the ions are sepa-rated from a neutral gas stream. Specific examples of ion focusing, gating, and separation (based on ion size) will be shown. In addition, experimental findings will be used to postulate a theory to develop a better understand of the behav-ior of gas-phase ions in acoustic fields. This discovery could have profound im-pacts in IMS/MS instrumentation as well as materials processing and charac-terization
Luminescent, Semiconductor Nanoparticle-Loadedpolymer Microbeads–Comparingparticlearchitectures
No full textLuminescent polymer microparticles (PMPs) are applied in various (bio)analytical and diagnostic processes.[1] The staining of these beads is important for the realization of optically distinguishable barcodes that can be read out, e.g., by a flow cytometer or fluorescence microscope. Typically, luminescent semiconductor nanoparticles (NPs) absorb in a broad wavelength range and show narrow emission bands, which enables simultaneous excitation of differently colored luminophores and facilitates a spectral discrimination.[1] This makes them ideal candidates for this purpose and encouraged us to explore and develop a simple, effective approach to luminescent semiconductor NP encoding of polystyrene PMPs and identify suitable synthesis conditions.[2]
Until now, mainly semiconductor quantum dots (QDs) have been used for the synthesis of luminescent PMPs, although NPs with different shapes could introduce beneficial new features. Aiming for the application of our developed procedure to non-spherical NPs, we systematically investigated the luminescence properties of the resulting NP-stained beads using fluorescence and integrating sphere spectroscopy as well as fluorescence and electron microscopy. These studies showed that the suitability of semiconductor NPs for the synthesis of luminescent PMPs depends not only on their shape, but also heavily on their surface chemistry.[3] The successful incorporation of nonspherical NPs opens the path to include even more NPs, and the results can help to deduce future applications for the beads which best suit their specific properties
Reconstruction of the time-averaged keyhole geometry in laser beam welding with electromagnetic support
No full textIn laser beam welding (LBW), the time-averaged keyhole shape provides statistical insights into the process compared to its transient geometry, offering a deeper understanding of the overall keyhole behaviour. However, capturing the time-averaged keyhole shape through experimental methods remains challenging. In this paper, a reconstruction algorithm for the time-averaged keyhole is developed and integrated into a three-dimensional transient multi-physical coupled numerical model. The algorithm can accurately capture the key characteristics of the keyhole, including its diameter and centroid. In addition, it can also successfully reproduce the experimentally observed phenomena of keyhole tailing. The overall shape of the keyhole appears smooth, without exhibiting obvious instability features. Furthermore, the time-averaged keyhole shape is compared under different magnetic flux densities when an external oscillating magnetic field is applied. The results indicate that the application of external magnetic fields does not fundamentally alter the overall keyhole shape. With increasing magnetic flux density, the trailing tail becomes progressively less pronounced and a noticeable increase in the curvature of the rear wall is observed. The standard deviation of the keyhole diameter can serve as an effective index for evaluating the keyhole instability. Keyhole stability in LBW of aluminium alloys is improved under the assistance of electromagnetic fields, and this stabilization is positively correlated with increasing magnetic flux density