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Braymer, Joseph J. ; Stehling, Oliver ; Stümpfig, Martin ; Rösser, Ralf ; Spantgar, Farah ; Blinn, Catharina M. ; Mühlenhoff, Ulrich ; Pierik, Antonio J. ; Lill, Roland
The biogenesis of iron–sulfur (Fe/S) proteins entails the synthesis and trafficking of Fe/S clusters, followed by their insertion into target apoproteins. In eukaryotes, the multiple steps of biogenesis are accomplished by complex protein machineries in both mitochondria and cytosol. The underlying biochemical pathways have been elucidated over the past decades, yet the mechanisms of cytosolic [2Fe-2S] protein assembly have remained ill-defined. Similarly, the precise site of glutathione (GSH) requirement in cytosolic and nuclear Fe/S protein biogenesis is unclear, as is the molecular role of the GSH-dependent cytosolic monothiol glutaredoxins (cGrxs). Here, we investigated these questions in human and yeast cells by various in vivo approaches. [2Fe-2S] cluster assembly of cytosolic target apoproteins required the mitochondrial ISC machinery, the mitochondrial transporter Atm1/ABCB7 and GSH, yet occurred independently of both the CIA system and cGrxs. This mechanism was strikingly different from the ISC-, Atm1/ABCB7-, GSH-, and CIA-dependent assembly of cytosolic–nuclear [4Fe-4S] proteins. One notable exception to this cytosolic [2Fe-2S] protein maturation pathway defined here was yeast Apd1 which used the CIA system via binding to the CIA targeting complex through its C-terminal tryptophan. cGrxs, although attributed as [2Fe-2S] cluster chaperones or trafficking proteins, were not essential in vivo for delivering [2Fe-2S] clusters to either CIA components or target apoproteins. Finally, the most critical GSH requirement was assigned to Atm1-dependent export, i.e. a step before GSH-dependent cGrxs function. Our findings extend the general model of eukaryotic Fe/S protein biogenesis by adding the molecular requirements for cytosolic [2Fe-2S] protein maturation.
Gregório, Bruno J.R. ; Ramos, Inês I. ; Marques, Sara S. ; Barreiros, Luísa ; Magalhães, Luís M. ; Schneider, Rudolf ; Segundo, Marcela A.
The presence of endocrine-disrupting compounds (EDCs) in water poses a significant threat to human and animal health, as recognized by regulatory agencies throughout the world. The Yeast Estrogen Screen (YES) assay is an excellent method to evaluate the presence of these compounds in water due to its simplicity and capacity to assess the bioaccessible forms/fractions of these compounds. In the presence of a compound with estrogenic activity, Saccharomyces cerevisiae cells, containing a lacZ reporter gene encoding the enzyme β-galactosidase, are induced, the enzyme is synthesised, and released to the extracellular medium. In this work, a YES-based approach encompassing the use of a lacZ reporter gene modified strain of S. cerevisiae, microcarriers as solid support, and a fluorescent substrate, fluorescein di-β-D-galactopyranoside, is proposed, allowing for the assessment of EDCs’ presence after only 2 h of incubation. The proposed method provided an EC50 of 0.17 ± 0.03 nM and an LLOQ of 0.03 nM, expressed as 17β-estradiol. The assessment of different EDCs provided EC50 values between 0.16 and 1.2 × 103 nM. After application to wastewaters, similar results were obtained for EDCs screening, much faster, compared to the conventional 45 h spectrophotometric procedure using a commercial kit, showing potential for onsite high-throughput screening of environmental contamination.
Guigues, Nathalie ; Uysal, Emrah ; Raveau, Sandrine ; Magar, Jérémie ; Billon, Gabriel ; Kahiluoto, Joonas ; Schneider, Rudolf ; Liv, Lokman ; Gençtürk Tosun, Serap ; Canteau, Gaëlle ; Lalere, Béatrice
Alternative Tools (AT) such as on-site test kits, on-site portable devices and continuous measuring devices, are useful to improve water quality assessment under EU directives, and water treatment processes, thus contributing to improving water management, as well as get insights on the dynamic of pollutants within water bodies. Although these tools have clear advantages (e.g. fast response allowing for real-time monitoring, ease-of-use, lower cost), they are perceived as less reliable than conventional analytical methods. Their alternative nature, innovative status, and non-standard operation mode require specific validation strategies that differ significantly from those of conventional analytical methods. Nevertheless, the validation of ATs, especially on-site test kits, portable devices and continuous measuring devices for water quality monitoring is crucial to support their acceptance, promote their use and make their application sustainable. In this paper, a validation procedure in 4 steps is proposed: (1) Comprehensive description of the AT; (2) Assessment of intrinsic metrological performance and operational factors within a single laboratory; (3) Assessment of inter-laboratory performances through an inter-laboratory comparison and, (4) Demonstration of the equivalence of results between the AT and a reference method. This paper discusses each step of the validation procedure, and examples to illustrate critical issues are provided.
Peptide pools consist of short amino acid sequences and have proven to be versatile tools in various research areas in immunology and clinical applications. They are commercially available in many different compositions and variants. However, unlike other reagents that consist of only one or a few compounds, peptide pools are highly complex products which makes their quality control a major challenge. Quantitative peptide analysis usually requires sophisticated methods, in most cases isotope-labeled standards and reference materials. Usually, this would be prohibitively laborious and expensive. Therefore, an approach is needed to provide a practical and feasible method for quality control of peptide pools. With insufficient quality control, the use of such products could lead to incorrect experimental results, worsening the well-known reproducibility crisis in the biomedical sciences. Here we propose the use of ultra-high performance liquid chromatography (UHPLC) with two detectors, a standard UV detector at 214 nm for quantitative analysis and a high-resolution mass spectrometer (HRMS) for identity confirmation. To be cost-efficient and fast, quantification and identification are performed in one chromatographic run. An optimized protocol is shown, and different peak integration methods are compared and discussed. This work was performed using a peptide pool known as CEF advanced, which consists of 32 peptides derived from cytomegalovirus (CMV), Epstein–Barr virus (EBV) and influenza virus, ranging from 8 to 12 amino acids in length.
Schmidt, Stephan ; Hoffmann, Holger ; Garbe, Leif-Alexander ; Harrer, Andrea ; Steiner, Markus ; Himly, Martin ; Schneider, Rudolf
The non-steroidal anti-inflammatory drug (NSAID) diclofenac (DCF) is an important environmental contaminant occurring in surface waters all over the world, because, after excretion, it is not adequately removed from wastewater in sewage treatment plants. To be able to monitor this pollutant, highly efficient analytical methods are needed, including immunoassays. In a medical research project, monoclonal antibodies against diclofenac and its metabolites had been produced. Based on this monoclonal anti-DCF antibody, a new indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed and applied for environmental samples. The introduction of a spacer between diclofenac and the carrier protein in the coating conjugate led to higher sensitivity. With a test midpoint of 3 mg L−1 and a measurement range of 1–30 mg L−1, the system is not sensitive enough for direct analysis of surface water. However, this assay is quite robust against matrix influences and can be used for wastewater. Without adjustment of the calibration, organic solvents up to 5%, natural organic matter (NOM) up to 10 mg L−1, humic acids up to 2.5 mg L−1, and salt concentrations up to 6 g L−1 NaCl and 75 mg L−1 CaCl2 are tolerated. The antibody is also stable in a pH range from 3 to 12. Cross-reactivity (CR) of 1% or less was determined for the metabolites 40-hydroxydiclofenac (40-OH-DCF), 5-hydroxydiclofenac (5-OH-DCF), DCF lactam, and other NSAIDs. Relevant cross-reactivity occurred only with an amide derivative of DCF, 6-aminohexanoic acid (DCF-Ahx), aceclofenac (ACF) and DCF methyl ester (DCF-Me) with 150%, 61% and 44%, respectively. These substances, however, have not been found in samples. Only DCF-acyl glucuronide with a cross-reactivity of 57% is of some relevance. For the first time, photodegradation products were tested for cross-reactivity. With the ELISA based on this antibody, water samples were analysed. In sewage treatment plant effluents, concentrations in the range of 1.9–5.2 mg L−1 were determined directly, with recoveries compared to HPLC-MS/MS averaging 136%.
Concentrations in lakes ranged from 3 to 4.4 ng L−1 and were, after pre-concentration, determined with an average recovery of 100%
Heavy-weight packages for the safe transport of radioactive material are equippedwith impact limiters often built ofwood-filled steel sheet structures to fulfil the requirements of the International Atomic Energy Agency (IAEA) regulations. The requirements definemechanical tests followed by a thermal test, including criteria ensuring the package design’s ability to withstand severe accidents and provide a high level of technical safety.
Impact limiters are a package component mainly designed for the packages to withstand severe mechanical accident scenarios. In drop tests the impact limiters absorb the kinetic energy during impact of the package. The package must then - with its pre-damaged impact limiters - endure a thermal test defined precisely in the IAEA regulations as a 30-min fully engulfing 800 °C-fire. After the fire, a wood-filled impact limiter may continue to release thermal energy from an ongoing combustion process, defining relevant package temperatures. The energy flow from a possible burning impact limiter to the package is important for the safety evaluation of transport packages. To investigate the combustion behaviour of densely packed layers of spruce wood, encapsulated in pre-damaged cylindrical metal enclosures, a test set-up has been realised. The set-up consists of a combustion chamber to perform these tests under defined boundary conditions. The temperature development of the test specimens will be observed fromoutside with a thermographic imager, with HD-Cameras, and the mass loss will be measured during the entire test. Airflow conditions in the combustion chamber are analysed using Computational Fluid Dynamics (CFD) calculations in OpenFOAM. The planned combustion test setup is described.
Scholtz, Lena ; Eckert, J. G. ; Graf, Rebecca T. ; Kunst, A. ; Wegner, Karl David ; Bigall, N. C. ; Resch-Genger, Ute
Luminophore stained micro- and nanobeads made from organic polymers like polystyrene (PS) are broadly used in the life and material sciences as luminescent reporters, for bead-based assays, sensor arrays, printable barcodes, security inks, and the calibration of fluorescence microscopes and flow cytometers. Initially mostly prepared with organic dyes, meanwhile luminescent core/shell nanoparticles (NPs) like spherical semiconductor quantum dots (QDs) are increasingly employed for bead encoding. This is related to their narrower emission spectra, tuneability of emission color, broad wavelength excitability, and better photostability. However, correlations between particle architecture, morphology, and photoluminescence (PL) of the luminescent nanocrystals used for encoding and the optical properties of the NP-stained beads have been rarely explored. This encouraged us to perform a screening study on the incorporation of different types of luminescent core/shell semiconductor nanocrystals into polymer microparticles (PMPs) by a radical-induced polymerization reaction. Nanocrystals explored include CdSe/CdS QDs of varying CdS shell thickness, a CdSe/ZnS core/shell QD, CdSe/CdS quantum rods (QRs), and CdSe/CdS nanoplatelets (NPLs).
Thereby, we focused on the applicability of these NPs for the polymerization synthesis approach used and quantified the preservation of the initial NP luminescence. The spectroscopic characterization of the resulting PMPs revealed the successful staining of the PMPs with luminescent CdSe/CdS QDs and CdSe/CdS NPLs. In contrast, usage of CdSe/CdS QRs and CdSe QDs with a ZnS shell did not yield luminescent PMPs. The results of this study provide new insights into structure–property relationships between NP stained PMPs and the initial luminescent NPs applied for staining and underline the importance of such studies for the performance optimization of NP-stained beads.
Fluorescent labels have strongly contributed to many advancements in bioanalysis, molecular biology, molecular imaging, and medical diagnostics. Despite a large toolbox of molecular and nanoscale fluorophores to choose from, there is still a need for brighter labels, e.g., for flow cytometry and fluorescence microscopy, that are preferably of molecular nature. This requires versatile concepts for fluorophore multimerization, which involves the shielding of dyes from other chromophores and possible quenchers in their neighborhood. In addition, to increase the number of readout parameters for fluorescence microscopy and eventually also flow cytometry, control and tuning of the labels’ fluorescence lifetimes is desired. Searching for bright multi-chromophoric or multimeric labels, we developed PEGylated dyes bearing functional groups for their bioconjugation and explored their spectroscopic properties and photostability in comparison to those of the respective monomeric dyes for two exemplarily chosen fluorophores excitable at 488 nm. Subsequently, these dyes were conjugated with anti-CD4 and anti-CD8 immunoglobulins to obtain fluorescent conjugates suitable for the labeling of cells and beads. Finally, the suitability of these novel labels for fluorescence lifetime imaging and target discrimination based upon lifetime measurements was assessed. Based upon the results of our spectroscopic studies including measurements of fluorescence quantum yields (QY) and fluorescence decay kinetics we could demonstrate the absence of significant dye-dye interactions and self-quenching in these multimeric labels. Moreover, in a first fluorescence lifetime imaging (FLIM) study, we could show the future potential of this multimerization concept for lifetime discrimination and multiplexing.
Chierici, Andrea ; Ciolini, Riccardo ; Lo Frano, Rosa ; D’Onofrio, Antonio ; Sabbarese, Carlo ; Pandalone, Antonio ; Romoli, Mauro ; di Meo, Paolo ; Finocchiaro, Paolo ; Conti, Enrico ; Gonella, Franco ; Andreetto, Paolo ; Checchia, Paolo ; Niederleithinger, Ernst ; d’Errico, Francesco
A monitoring and surveillance system is a mandatory element to ensure that a radioactive waste disposal facility provides and meets the required level of safety during both its operational and closure periods. In this study an innovative approach for the identification and monitoring of the structural integrity of stored radioactive drums is presented. The activities were carried out in the context of the European Project PREDIS, whose goal is the development of a robust and reliable sensing technology for monitoring and long-term storage of radioactive waste packaging systems.
Specifically, the focus was set on the development of innovative and smart sensor technologies, non-destructive examination tools, and/or devices capable to improve the safety of the storage by minimizing the number of interventions of cemented waste packages. Both conventional and innovative techniques, such as muon-tomography, SiLiF neutron and SciFi gamma detection, or contactless and smart radio transceiver technology provided with radiation monitoring sensors, have been considered and adapted for the use under repository conditions. Indeed, gamma and neutron detection techniques exploit the radiological information coming from inside the drums, while imaging techniques proved to be effective in spotting high density objects embedded inside the concrete: together, they allow to improve safety and security and can provide an early alert on behavioral changes hinting at anomalies in the drums.
A reliable monitoring and oversight system is essential to guarantee the safe operation and eventual closure of radioactive waste disposal facilities. With recent technological advancements, there is now the capability to deploy distributed wireless sensor networks that are cost-effective and low in power consumption. Such networks are versatile, finding applications in several civil, environmental, and industrial sectors. This work presents a novel system and method for identifying and continuously monitoring the integrity of stored radioactive waste packages. The proposed approach, developed by the University of Pisa in the context of the H2020 European Project PREDIS, employs a network of wireless node devices, provided with solid-state micro-power radiation detectors tasked with the measurement of gamma-rays and thermal neutrons coming from within cemented waste drums. Collected data are automatically transmitted across the storage site via Long Range radio technology and forwarded to cloud-based or offline platforms, allowing for further visualization, data processing, and safe storage. The system highlights the feasibility of autonomously and passively gathering data from radioactive waste drums over extended distances (more than 250 m in non-line-of-sight conditions), decreasing the reliance
on portable or automated scanning mechanisms. In line with its capability for autonomous, long-range data collection, the system satisfies the requirement for structural integrity, containment, and confinement of packaging throughout both interim and long-term disposal of radioactive wastes, thereby playing a key role in reinforcing the safe management of radioactive waste.
Any surface in the environment acts as hotspot for microbial attachment and activity. These biofilms represent the interface between humans and the environment.
While in the past biofilms were often seen as disturbance, we now start to understand the enormous potential of beneficial biofilms. They can be used in a broad range of applications and are sources for new microorganisms and traits. After all, biofilms represent a great example for a collaborative lifestyle.
Residual stress formation during repeated gouging and repair welding cycles of high-strength steels
(2024)
The construction of foundation and erection structures for wind power plants requires the use of modern, sustainable and resource-efficient high-strength fine-grained structural steels. Weld defects due to the welding process are unacceptable. To overcome this issue, local thermal gouging followed by re-welding is a common and cost-effective method. The high shrinkage restraint of the gouge by the surrounding structure can cause crack initiation when design and re-weld induced residual stresses are superimposed. This risk is intensified by the progressive degradation of the microstructure and mechanical properties of high-strength steels during the weld repair process.
This investigation focuses on high-strength steels S500MLO for offshore applications and S960QL for mobile crane applications. The reduction and development of residual stresses caused by local thermal gouging and re-welding was investigated. Digital Image Correlated (DIC) stress-strain analysis was performed during preheating, welding and cooling. The results of the global DIC analysis and local longitudinal and transverse residual stresses of the weld determined by X-ray diffraction were found to be in good agreement. Furthermore, different stress levels were identified during gouging and welding. Repeated repair cycles led to an increase of longitudinal and transverse residual stresses in the weld metal as well as a hardness increase in the heat affected zone.
Machine learning-assisted equivalent circuit identification for dielectric spectroscopy of polymers
(2024)
Albakri, Bashar ; Turski Silva Diniz, Analice ; Benner, Philipp ; Muth, Thilo ; Nakajima, Shinichi ; Favaro, Marco ; Kister, Alexander
Polymers have become indispensable across fields of application, and understanding their structure–property relationships and dynamic behaviour is essential for performance optimization. Polymer membranes, particularly ion exchange membranes, play a crucial role in renewable energy conversion technologies, fuel cells, solar energy conversion, and energy storage. In this context, broadband dielectric spectroscopy (BDS) offers a powerful, non-destructive approach to investigate the electrical response and relaxation dynamics of polymers. These properties are investigated by parametrizing the system’s impedance response in terms of a network of circuit elements, i.e. the electrical equivalent circuit (EEC), whose impedance resembles the one of the system under investigation. However, the determination of the EEC from BDS data is challenging due to system complexity, interdependencies of circuit elements, and researcher biases. In this work, we propose a novel approach that incorporates a convolutional neural network (CNN) model to predict the EEC topology. By reducing user bias and enhancing data analysis, this approach aims to make BDS accessible to both experienced users and those with limited expertise. We show that the combination of machine learning and BDS provides valuable insights into the dynamic behaviour of polymer membranes, thus facilitating the design and characterization of tailored polymers for various applications. We also show that our model outperforms state-of-the-art machine learning methods with a top-5 accuracy of around 80% for predicting the circuit topology and a parameter fitting error as low as 0.05%.
Kowalski, Kurt ; Hulshoff, S.J. ; Ströer, P. ; Withag, J. ; Genot, A. ; Morgans, A.S. ; Bake, Friedrich ; Venner, K. ; Sanders, M.P.J. ; Hirschberg, Lionel
Indirect combustion noise due to the interaction of flow inhomogeneities with a choked combustion-chamber exit is an important cause of combustion instability in solid rocket motors.
Moreover, it is believed to be an issue in electrical-power generation turbines and aero-engines. If these flow inhomogeneities are essentially characterized by the fluid having a locally appreciablydifferent thermodynamic state, the acoustic response engendered by its interaction with the combustion-chamber exit is commonly referred to as entropy noise. In this paper, dedicated numerical-simulation results of entropy-patch choked-nozzle interactions are presented. Two types of entropy patches were considered: rectangular slugs and circular spots. Moreover, analytical-model-based analysis, of said simulation results, is presented. Based on said analysis, the authors posit the existence of three modeling regimes: the quasi-steady-modeling regime, the blended-physical-effects regime, and the inertial-modeling regime.
This presentation provides an introduction and intermediate results of the Horizon-Europe STAR4BBS project.It focuses on how to maximize the potential of Sustainability Certification Schemes (SCS) and labels to support a successful transition to a sustainable bio-based economy by assessing their effectiveness, robustness, and credibility.
Trace elemental analysis in human serum is integral in both clinical and research settings. Analyzing the level of some specific elements like Se and Zn helps indicate the nutritional and health status. Furthermore, elucidating the roles of trace elements in various physiological and pathological conditions can shed light on disease mechanisms and potential treatments. Inductively coupled plasma mass spectrometry (ICP-MS) stands out as a preeminent method for trace elemental analysis, given its exceptional sensitivity and minimal sample requirements. However, ICP-MS has challenges, such as argon-related interferences that hinder the accurate quantification of elements like Ca, Fe, and Se. The naturally most abundant isotopes of Ca (40Ca), Fe (56Fe), and Se (80Se) are subject to isobaric interference from 40Ar+, 40Ar16O+, and 40Ar2+, thereby complicating their direct measurement and preventing isotope dilution analysis.
In response to these challenges, nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) emerges as a viable alternative to ICP-MS, eliminating argon consumption and associated interferences. This study employed MICAP-MS to quantify Ca, Fe, and Se in 11 certified reference human serums using matrix-matched calibration and isotope dilution with the isotopes 40Ca, 56Fe, and 80Se. The results obtained with both methods were validated against certified values, and the suitability of MICAP-MS for isotope dilution was evaluated. Additionally, the performance of MICAP-MS in the Na matrix was investigated and discussed alongside the impact of organic species.
We present our approach and methodology for simulating piping erosion, which occurs during the installation process of suction bucket foundations for offshore wind turbines. We show several simulations and analyze the hydrodynamic and contact forces acting on the granular fabric and the differential pressure of the fluid phase. We demonstrate weak scaling performance on the LUMI supercomputer with a parallel efficiency of up to 90% for 4096 Graphics Compute Dies.
Barriers to transitioning to a circular bio-based economy: Findings from an industrial perspective
(2024)
Dace, Elina ; Cascavilla, Alessandro ; Bianchi, Marco ; Chioatto, Elisa ; Zecca, Emy ; Ladu, Luana ; Yilan, Gülsah
The transition from a linear fossil-based to a circular bio-based economy represents an opportunity and a suitable pathway for achieving several sustainable development goals. However, the transition is a complex process since it requires transformative policies, purposeful innovation, access to finance, risk-taking capacity as well as new and sustainable business models and markets. Accordingly, the first step in this transition process is the identification of barriers that are hampering the transition to a sustainable circular bio-based economy. With this motivation in mind, this study reviews grey literature to identify barriers focusing on four critical sectors facing major challenges within the current linear economy and requiring a sustainable transition most urgently: construction, chemicals, plastics, and textile sectors. Employing an adapted STEEP methodology (Social, Technological, Economical, Environmental, Political), a total of 193 different barriers have been identified and clustered under six categories: cultural, technical, economic, environmental, governance, and structural. Regardless of the sector, cultural and structural barriers are identified as the most prominent; the lack of incentives for consumer behaviour change and lack of stakeholder collaboration were the most cited barriers among the literature records. From a value chain perspective, most of the barriers are related to the material processing and product manufacturing stage. Finally, potential solutions, extracted from the grey literature, are proposed to fill the gaps and overcome the identified barriers. Many of the identified barriers are common across the four investigated sectors, indicating the solutions or measures can be applicable in a wider perspective to promote the transition in the right direction.
Pavasarytė, Lina ; Azevedo do Nascimento, Allana ; Cysne Barbosa, Ana Paula ; Trappe, Volker ; Melo, Daniel
Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables.
The Microplastic Microbiome
(2024)
Microplastics represent man-made and newly emerging surfaces in our ecosystems, where they interact with microorganisms. The ecosystem in focus of this presentation will be the aquatic environment. It will be portrayed, which microorganisms use microplastics as a habitat, how environmental factors shape this colonization, and why the biodegradation of plastics in the ocean is an overall unlikely process. We will also discuss whether potentially pathogenic microorganisms use microplastics as a raft. Finally, possible adaptation mechanisms of plastic-colonizing microorganisms will be presented, such as the production of photoreactive molecules. The microplastic microbiome has a large potential to harbor so far unknown species with curious traits, representing an exciting research topic for the future.
Various software products for the simulation of industrial X-ray radiography have been developed in recent years (e.g., aRTist 2, CIVA CT, Scorpius XLab, SimCT, Wilcore) and their application potential has been shown in numerous works. However, full systematic approaches to characterise a specific CT system for these simulation software products to obtain a truthful digital twin are still missing. In this contribution, we want to present two approaches to obtain realistic grey values in X-ray projections in aRTist 2 simulations based on measured projections. In aRTist 2, the displayed grey value of a pixel is based on the energy density incident on that pixel.
The energy density is calculated based on the X-ray tube spectrum, the attenuation between source and detector as well as an energy-dependent sensitivity curve of the detector. The first approach presented in this contribution uses the sensitivity curve as a free modelling parameter. We measured the signal response at different thicknesses of Al EN-AW6082 at different tube voltages (i.e., different tube spectra). We then regarded the grey values displayed by these projections as a data regression respectively an optimisation problem and obtained the sensitivity curve that is best able to reproduce the measured behaviour in aRTist 2. The resulting sensitivity curve does not necessarily hold physical meaning but is able to simulate the real system behaviour in the simulation software.
The second approach presented in this contribution is to estimate the sensitivity curve based on assumptions about the characteristics of the scintillation detector (e.g., scintillator material, scintillator thickness and signal processing characteristics). For this approach, a linear response function (linear relationship between the deposited energy per pixel and the resulting grey value) is assumed. If the detector characteristics, which affect the simulated deposited energy, are properly modelled, the slope and offset of the response function to match the measured grey values should be the same for different tube spectra. As the offset is constant and given by the grey values measured at no incident radiation, the slope is the remaining parameter to evaluate the success of the detector modelling. We therefore adapted the detector characteristics by changing the detector setup until the slope was nearly the same for all measured tube spectra. We are aware that the resulting parameters of the scintillator material and thickness might not be the real ones, but with those modelling parameters we are able to simulate realistic grey values in aRTist 2. Both of those approaches could potentially be a step forward to a full systematic approach for a digital twin of a real CT system in aRTist 2.
Lithium-ion batteries are a key technology for tackling challenges in energy and climate crisis, but up to 30 % are discarded right after production. Quality is closely related to the homogeneity of the used materials and coatings. Fluorine compounds, both in the polymer and from degradation of the electrolyte, are of special interest for the formation and aging of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) emerged as a fast and convenient method for depth-profiling of battery materials. However, fluorine remains a spectroscopic challenge due to a high excitation energy and only few strong emission lines in the UV/Vis spectral range.
We investigated the partial substitution of argon with neon in the plasma gas. The main emission line at 685.603 nm was monitored by both photo multiplier tube (PMT) with Czerny-Turner monochromator at 20 µm slit-size, and charge-coupled device (CCD) with 1200 lines/mm grating. For calibration, we used a set of hot-pressed copper cylinders with varying calcium fluoride amount fraction, ranging from 1.6 % to 4.4 %. Plasma gas mixtures with a mole fraction of 5 %, 10 % and 20 % neon in argon were used. Sensitivity in comparison to pure argon was increased by factor 4, 7 and 14, respectively. In general, PMT detection was more sensitive than CCD. As expected, sputter rates decreased with higher neon content in the plasma gas. Depth-profiling of the cathodes was performed in pulsed mode at constant voltage and pressure, which resulted in stable plasma conditions. We achieve matrix-independent quantitative information on fluorine distribution by correction based on sputter rates.
This advancement in GD-OES provides a more accurate analytical approach for evaluating the homogeneity of lithium-ion battery materials, potentially leading to more sustainable and cost-effective manufacturing processes.
To address the challenges of the climate crisis, multiple solutions for sustainable energy sources and storage systems are needed. One such solution is lithium-ion batteries (LIBs). Currently, 5 to 30 % of LIBs are discarded immediately after manufacturing. The homogeneous distribution of all materials used in the coating of cathodes and anodes is critical for the quality of LIBs. Furthermore, during formation i.e., the first steps of the charge/discharge cycling, the solid-electrolyte interphase forms on the anode particles, which has a huge impact on the performance. The same happens to some extent on the cathode, forming the cathode-electrolyte interphase. Fluorinated polymers and electrolytes are used in the manufacturing of LIBs. The electrolyte in particular is prone to degradation during formation and aging of the batteries. The interface of the cathode material with the aluminum current collector is also a critical point where degraded fluorine components cause pitting corrosion and at the same time promote passivation of the metal foil. Monitoring the spatial distribution of fluorine on these surfaces and interfaces is essential for sustainable LIB production.
Voss, Heike ; Knigge, Xenia ; Knapic, D. ; Weise, Matthias ; Sahre, Mario ; Hertwig, Andreas ; Sacco, A. ; Rossi, A. M. ; Radnik, Jörg ; Müller, Kai ; Wasmuth, Karsten ; Krüger, Jörg ; Hassel, A. W. ; Hodoroaba, Vasile-Dan ; Bonse, Jörn
Recent publications indicate that the order of electrochemical anodization (before or after the laser processing step) plays an important role for the response of bone-forming osteoblasts—an effect that can be utilized for improving permanent dental or removable bone implants. For exploring these different surface functionalities, multimethod morphological, structural, and chemical characterizations are performed in combination with electrochemical pre- and postanodization for two different characteristic microspikes covered by nanometric laser-induced periodic surface structures on Ti–6Al–4V upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ≈1 ps pulse duration, 67 and 80 kHz pulse repetition frequency) at two distinct sets of laser fluence and beam scanning parameters. This work involves morphological and topographical investigations by scanning electron microscopy and white light interference microscopy, structural material examinations via X-ray diffraction, and micro-Raman spectroscopy, as well as near-surface chemical analyses by X-ray photoelectron spectroscopy and hard X-ray photoelectron spectroscopy. The results allow to qualify the mean laser ablation depth, assess the spike geometry and surface roughness parameters, and provide new detailed insights into the near-surface oxidation that may affect the different cell growth behavior for pre- or postanodized medical implants.
In order to reduce global warming, the use of hydrogen as a renewable energy source is becoming more important. To enable this transition, unprecedently large amounts of hydrogen need to be safely transported and stored. Since hydrogen is usually stored and transported under pressure, one scenario to be considered is the release of hydrogen from a leakage with subsequent ignition. The resulting jet flame must be characterized with respect to the thermal radiation emitted into the environment to define safety distances. Various models that characterize the resulting flame shape and radiation already exist in the literature, but these are mainly based on empirical data from hydrocarbon jet flames. To verify the applicability of these models to hydrogen, real-scale tests are carried out at the BAM Test Site for Technical Safety (BAM-TTS) with the aim to assess the flame geometry and the emitted thermal radiation. Parameters such as leakage diameter (currently up to 30 mm), pressure (currently up to max. 250 bar) and mass flow (up to max. 0.5 kg/s) are varied. In particular, the focus will be laid on the measurement and modelling of the thermal radiation. The challenge here is the characterization of the flame geometry in an open environment and its impact on the thermal radiation. Existing heat radiation data from literature are mostly based on unsteady outflow conditions. The experimental setup used here allows for the generation of a steady-state outflow for several minutes and thus a direct comparability with existing (steady-state) models. Furthermore, stationary outflow tests with hydrocarbons (methane) were also carried out, which are intended to serve as reference tests for checking flame models based on hydrocarbon data. Following from the experimental investigations, modelling parameters such as the Surface Emissive Power (SEP) and the radiant heat fraction for hydrogen and methane will be compared to literature data.
Science Café Adlershof is having its next edition in 2024 on February 20th '24! We will have one speaker next week: Alexander Winckelmann is a PhD student at Bundesanstalt für Materialforschung und -Prüfung and will give a talk about his stay abroad in Switzerland - there will be free chocolates! There will be enough time to ask questions or simply chat with the guests and participants.
Sacrifice Few to Save Many: Fire Protective Interlayers in Carbon- Fiber-Reinforced Laminates
(2024)
The fire protection of carbon-fiber-reinforced polymer (CFRP) laminates often relies on flame-retardant coatings, but in some applications, their efficacy may diminish upon direct fire exposure due to rapid pyrolysis. This study introduces an innovative approach by integrating protective interlayers within the laminate structure to enhance the fire resistance. Various materials, including ceramic composite WHIPOX, titanium foil, poly(etherimide) (PEI) foil, basalt fibers, rubber mat, and hemp fibers, were selected as protective interlayers. These interlayers were strategically placed within the laminate layout to form a sacrificial barrier, safeguarding the integrity of the composite. Bench-scale fire resistance tests were conducted, where fire (180 kW/m2) was applied directly to the one side of the specimen by a burner while a compressive load was applied at the same time. Results indicate significant prolongation of time to failure for CFRP laminates with protective interlayers, which is up to 10 times longer. This innovative approach represents a potential advance in fire protection strategies for CFRP laminates, offering improved resilience against fire-induced structural failure.
Technological innovation and digitalization are transforming industries and organizations worldwide. Digital Maturity Models often serve as a reference point to monitor the digitalization progression through prescribed stages. Yet, little is still understood about (i) how a digital maturity model should be designed and deployed in a specific industry setting and (ii) the association between digital maturity and technology adoption. Building on extant literature and extensive interviews with industry experts, we first develop a digital maturity model in the context of the conformity assessment industry (a globally regulated industry responsible for assessing compliance of organizations with standards and regulations). Second, we implement the model and conduct a survey across 1447 organizations in 15 countries. Our findings reveal that the digital transformation journey of the industry progresses along five stages of maturity (with most organizations in the early/ intermediate stages of digital maturity) with distinctive patterns of technical and managerial practices across all stages. Adoption of technologies is (unsurprisingly) associated with higher digital maturity levels - albeit that association does not hold for complex technologies (such as Blockchain) and is impacted by country specifics (measured by the Digital Skills Gap Index). Our study provides insights into digital maturity and the adoption of technologies in an institutional environment that is highly regulated and conservative, in which high integrity of service provision is primary, and digitalization is a secondary focus of organizations.
Junge, Florian ; Wittwer, Philipp ; Sommerfeld, Thomas ; Gehrenkemper, Lennart ; Zoister, Christian ; Nickl, Philip ; Koch, Matthias ; Meermann, Björn ; Haag, Rainer
A systematic series of industrial-relevant polystyrene-based anion exchange resins that are functionalized with hydro- or fluorocarbon chains are compared regarding their adsorption behavior toward perfluorocarboxylic acids (PFCA) in respect to their charge, chain length, and type of chain. The results clearly show the dominance of electrostatic interactions in the adsorption process as uncharged adsorber materials showed no adsorption at all. In contrast, the charged adsorber materials showed in general a PFCA removal of 80% to 30% over the experiment depending on effluent fraction.
Unexpectedly, for perfluorobutanoic acid (PFBA) the highest removal rate is found with consistently >90%. Despite observing significant benefits in the adsorption of PFCA for fluoroalkylated adsorbers in comparison to their non-fluorinated counterparts, this effect of fluoroalkylation is comparatively small and can not be clearly attributed to fluorophilic interactions between the fluoroalkyl chains. These findings help clarifying that the introduction of fluorocarbon moieties in adsorber materials is not necessary in order to remove fluorocarbon molecules from the environment.
Schubert, Sven ; Komann, Steffen ; Neumann, Martin ; Reichardt, Adrian ; Müller, Lars ; Wille, Frank
The consideration of ageing mechanisms is with integration into the IAEA-requirements now obligatory for the design of transport packages. For packages intended to be used for shipment after storage the consideration of the effects of ageing mechanisms during storage in safety analyses and the implementation of corresponding instructions for operation and maintenance are required. Therefore, these packages have been maintained during storage in a manner that all requirements specified in the IAEA-requirements and in the applicable certificates of approval have been fulfilled.
BAM is the competent authority in Germany for evaluating the thermal and mechanical design of packages for the transport of radioactive materials. In this context, BAM also evaluates the aging mechanisms and aging effects occurring during the long-term storage period of such transport packages. BAM has developed a guideline for the implementation of ageing assessment and of the measures for ageing management into the approval procedure based on IAEA-requirements.
The goal of the presented paper is to introduce this guideline and the general approach for ageing management requirements and to describe the application to a specific package design. The type and amount of the ageing management not only depend on the use of the packaging, but also on the accessibility of the components that are considered in the ageing assessment. The different operating phases of a packaging are considered for the ageing assessment, such as loading, interim storage or transport.
The implementation of measures for ageing management is divided into three levels – systemic measures, package design related measures and documentation. The systemic measures are attributed to the general management system and define the whole activities for organization of ageing management like structure, responsibilities, documentation, reports and evaluation. The package design related measures are defined in an ageing management plan. These measures shall ensure that the anticipated changes of the package design under consideration of ageing effects still complies with the design approval specification. Therefore, an ageing surveillance program and, if necessary, a gap analysis program shall be developed. The ageing management documentation ensures the continuous documentation of the compliance of a specific package to the approved package design, comprising mainly records resulting from operation and surveillance.
Morphological and chemical analysis of mesoporous mixed IrOx-TiOy thin films as electrode materials
(2024)
Porous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too.
In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted.
Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation.
In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too.
ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to
measure the relative nanoparticle concentrations (relative populations of the two modes).
The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted.
Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene
(2024)
The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements.
Highlights
- Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques
- Determined growth rates depend on distinction between craze zone and crack
- The ratio of the present crack to the anteceding craze zone is validated theoretically
- The transition from crack propagation to ductile shear deformation is identified
- An already formed craze zone may still fail by ductile mechanisms
Bordeenithikasem, Punnathat ; Carpenter, Kalind C. ; Hofmann, Douglas C. ; White, Victor E. ; Yee, Karl Y. ; Rizzardi, Quentin ; Maher, Jacob ; Maaß, Robert
Advancements in bulk metallic glass thermoplastic forming unleash the potential to fabricate microscale metallic features with unparalleled precision and durability, i.e. microspine gripping structures for mobility platforms on planetary or in-space robots. Four designs of grippers were fabricated and rigorously tested. Coefficient of friction on four test surfaces were measured and compared to SiC paper and Velcro. The hardness and elasticity of the bulk metallic glasses make them a game-changer in the field, offering a superior alternative to conventional nonmetallic grippers.
Dzugan, J. ; Lucon, E. ; Koukolikova, M. ; Li, Y. ; Rzepa, S. ; Yasin, M.S. ; Shao, S. ; Shamsaei, N. ; Seifi, M. ; Lodeiro, M. ; Lefebvre, F. ; Mayer, U. ; Olbricht, J. ; Houska, M. ; Mentl, V. ; You, Z.
An interlaboratory study, involving eigth international laboratories and coordinated by COMTES FHT (Czech Republic), was conducted to validate tensile measurements obtained using miniature specimens on additively manufactured (AM) components and artifacts. In addition to AM 316L stainless steel (316L SS), a wrought highstrength steel (34CrNiMo6V, equivalent to AISI 4340) was also used. Based on the results, a precision statement in accordance with ASTM E691 standard practice was developed, intended for inclusion in a proposed annex to the ASTM E8/E8M tension testing method. The primary outcomes of the study highlighted the agreement between yield and tensile strength measured from miniature and standard-sized tensile specimens. Furthermore, most tensile properties exhibited similar standard deviations, offering users insight into the efficacy of miniature specimen applications.
The consideration of ageing mechanisms is with integration into the IAEA-requirements now obligatory for the design of transport packages. For packages intended to be used for shipment after storage the consideration of the effects of ageing mechanisms during storage in safety analyses and the implementation of corresponding instructions for operation and maintenance are required. Therefore, these packages have been maintained during storage in a manner that all requirements specified in the IAEA-requirements and in the applicable certificates of approval have been fulfilled.
BAM is the competent authority in Germany for evaluating the thermal and mechanical design of packages for the transport of radioactive materials. In this context, BAM also evaluates the aging mechanisms and aging effects occurring during the long-term storage period of such transport packages. BAM has developed a guideline for the implementation of ageing assessment and of the measures for ageing management into the approval procedure based on IAEA-requirements.
The goal of the presented paper is to introduce this guideline and the general approach for ageing management requirements and to describe the application to a specific package design. The type and amount of the ageing management not only depend on the use of the packaging, but also on the accessibility of the components that are considered in the ageing assessment. The different operating phases of a packaging are considered for the ageing assessment, such as loading, interim storage or transport.
The implementation of measures for ageing management is divided into three levels – systemic measures, package design related measures and documentation. The systemic measures are attributed to the general management system and define the whole activities for organization of ageing management like structure, responsibilities, documentation, reports and evaluation. The package design related measures are defined in an ageing management plan. These measures shall ensure that the anticipated changes of the package design under consideration of ageing effects still complies with the design approval specification. Therefore, an ageing surveillance program and, if necessary, a gap analysis program shall be developed. The ageing management documentation ensures the continuous documentation of the compliance of a specific package to the approved package design, comprising mainly records resulting from operation and surveillance.
We introduce a passive smart dust concept as a novel solution for environmental monitoring. Utilizing chemical reagents like colorimetric indicators and other chemosensors, these particles detect varying environmental conditions. We developed paper-based sensors that are both cost-effective and eco-friendly. In practical tests, these sensors, dispersed over a designated area, successfully identified hazardous substances by changing their color when exposed to acids or bases. This color change was remotely detectable using a drone-mounted color camera. The data thus obtained was processed through specialized software, accurately pinpointing areas of contamination. This method proves the efficacy and scalability of passive smart dust technology for real-time, environmentally sustainable remote sensing of hazardous materials
Use/distribution of cost-effective and biocompatible pieces of cellulose paper as passive optical chemosensors and readout by the camera system.
Modification of the paper surface using various chemically sensitive dyes (indicators) provides an optically detectable reaction and conclusions about the target substances and precise location.
Changes in Black Truffle (Tuber melanosporum) Aroma during Storage under Different Conditions
(2024)
The enticing aroma of truffles is a key factor for their culinary value. Although all truffle species tend to be pricy, the most intensely aromatic species are the most sought after. Research into the aroma of truffles encompasses various disciplines including chemistry, biology, and sensory science. This study focusses on the chemical composition of the aroma of black truffles (Tuber melanosporum) and the changes occurring under different storage conditions. For this, truffle samples were stored under different treatments, at different temperatures, and measured over a total storage time of 12 days. Measurements of the truffle aroma profiles were taken with SPME/GC–MS at regular intervals. To handle the ample data collected, a systematic approach utilizing multivariate data analysis techniques was taken. This approach led to a vast amount of data which we made publicly available for future exploration. Results reveal the complexity of aroma changes, with 695 compounds identified, highlighting the need for a comprehensive understanding. Principal component analyses offer initial insights into truffle composition, while individual compounds may serve as markers for age (formic acid, 1-methylpropyl ester), freshness (2-Methyl-1-propanal; 1-(methylthio)-propane), freezing (tetrahydrofuran), salt treatment (1-chloropentane), or heat exposure (4-hydroxy-3-methyl-2-butanone). This research suggests that heat treatment or salt contact significantly affects truffle aroma, while freezing and cutting have less pronounced effects in comparison. The enrichment of compounds showing significant changes during storage was investigated with a metabolomic pathway analysis. The involvement of some of the enriched compounds on the pyruvate/glycolysis and sulfur pathways was shown.
In infrared thermography, the interaction of the heat flow with the internal geometry or inhomogeneities in a sample and their effect on the transient temperature distribution is used, e.g., to detect defects non-destructively. An equivalent way of describing this is the propagation of thermal waves inside the sample. Although thermography is suitable for a wide range of inhomogeneities and materials, the fundamental limitation is the diffuse nature of thermal waves and the need to measure their effect radiometrically at the sample surface only. The crucial difference between diffuse thermal waves and propagating waves, as they occur, e.g., in ultrasound, is the rapid degradation of spatial resolution with increasing defect depth. This degradation usually limits the applicability of thermography for finding small defects on and below the surface.
A promising approach to improve the spatial resolution and thus the detection sensitivity and reconstruction quality of the thermographic technique lies in the shaping of these diffuse thermal wave fields using structured laser thermography.
Some examples are:
• Narrow crack-like defects below the surface can be detected with high sensitivity by superimposing several interfering thermal wave fields,
• Defects very close to each other can be separated by multiple measurements with varying heating structures,
• Defects at different depths can be distinguished by an optimized temporal shaping of the thermal excitation function,
• Narrow cracks on the surface can be found by robotic scanning with focused laser spots.
We present the latest results of this technology obtained with high-power laser systems and modern numerical methods.
Thermographic NDT is based on the interaction of thermal waves with inhomogeneities. The propagation of thermal waves from the heat source to the inhomogeneity and to the detection surface according to the thermal diffusion equation leads to the fact that two closely spaced defects can be incorrectly detected as one defect in the measured thermogram. In order to break this spatial resolution limit (super resolution), the combination of spatially structured heating and numerical methods of compressed sensing can be used.
The improvement of the spatial resolution for defect detection then depends in the classical sense directly on the number of measurements. Current practical implementations of this super resolution detection still suffer from long measurement times, since not only the achievable resolution depends on performing multiple measurements, but due to the use of single spot laser sources or laser arrays with low pixel count, also the scanning process itself is quite slow. With the application of most recent high-power digital micromirror device (DMD) based laser projector technology this issue can now be overcome.
Our studies deal with the application of fully 2D-structured DMD-based excitation and subsequent super-resolution-based defect reconstruction. We analyze the influence of different testing parameters, like the number of measurements or the white content of the excitation pattern. Furthermore, we have dealt with the choice of parameters in the reconstruction that have an influence on the underlying minimization problem in terms of compressed sensing. Finally, the results of the super resolution reconstruction are compared with the results based on conventional thermographic testing methods.
Salari, Farid ; Zocca, Andrea ; Bosetti, Paolo ; Hlaváček, Petr ; Italiano, Antonino ; Gobbin, Filippo ; Colombo, Paolo ; Kühne, Hans-Carsten ; Sglavo, Vincenzo M.
The present work addresses powder bed binder jetting additive manufacturing by selective magnesium phosphate cement activation. Despite the potential of this technology to aid the digitalization of the construction industry, the effect of processing parameters on the mechanical performance of printed materials has not yet been studied to generate a guideline for the further development of the technology. Statistical methodologies were used to screen the effect of four printing process parameters (printing speed, layer thickness, raster angle, and build direction on flexural and compressive strength). As the exploited technology works with constant fluid pressure, the physical interpretation of the effect of each factor can be considered taking into account the interactions between the binder materials in the powder bed. Analysis of variance (ANOVA) indicated that printing speed and layer thickness significantly affect mechanical performances. Furthermore, the layout of samples for the printing process is preferable to be parallel the printhead movement. An anisotropic behavior was observed, and the samples subjected to compressive forces parallel to the layer plane possessed lower strength values. This effect can be interpreted as a result of a weak area of low density in between layers, leading to a pronounced delamination under compression. Even though the strength of the printed material is not suitable for a structural concrete, it can be marginally improved by design of experiment and optimized for non-structural applications, such as for porous artificial stone. Design of experiment coupled with ANOVA methods can be used in the future to support the development of novel material mixtures, thus expanding the fields of application of this novel additive manufacturing technology.
A widespread recovery of waste heat requires a cost‐effective production of thermoelectric generators. Thermoelectric oxides are predestined for use at high temperatures. For manufacturing reasons, a multilayer generator design will be easily scalable and cost‐effective. To evaluate the potential of ceramic multilayer technology for that purpose, a multilayer of the promising thermoelectric oxides calcium cobaltite (Ca3Co4O9), calcium manganate (CMO, CaMnO3), and glass–ceramic insulation layers is fabricated. Cracks and reaction layers at the interfaces are observed in the microstructure. The compositions of these reaction layers are identified by energy‐dispersive X‐ray spectroscopy and X‐ray diffraction. Mechanical and thermal properties of all layers are compiled from literature or determined by purposeful sample preparation and testing. Based on this data set, the internal stresses in the multilayer after co‐firing are calculated numerically. It is shown that tensile stresses in the range of 50 MPa occur in the CMO layers. The reaction layers have only a minor influence on the level of these residual stresses. Herein, it is proven that the material system is basically suitable for multilayer generator production, but that the co‐firing process and the layer structure must be adapted to improve densification and reduce the tensile stresses in the CMO.
Bauer, L.J. ; Wieder, Frank ; Truong, V. ; Förste, F. ; Wagener, Y. ; Jonas, A. ; Praetz, S: ; Schlesiger, C. ; Kupsch, Andreas ; Müller, B.R. ; Kanngießer, B. ; Zaslansky, P. ; Mantouvalou, I.
Confocal micro-X-ray fluorescence (micro-XRF) spectroscopy facilitates three-dimensional (3D) elemental imaging of heterogeneous samples in the micrometer range. Laboratory setups using X-ray tube excitation render the method accessible for diverse research fields but interpretation of results and quantification remain challenging. The attenuation of X-rays in composites depends on the photon energy as well as on the composition and density of the material. For confocal micro-XRF, attenuation severely impacts elemental distribution information, as the signal from deeper layers is distorted by superficial layers. Absorption correction and quantification of fluorescence measurements in heterogeneous composite samples have so far not been reported. Here, an absorption correction approach for confocal micro-XRF combining density information from microcomputed tomography (micro-CT) data with laboratory X-ray absorption spectroscopy (XAS) and synchrotron transmission measurements is presented. The energy dependency of the probing volume is considered during the correction. The methodology is demonstrated on a model composite sample consisting of a bovine tooth with a clinically used restoration material.
Amphiphilic nanogels (ANGs) are promising carriers for hydrophobic cargos such as drugs, dyes, and catalysts.
Loading content and release kinetics of these compounds are controlled by type and number of hydrophobic groups in the amphiphilic copolymer network. Thus, understanding the interactions between cargo and colloidal carrier is mandatory for a tailor-made and cargo-specific ANG design. To systematically explore the influence of the network composition on these interactions, we prepared a set of ANGs of different amphiphilicity and loaded these ANGs with varying concentrations of the solvatochromic dye Nile Red (NR). Here, NR acts as a hydrophobic model cargo to optically probe the polarity of its microenvironment. Analysis of the NR emission spectra as well as measurements of the fluorescence quantum yields and decay kinetics revealed a decrease in the polarity of the NR microenvironment with increasing hydrophobicity of the hydrophobic groups in the ANG network and dye–dye interactions at higher loading concentrations. At low NR concentrations, the hydrophobic cargo NR is encapsulated in the hydrophobic domains. Increasing NR concentrations resulted in probe molecules located in a more hydrophilic environment, i.e., at the nanodomain border, and favored dye–dye interactions and NR aggregation.
These results correlate well with release experiments, indicating first NR release from more hydrophilic network locations. Overall, our findings demonstrate the importance to understand carrier–drug interactions for efficient loading and controlled release profiles in amphiphilic nanogels.
In this paper, we investigate the influence of different heat source pulse shapes by Infrared impulse thermography (IRT) on the results of the thermal shock response spectrum (TSRS) methodology. TSRS is a new alternative approach for evaluating impulse thermography (IRT) data based on an analogy to Shock Response Spectrum (SRS) analysis (ISO 18431) for mechanical systems. It allows processing the entire recorded signal without truncating the saturated thermogram, as in pulse-phase thermography (PPT) or thermal signal reconstruction (TSR). For this purpose, we use a widespread halogen lamp as heat source as well as laser spot. The laser source enables not only to generate a precise shape of the pulse, but also to heat a specific area of the sample uniformly. This makes it possible to suppress influences of lateral fluxes due to uneven distribution of the excitation source on the surface of the specimen and leads to improved results. In order to quantitatively compare the results and to investigate the possible influence of the source shape on the TSRS, the Tanimoto criterion and the signal-to-noise ratio (SNR) were applied to the region of interest (ROI) of the carbon fiber reinforced polymer (CFRP) laminate with artificial defects as defect detectability criterion.
Kianinejad, Kaveh ; Darvishi Kamachali, Reza ; Khedkar, Abhinav ; Manzoni, Anna ; Agudo Jácome, Leonardo ; Schriever, Sina ; Saliwan Neumann, romeo ; Megahed, Sandra ; Heinze, Christoph ; Kamrani, Sepideh ; Fedelich, Bernard
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.