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Organisationseinheit der BAM
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Eingeladener Vortrag
- nein (1)
In times of digital data processing and sharing, a central challenge for the Materials Science and Engineering (MSE) community is the complete digital representation of materials, including their relevant processing and microstructure details and the resulting properties. This digital representation, supported by digital infrastructures, enables entirely new qualities of collaborative work and is central to how we will conduct MSE research and develop products in the future. The main challenges are the composition, shaping, and description of the data so that it can be easily interpreted, trusted, and re-used. This presentation introduces our current effort to develop a best practice framework for generating and distributing creep reference datasets for Ni-based superalloys, which builds on previous approaches. Researchers can use such datasets to compare their own experimental or simulation results, used, for instance, to perform simulation-based alloy design and optimization or in the verification of the own testing equipment. The concept includes building an easily accessible digital infrastructure to annotate and discover the datasets and the integration of an ontology that aligns with the necessary metadata schema. With the help of an ontology, the reference dataset for creep can be semantically described, thus enabling the digital representation and reusage of shared concepts from domain experts and the community. To achieve this, it is necessary to establish a defined vocabulary with corresponding relations and annotations. The interplay between a digital infrastructure, the agreement on the necessary metadata and related metadata schema, and an underlying ontology will ensure that data and results can be easily shared, taken up, and re-used, thus fulfilling the FAIR principles (Findable, Accessible, Interoperable, Reusable). Furthermore, we aim to develop a widely accepted definition of reference data and data quality levels and to reach a self-supported community process. We intend to motivate the discussion about reference material datasets, necessary metadata, and future collaborations within the creep community.
The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM).
For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary.
The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM.
With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically).
❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility.
❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs.
❑ Selection of the threshold algorithm can significantly alter the reported ECD.
Non-equilibrium microstructure evolution in additive manufacturing (AM) is a major barrier for establishing a safe and sustainable application of AM in industrial processes. The constant heat source in the AM continuously affects the just-solidified grains beneath the melting pool, leading to directional grain growth (DGG). While real-time measurements of the non-equilibrium microstructure evolution is challenging, here developing a computational framework to systematically explore DGG becomes imperative.
We have advanced a comprehensive approach, integrating mean-field modeling and phase-field simulations, to elucidate the dynamics of DGG under an external driving force. Our simulations unveil a steady-state power-law grain growth kinetics during DGG, characterized by the interplay between curvature-driven dynamics at grain boundary junctions and directional driving forces.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Hybrid additive manufacturing is becoming increasingly important in the field of additive manufacturing. Hybrid approaches combine at least two different manufacturing processes. The focus of this work is the build-up of geometries onto conventionally manufactured parts using laser-based powder bed fusion of metals (PBF-LB/M). The hybrid build-up requires a precise position detection system inside the PBF-LB/M machines to determine the exact position of the existing component. For this purpose, high-resolution camera systems can be utilized. However, the use of a camera system is associated with several challenges. The captured images are subject to various distortions of the optical path. Due to these distortions, it is not possible to use the images for measurements and, therefore, it is not possible to calculate the positions of objects. In this study a homography matrix is calculated to correct keystone distortion in the images. Different calibration patterns have been tested for the calculation of the homography matrix. The influence of the number of calibration points on the precision of position detection of objects is determined. Furthermore, the influence of an additional camera calibration by using ChArUco boards is evaluated. The result is a camera calibration workflow with associated calibration pattern for a precise position detection of parts inside PBF-LB/M machines allowing a hybrid build-up with minimum physical offset between base component and build-up.
The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022.
Guaranteeing safety and security of citizens requires a significant effort and innovative tools from national and international agencies and governments, especially when it comes to the field of explosives detection. The need to detect Improvised Explosive Devices (IEDs) and Home-made Explosives (HMEs) at a point of suspicion, has grown rapidly due to the ease with which the precursors can be obtained and the reagents synthesised. The limited availability of immunoanalytical tools for HME detection presents an opportunity for the development of new devices, which enable a rapid detection and recognise the target analyte with high specificity and sensitivity. In this work, we introduce an optical biosensor for highly specific and sensitive HME detection. The immunoassay system is placed in a hydrogel environment permeable to the analyte and transparent to light interrogating the fluorescently labelled antibodies. The readout of the immunoanalytical system is realized with Supercritical Angle Fluorescence (SAF), an advanced microscopy technique. To accomplish this, we made use of recent, commercial high resolution (< 22 µm) Liquid Crystal Display 3D printers to fabricate a parabolic optical element with high refractive index (RI>1.5) and transmission values (>90%) from photo-resin. Aiming at a new generation of sensors, which not only can meet the requirements of trace detection, but can also be used for substance identification, the combination of immunoanalytical recognition with SAF detection offers a modularity and versatility that is principally well suitable for the measurements of target analytes at trace levels.
Revealing surface functionalities of micro- and nanoplastic particles’ surface by means of XPS
(2024)
Over the last 20 years, many researchers, politicians, and citizens themselves have become increasingly aware of the growing plastic problem of our time. Inadequate recycling concepts, collection points, and careless dumping of plastic products in the environment lead to an accumulation of plastic. External weather influences can cause these to degrade and fractionate, so that today microplastics (1-1000 µm, ISO/TR 21960:2020) [1] of different polymer materials can be detected in all parts of the world.
The precautionary principle applies to microplastics. The particles can break down further to form nanoplastics (<1 µm, ISO/TR 21960:2020) [1]. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending, however, investigations into the frequency, transport, possible sinks and entry paths must be taken into account. This is why monitoring of microplastics is already required in the revision of the Drinking Water Framework Directive [2]. The same is still pending in the final version of the revision of the Waste Water Framework Directive this year, but is expected.
Nanoplastics are particularly under discussion for having a toxic effect on humans and animals, as these particles are small enough to be absorbed by cells. For targeted toxicological studies, it is important to have test and reference materials that resemble the particles found in the environment. To mimic environmental samples, these materials should also have an irregular shape and show aging at the surface, which can be detected with XPS or SEM/EDS.
BAM in collaboration with the EMPIR project "PlasticTrace" works on a reference material candidate of nano-sized polypropylene (nano-PP) [3]. The nano-PP vials were tested for homogeneity with PTA and further characterized with bulk and surface-sensitive techniques. An SEM image and a corresponding XPS spectrum are presented in Figure 1. Raman measurements as well as XPS indicate an aged surface.