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Die Ziele zur Verringerung der CO2-Emissionen sind eng verknüpft mit der Entwicklung hocheffizienter und wirtschaftlicher Komponenten aus Stahl in der Anlagen-, Verfahrens- und Kraftwerktechnik, die für hohe kombinierte korrosive, tribologische, thermische und mechanische Beanspruchungen auf Anwendungsfall und Stahlwerkstoff abgestimmte Verschleißschutzschichten erfordern. Neben zunehmenden Forderungen infolge des Preis- und Lieferrisikos konventionelle Kobalt- durch Nickellegierungen zu ersetzen, wächst in der Industrie der Bedarf nach definierten Oberflächen hoher Güte bzw. Funktionsflächen für die Schutzschichten. Eine für Bauteile mit komplexer Geometrie erforderliche Fräsbearbeitung ist insbesondere für KMU aufgrund hohen Werkzeugverschleißes oftmals nicht wirtschaftlich realisierbar, jedoch für viele Einsatzfälle dringend notwendig.
In einem Gemeinschaftsvorhaben der BAM und des ISAF der TU Clausthal (Fosta P1550/IGF 21959 N) wird daher untersucht, wie mittels Legierungsmodifikationen der Schweißzusätze für nickelbasierte plasmaauftraggeschweißte Verschleißschutzschichten und durch Einsatz innovativer ultraschallunterstützter Fräsprozesse eine günstigere Zerspanbarkeit erreicht werden kann, ohne das Verschleißschutzpotential zu mindern.
Im vorliegenden Beitrag wird der Einfluss der mittels Legierungsmodifikation eingestellten Gefüge- und Ausscheidungsmorphologie auf die Zerspanung untersucht. Dies erfolgt anhand einer typischerweise für Schneckenmaschinen eingesetzte Verschließschutzlegierung zur Substitution entsprechender CoCr-Legierungen (Stellite), einer NiCrMoSiFeB-Legierung (Handelsname: Colmonoy 56 PTA). Durch metallurgische Untersuchungen und In-situ-Messung auftretender Prozesskräfte und Temperaturen an der Werkzeugschneide beim Fräsprozesses sowie der anschließenden Untersuchung von Werkzeugverschleiß und Oberflächenintegrität ist eine detaillierte Analyse und Korrelation zwischen den mikrostrukturellen Eigenschaften und der Zerspanbarkeit möglich. Die Vorgehensweise erlaubt einer Beurteilung des Einflusses der ultraschallunterstützten Fräsbearbeitung auf den Prozess sowie die resultierenden Oberflächenintegrität. Unter systematischer Anwendung dieser Methodik sowie der Berücksichtigung der Anbindung zum Stahlsubstratwerkstoff und der Wirksamkeit des Verschleißschutzes lässt sich letztlich eine gezielte Optimierung der Zerspanungssituation und des Verschleißschutzes erreichen. Die Erkenntnisse erlauben Handlungsanweisungen und Empfehlungen für Normen und Verarbeitungsrichtlinien, die besonders KMU eine sichere und wirtschaftliche Fertigung hochbelasteter Stahlkomponenten mit unkritischen, kostenreduzierten Werkstoffen ermöglichen sollen.
Alloy Modification and ultrasonic assisted milling of wear resistant alloys with defined surfaces
(2023)
The targets for reducing CO2 emissions are closely linked to the development of highly efficient and economical steel components in plant, process and power plant technology, which require wear protection coatings tailored to the application and steel material for high combined corrosive, tribological, thermal and mechanical stresses. In addition to increasing demands to replace conventional cobalt alloys with nickel alloys as a result of price and supply risks, there is a growing demand in industry for defined functional surfaces of high quality for these coatings. Milling is a standard process for finish machining. The desired properties of wear resistant alloys imply significant challenges for the milling process due to high tool wear and surface defects. Besides the hardness of the coating materials, especially due to the precipitations, inhomogeneous, anisotropic weld structures of the claddings lead to further deteriorations of milling processes due to unstable milling conditions and process forces.
A joint project of BAM and ISAF of TU Clausthal (Fosta P1550/IGF 21959 N) investigates the optimization of these challenging machining conditions by means of alloy modifications of the welding powder for plasma transferred arc cladding, without reducing the wear protection potential and using ultrasonic assisted milling process.
In this paper, the influence of the microstructure and precipitation morphology adjusted by means of alloy modification on machining is investigated. The alloy used is a NiCrMoSiFeB alloy (trade name: Colmonoy 56 PTA). Through metallurgical investigations and in-situ measurement of cutting forces and temperatures at the cutting edge during the milling process as well as the subsequent investigation of tool wear and surface integrity, a detailed analysis and correlation between microstructural properties and machinability is feasible. The findings allow recommendations for standards and processing guidelines, enabling safe and economical production of highly stressed steel components with non-critical, cost-reduced materials.
The safety demonstration of heavy weight type B transport packages used for storing spent nuclear fuel (SNF) or radioactive waste is ensured by a combination of physical testing and numerical calculations. While experiments are performed in accordance with the IAEA regulations for selected drop scenarios, Finite-Element-Method (FEM) simulations are used to predict the most damaging case and to investigate additional drop positions.
BAM as competent authority in Germany has performed different investigations of a welding seam for a typical large transport package made of A508 forged steel, where the bottom plate is welded to the cylindrical shell. The package has a mass of approx. 120 t. Results of physical drop tests with a full-scale model and accompanying preliminary FEM simulations are presented to determine the decisive stresses in the welding seam. A drop test only represents one set of a package and test parameters. A further parameter analysis is considered to account for allowable variations of packaging properties (e.g. resulting from the manufacturing process) and, based on IAEA requirements, the temperature dependence of the material behaviour. The results of the stress analyses from the drop test and the simulation form the basis and provide the input parameters for a fracture mechanics analysis. In addition to the IAEA specifications, further standards are taken into account for an in-depth investigation, see R6 [1], BS 7910 [2] and API 579-1/ASME FFS1 [3].
All the above-mentioned standards require a manufacturer-specific defect analysis with respect to size and position. Both result from the welding process and the following heat treatment regime. The maximum defect sizes are ensured with non-destructive test methods (such as ultrasonic or particle methods) as integral part of the manufacturing process of the welding seam. Another important parameter in the welding process is the residual stress (secondary stress). The combination of the primary and secondary stress determines the total stress in the welding seam. The most damaging case of the welding seam is determined and evaluated with help of the above-mentioned standards and taking into account the IAEA requirements with respect to defect sizes, material properties, primary and residual stress, yield strength etc.
The safe storage of radioactive material in nuclear waste repositories is a major task of our societies. The sealing function of such repositories is depending on the ability of the applied construction materials to form and maintain a geotechnical barrier with the surrounding rock. Corrosion of the construction material can lead to leakage of radioactive compounds and must therefore be avoided or minimized. Since concretes based on conventional Portland cement have not been found suitable in this context, alternative binders must be evaluated.
One such class of binders are hybrid cements, which are blends of low fractions of Portland cement or Portland clinker and high fractions of supplementary cementitious materials, such as blast furnace slag and fly ash, activated by an alkali salt. Besides a low heat of hydration and a sufficient early compressive strength [1], chemical similarities with ancient Roman concrete suggest an excellent durability in saline environments [2], which makes these cements potentially suitable for applications in nuclear waste repositories in evaporite rock, such as the Morsleben repository in Germany.
In the present study, two previously designed and characterized [3] hybrid cements, an alkali-activated slag/fly ash blend, and an OPC paste were studied regarding their resistance against corrosion in an aggressive saline solution. The saline solution was designed by the Gesellschaft für Anlagen- und Reaktorsicherheit (GRS) [Association for Facility and Reactor Safety] as a reference representing a solution forming as the result of contact of surface water with evaporite rock. The cement pastes were exposed to the saline solution up to 70 days and characterized by X-ray diffraction, thermogravimetric analysis and spatially resolved X-ray fluorescence spectroscopy. In addition, thermodynamic modelling was performed to simulate the alterations of the phase assemblage with increasing exposure to the saline solution and, thus, provide indications on the long-term durability of the cement pastes.
The experimental results revealed a correlation between the Portland clinker content of the cements and the resistance of the cement pastes against attack by the saline solution. This outcome was related to the formation of portlandite when sufficient clinker was available, which maintained the pore solution pH at ~12.5, and thus prevented the dissolution of cementitious phases. Once portlandite was consumed, C-N-A-S-H and ettringite dissolved and released calcium, aluminium, and hydroxide ions in the solution, maintaining the pH at ~10. In this pH range, the formation Cl-AFm phases was observed. At lower pH values, i.e., extended exposure durations, gypsum was the major corrosion product. The pH-dependent dissolution and formation of phases lead to pronounced zonation in the exposed cement pastes. Thermodynamic modelling indicated that the dissolved silicon from C-N-A-S-H reacts with magnesium ions in the saline solution to form M-S-H, and that long-term exposure eventually leads to a material rich in amorphous silica and brucite.
Blast furnace cements (CEM III) and alkali-activated slags are binders for concretes with several advantageous engineering properties, and their increased adoption in construction industry could contribute to reducing the CO2 emissions associated with cement production and use. However, the current knowledge about how these cements protect steel reinforcement in concretes against corrosion is very incomplete, which impedes their large-scale application. This knowledge gap is mainly due to the fact that these cements release sulfide and other reduced sulfur species into the concrete pore solution, the consequences of which for the state of the reinforcement and electrochemical measurements are not fully understood.
The present contribution first describes peculiarities of electrochemical measurements of steel in sulfide-containing cementitious materials and related solutions as reported in the literature and a recent report by EFC Working Party 11. It is demonstrated that the high sulfide concentrations in these systems lead to low open circuit potentials and low polarisation resistances, which may be incorrectly interpreted as indicating active corrosion of the steel.
Second, preliminary results of an ongoing project [funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) – 458297195] related to the passivation and corrosion initiation of steel in sulfide-containing solutions and mortars are presented. Eight mortars based on one alkali-activated blast furnace slag (BFS), three alkali-activated BFS/fly ash blends, one sodium sulfate-activated CEM III/C (‘hybrid cement’), one CEM III/C, one CEM III/B, and one CEM I (ordinary Portland cement, OPC) were produced, and their pore solutions expressed and analysed after 7, 14, 28, and 56 days of curing. The pH values of the solutions differed systematically, with the highest pH values recorded for the CEM I and the alkali-activated BFS/fly ash blends with a high proportion of fly ash, and the lowest pH recorded for the CEM III/B. The redox potentials of the solutions were between −500 mV and −340 mV vs. Ag/AgCl for the alkali-activated binders, approx. +10 mV vs. Ag/AgCl for the CEM I, and in between for the CEM III/B and the CEM III/C. As expected, the electrical conductivity was highest for the alkali-activated binders. These results are explained by the chemical compositions of the pore solutions of the mortars.
Finally, a test set-up to investigate the behaviour of steel in sulfide-containing solutions and the changes on subsequent oxygen and/or chloride addition is introduced. Preliminary electrochemical measurements of steel in sulfide-containing solutions are presented and discussed in the context of the above-mentioned data from the literature and the compositions of the pore solutions of the studied mortars.
Avoiding antimony – effect of Ca(H2PO2)2 on smoke emission and fire behaviour in brominated ABS
(2023)
The replacement of antimony trioxide (Sb2O3) in brominated flame-retardant ABS (ABS/FR) is of great interest. This study investigates the influence of calcium hypophosphite (CaP) in ABS/FR on flame retardancy and smoke emission. Different amounts of talc are added to ABS/FR/CaP to evaluate the influence of an inorganic barrier on smoke emission and flame retardancy. The cone calorimeter unveiled a reduction by 46% in PHRR for ABS/FR/CaP. Additional 8 wt.-% talc (ABS/FR/CaP/8Talc) reduced the PHRR by 61%. ABS/FR/CaP exhibited a more condensed phase action, which resulted in less smoke emission. The study investigates the influence of CaP in ABS/FR on the smoke toxicity, smoke density and the smoke particles distribution in the smoke density chamber (ISO 5659-2) coupled to a FTIR spectrometer and electrical low pressure cascade impactor (ELPI).
Human-made systems, also called “build environment” or “technosphere”, sustain human comfort as well as our industrial activities. These systems have become particularly widespread since the Industrial Revolution, i.e., since the 17th century. At the same time, these technical systems – buildings, monuments, energy production, transformation and transmission, water purification and supply systems - serve as new habitats for living organisms.
Life is ubiquitously present on our planet since a very long time: the Earth is 4.54 billion years old and microbial communities have played a key role on our planet for 3.7 billion years. Once human-made system appeared, microorganisms became an integral part of all types of technosphere infrastructure as well.
Here we will illustrate biosphere-technosphere interactions using a specific example of the black fungi and their impact on the efficiency of solar (photovoltaic) panels. This expanding renewable infrastructure for electricity generation is growing on all continents - and create a specific, arid habitat for stress-tolerant black fungi.
Black fungi were once discovered in hot and cold natural deserts – and now belong to the persistent colonisers of human-made deserts of solar parks. This new niche is evolving an impressive biodiversity. So far more than 60 isolates of black fungi belonging to Arthoniomycetes, Eurotiomycetes and Dothideomycetes were obtained from solar panels in Europe and Americas. Here we will present the analysis of this emerging anthropogenic biodiversity.
Opportunities for future research in the field include quantification of the microbial load on technosphere surfaces – along with characterisation of the corresponding microbial diversity. The strategy of precise measurement and characterisation will enable us to reliably determine the beneficial and harmful functions that living microorganisms play in the functioning of energy-generating systems – and technosphere in general.
The aim of the project is to develop an adequate model of laser induced plasma for conditions expected in space missions, i.e., vacuum, or low-pressure CO2 atmosphere. Numerical modeling will help to find optimal experimental parameters for the laser ablation under artificial lunar or Martian environments and obtain both qualitative, in terms of a composition, and quantitative, in terms of an elemental abundance, information about interrogated samples based on spectral data generated by the model. The best operational conditions will be found at a low cost without conducting tedious and time-consuming optimization experiments. The modeling approaches will be supported by machine learning to accelerate the optimization.
Improved Data Processing for Accurate Plasma Diagnostics with Implications for Calibration-Free LIBS
(2023)
Many LIBS papers report the determination of plasma temperature using the Boltzmann plot method or the determination of electron density using the Stark line broadening relation. This requires measuring the integrated intensities of the spectral lines and the linewidth under the assumption of optical thinness. It is taken for granted that this can be easily done either by working with the raw spectra or by fitting the appropriate function to the observed spectral lines. However, extracting the necessary information from raw spectral data is not as easy as it might seem. The quality of such extraction will depend to a decisive extent on the type of spectral instrument used. The spectrum emitted by the plasma is distorted by the device; an example is shown in Fig. 1. The elimination of this distortion belongs to the class of inverse problems, the successful solution of which fundamentally depends on the quality of the available information. When it comes to spectroscopy, the quality of information primarily means high spectral resolution and low noise. Not all spectrometers used in LIBS can provide the quality needed to solve the inverse problem; this casts doubt on many published plasma measurements. This communication will be devoted to the general shortcomings of spectral data processing and the inaccuracies in determining the plasma parameters resulting from these shortcomings. The analysis is based on the use of synthetic spectra generated by plasma with known temperature, particle density and electron density. The estimation of errors caused by inadequate processing of spectral data is made by comparing the initial and measured plasma parameters from the spectra. Recommendations will be made for which analytic function best approximates the observed spectral lines, and how data processing errors affect the accuracy of calibration-free LIBS will be discussed. These issues were only partially covered in previously published works, for example [1, 2].
In the LIBS literature, almost every second article reports the determination of the plasma temperature using the Boltzmann plot method or the determination of the electron density using the Stark line broadening relation. The first requires the measurement of the integrated intensities of the spectral lines, and the second requires the measurement of the linewidth, under the same assumption of optical thinness. It is taken for granted that this can be easily done either by working with the raw spectra or by fitting an appropriate function to the observed spectral lines. As a rule, reported data are not verified either by an alternative method (e.g., Thomson scattering) or by computer simulations using synthetic spectra.
However, the question of how to extract the necessary information from the raw spectral data is not as simple as it might seem. The quality of such an extraction will depend critically on the type of spectral instrument used, its resolution, and the noise superimposed on the data. The problem is that we do not see the spectrum emitted by the plasma, but the spectrum distorted by the measurement; an exaggerated example of such a distortion is shown in Fig. 1. The elimination of this distortion belongs to the class of inverse problems, the so-called ill-posed problems, whose successful solution crucially depends on the quality of the information available. When it comes to spectroscopy, quality of information primarily means high spectral resolution and low noise. Not all spectrometers used in LIBS can provide the quality needed to solve the inverse problem; this casts doubt on many published plasma measurements.
The current presentation will be devoted to general shortcomings in the processing of spectral data and inaccuracies in the determination of plasma parameters resulting from these shortcomings. The analysis is based on the use of synthetic spectra produced by plasma with known characteristics, i.e., temperature, species densities, and electron density. The estimation of errors caused by inadequate processing of spectral data is made by comparing the initial and reconstructed plasma parameters. Recipes will be given for which the analytic function best approximates the observed spectral lines, and how data processing errors affect accuracy of calibration-free LIBS will be discussed. These issues were only partially covered in previously published works, for example [1, 2, 3].
Many applications of LIBS require the measurement of plasma temperature and electron density, which in turn requires knowledge of the integrated line intensity and the shape of the spectral lines. While the integral intensity is preserved as light passes through the spectrometer, the shape emitted by an individual atom or ion is greatly distorted. This is due, firstly, to the transfer of light through the plasma (self-absorption), secondly, to the influence of the instrumental function of the spectrometer, and, thirdly, to the aberrations of the optical system. In addition, processing of spectral information, such as background removal, noise reduction, deconvolution, and line fitting, introduces additional errors in the reconstructed linewidth and line integral, which leads to erroneous temperature and electron density values.
This communication will be devoted to the general shortcomings of spectral data processing and the resulting inaccuracies in determining the plasma parameters. The analysis is based on the use of synthetic spectra generated by plasma with known temperature and particle density. The estimation of errors caused by inadequate processing of the spectral data is made by comparing the initial and determined plasma parameters. As a result, an improved data processing method will be proposed that takes into account the spectrum distortion by the instrumental function and integration on the pixel detector. The former is accounted for by convolution (instead of deconvolution) of the estimated line profile using a predetermined slit function, and the latter is achieved by piecewise integration of the line profile by the pixel detector, taking into account the pixel size and uniform or non-uniform pixel separation. Recommendations will be made for which analytic function best approximates the observed spectral lines and examples will be given for the application of this routine to calibration-free LIBS using both synthetic and experimental data.
Laser breakdown spectroscopy (LIBS) is a common tool for applications in various fields of science and technology. Originally an atomic analysis technique, LIBS was later extended to molecular analysis due to the transient nature of the laser-induced plasma, which develops from a hot dissociation stage on a nanosecond to several microsecond scale to a relatively cold recombination stage on a scale of 10 to 100 microseconds after breakdown. Molecules formed during the recombination stage or incompletely dissociated after ablation can be efficiently detected, allowing the analysis of "difficult" elements or even molecular isotopes. However, with a small amount of ablated material and a short lifetime of the luminous plasma, analytical signals, especially molecular ones, can be very weak.
Several methods have been proposed for reheating the plasma and increasing its lifetime, for example, a two-pulse LIBS or a LIBS combined with microwave radiation or with an electric spark discharge. Here we propose another one, LIBS combined with a capacitively coupled RF discharge at 13.6 MHz. The advantages of this combination are an increase in the lifetime of atomic and molecular emission and operation in a low-pressure atmosphere, which significantly reduces pressure line broadening and allows high-resolution spectroscopy. Another major advantage is operating in a chemically controlled atmosphere that can predictably drive desired chemical reactions. In this presentation, we will show the first results obtained with RF-LIBS combination. These will include separate and joint characterization of LIBS and RF plasmas and evaluation of its potential for elemental and molecular analysis and for plasma enhanced chemical vapor deposition.
In Neutron-Bragg-Edge Imaging (NBEI) experiments, we studied the phase transition during butt-welding of supermartensitic steel plates. Gas tungsten arc welding (GTAW) was used with a motorized torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) underneath the welding head could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. Also, the re-transformation into the martensitic phase upon cooling was detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm that is a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature.
As the world shifts to a decarbonized economy, the demand for hydrogen-based technologies is rapidly increasing. In order to make optimal use of hydrogen as an energy carrier, the infrastructure for hydrogen storage and transport in particular, must meet high technical safety standards. The indispensable basis for such safety assessments are the material properties, which must be evaluated under operating conditions that are as real as possible.
The conventional method for the assessment of the material properties in gaseous hydrogen is conducted by testing materials in high-pressure hydrogen gas in a pressure vessel (autoclave). It is an established method that allows to perform common standardized tests such as tensile, fatigue and crack growth tests under varying hydrogen conditions. However, this method is complex and entails high costs due to extensive safety regulations.
The hollow specimen technique is a more efficient test method, which can be used to assess the mechanical properties of materials under high-pressure hydrogen gas. The procedure is conducted by enclosing high-pressure gas into a hole along the axis of the tensile test specimen. Recently, this method has been successfully performed at pressures up to 1000 bar and over a wide range of temperatures. Due to the low hydrogen volume needed, this method requires minimal safety regulation; therefore, the costs are reduced when compared to the conventional autoclave technique. This method is now in a standardization process, which has been initiated by Japan as a new working package in ISO (TC 164/SC 1/WG 9).
The following contribution presents preliminary results obtained testing common grades of metastable austenitic stainless steel. For this purpose, the mechanical properties and fracture surface of solid and tubular specimens were assessed and compared using slow strain rate tensile (SSRT) test as part of the preliminary work at the Fraunhofer IWM. In a similar way, pipeline steels evaluated under hydrogen atmospheres using the geometry adapted by BAM will be presented. Within the framework of the TransHyDE flagship project, more results with the goal of supporting the standardization of the hollow specimen technique are expected to be obtained.
Volatile organic compounds (VOCs) emitted by furniture and
building materials can cause health issues. For an
improvement of indoor air quality low emitting materials
should be used. Quality assurance and –control (QA/QC)
measures require an emission reference material (ERM) with a
predictable emission rate of VOCs. The idea is to use porous
materials as ERM, which store the VOCs inside their pores and
emit them constantly.
Im Rahmen dieses Vortrags wurden aktuelle Arbeiten der BAM im Rahmen der Forschungszusammenarbeit mit dem Bundeswehrkrankenhaus Berlin zum primären Explosionstrauma vorgestellt. Den Schwerpunkt des Vortrags bildeten die Auswirkungen der kumulierten Belastung durch "low-level blast" auf das Gehirn von Einsatzkräften und Rückschlüsse für den Arbeitsschutz und die Arbeitsmedizin.
EU project ODYSSEUS
(2023)
Es werden das EU-finanzierte FE-Projekt ODYSSEUS, ausgewählte Ergebnisse zum Thema Home-made-explsosives (HMEs) und precursers, aktuelle Fragestellungen und ein Ausblick vorgestellt.
The ODYSSEUS project aims at improving knowledge about explosives precursers/HMEs and at developing and improving prognostic and detection tool to counter and prevent terrorist attacks. The contribution presents an overview of the ODYSSEUS approaches in countering and preventing terrorist attacks. The lecture will also show what knowledge has been gained to date about HMEs and new precursers and what consequences result from this.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen als auch die abgetrennten Partikel können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen. Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Nichtelektrischer Explosionsschutz - Grundlagen und Maßnahmen zum nichtelektr. Explosionsschutz
(2023)
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen als auch die abgetrennten Partikel können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen. Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Reducing CO2 emissions to 62 percent up to 2030 and achieving greenhouse neutrality up to 2050 are the key goals of the EU's climate protection legislation. The expansion of technologies for climate-neutral energy generation is not the only important contribution to reducing greenhouse gases, the efficient use of material systems is also a key factor. In the area of plant engineering, steel components are provided with a wear-protection coating for efficient use to protect them against corrosive, tribological, thermal and mechanical stresses. The wear-protection coatings are primarily made of Co alloys, which are to be replaced by alternative materials, such as nickel alloys, because of the poor working conditions regarding the extraction of the cobalt and because of the health risks. In terms of corrosion behavior, many applications require a crack-free wear protection layer and additional machining. Machining by milling is not economical for wear materials, especially for SME because of the high tool wear, but it is essential to produce defined surfaces with high quality.
Alloy modifications of the filler metals for nickel-based plasma deposition welded wear protection coatings and the use of innovative ultrasonic-assisted milling processes are examined to determine how more favorable machinability can be achieved without reducing the wear protection potential. The focus is on the NiCrSiFeB alloy, which is intended to replace CoCr alloys in the area of screw machines. The modification of hard facing layers in terms of microstructure and precipitation morphology as well as suitability for machining is investigated and compared with the CoCr alloy. In this aspect, the alloy modifications are generated by a PTA process by systematically adjusting the preheating and interpass temperatures, a crack-free wear-resistant layer can be generated, which is subsequently machined by a milling process. In addition to the crack-free properties,
the microstructure, the bonding as well as the mixing between the NiCrFeB alloy and a 1.8550 as well as between the CoCr alloy and a 1.4828 are analyzed and compared in the joining areas. In addition, heating and cooling rates are determined and a chemical analysis of the weld metals is performed. This study provides important knowledge about the differences between NiCrFeB alloy and CoCr alloys in terms of microstructure morphology, bonding and mixing behavior in the joining zones to the basic material.
Metal-organic framework-based biocomposites (MOF-biocomposites) are promising materials for biosensing, biocatalysis, and delivery of biopharmaceuticals. One of the most studied MOFs for bioapplications is ZIF-8 (zeolitic imidazolate framework 8) due to its high surface area, high thermal and chemical stability, and low cytotoxicity. The conventional synthesis of ZIF-8-biocomposites called biomimetic mineralization includes mixing selected biomolecules 2-methylimidazole, and soluble Zn2+ source in water.[3] Despite the high efficiency of the method, it does not allow for large-scale production and is restricted to hydrophilic biomolecules. Aimed at developing a scalable and versatile approach, we adapted our recently-reported ZIF-8 reactive extrusion for biocomposite production.
We selected bovine serum albumin (BSA) as an inexpensive model biomacromolecule for the preparation of biocomposites. The synthesis of BSA@ZIF-8 was performed using a twin-screw extruder ZE 12 HMI (Three-Tec Gmbh) at a mild temperature of 40 °C. Automatic volumetric feeder ZD 12B (Three-Tec GmbH) was used to supply the reagent mixture consisting of 2-methylimidazole, zinc source, and BSA. To initiate the reaction, a catalytic amount of EtOH was added using a peristaltic pump BT-L (Lead Fluid, China). Powder X-Ray diffraction (PXRD), thermogravimetric analysis (TGA), FTIR, and N2 adsorption were used to characterize the extrudates.
Highly crystalline and pure BSA@ZIF-8 with different BSA loadings was isolated after washing the extrudate with EtOH and sodium dodecyl sulfate. The EtOH feeding rate was optimized by following the protein encapsulation efficiency at a BSA mass fraction of 10%. A continuous extruder operation under optimized conditions showed good reproducibility and capability of producing biocomposites on the kilograms scale. These results provide highly valuable information for cheap and large-scale production of ZIF-8-based biocomposites. Due to the lack of restrictions on molecule size and solubility, our proof-of-concept study may significantly expand the selection of biomolecules for immobilization in ZIF-8, making the method applicable to various functional applications
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with laser light into the volume of a ceramic powder compound its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP) for the additive manufacture of filigree structures within the volume of ceramic slurries.
Manipulating ceramic powder compacts and ceramic suspensions (slurries) within their volume with light requires a minimum transparency of the materials. Compared to polymers and metals, ceramic materials are unique as they offer a wide electronic band gap and thus a wide optical window of transparency. The optical window typically ranges from below 0.3 µm up to 5µm wavelength. Hence, to penetrate with laser light into the volume of a ceramic powder compound its light scattering properties need to be investigated and tailored. In the present study we introduce the physical background and material development strategies to apply two-photon-polymerization (2PP) for the additive manufacture of filigree structures within the volume of ceramic slurries.
In this lecture, the safety assessment of hydrogen gas storage systems is presented using the example of composite pressure vessels. The main element is a probabilistic approval approach based on five steps. Firstly, the testing and evaluation of properties at the beginning of life are shown. Secondly, methods for artificial aging and the effect on the residual strength are presented. Thirdly, testing against dedicated accidents is introduced. Fourthly, effects on the surveillance of production quality are discussed. Finally, degradation and the end of life are estimated. Background information and examples are given for each step. The assessment presented is a method applicable for many safety-related systems.
In this lecture, the safety assessment of hydrogen gas storage systems is presented using the example of composite pressure vessels. The main element is a probabilistic approval approach based on five steps. Firstly, the testing and evaluation of properties at the beginning of life are shown. Secondly, methods for artificial aging and the effect on the residual strength are presented. Thirdly, testing against dedicated accidents is introduced. Fourthly, effects on the surveillance of production quality are discussed. Finally, degradation and the end of life are estimated. Background information and examples are given for each step. The assessment presented is a method applicable for many safety-related systems.
Der Vortrag stellt das Forschungsvorhaben RUNOFF vor, welcher auf der zweitägigen Veranstaltung „24. Projekttage der Bauforschung“ gehalten wurde. Die Präsentation erläutert zunächst die Bedeutung der Abschwemmung von Metallionen für die Bauindustrie und Umwelt. Dabei werden Faktoren, welche den Schadstofftransport im urbanen Raum begünstigen sowie Stadtentwässerungstypen vorgestellt. Anschließend folgen Folien zum wissenschaftlichen Hintergrund zur Ausbildung von Deckschichten, aktuellen Wissensstand sowie Lücken in der Korrosionsforschung von metallenen Werkstoffen unter atmosphärischen Bedingungen. Nach einer kurzen Übersicht zu den Hauptzielen des Forschungsvorhabens wurde detaillierter auf die Versuchsdurchführung sowie fünf der acht Arbeitspakete mitsamt Zwischenergebnissen eingegangen.
Der Vortrag stellt den aktuellen Stand des Forschungsprojekts RUNOFF vor. Dabei liegt der Fokus auf die Neubewertung der Dauerhaftigkeit von Zink und feuerverzinktem Stahl. Unter bewitterten Bedingungen erreichen beide Materialien stabile, karbonathaltige Deckschichten bereits nach einer Auslagerungszeit von zwei Monaten. In den parallel zu den Feldversuchen laufende Laborversuche werden aktuell der Einfluss dreier Faktoren (Ph-Wert, Winkel des Probenmaterials, Niederschlagsintensität) auf das Abschwemmverhalten von Zinkionen mithilfe eines an der BAM konstruierten Niederschlagsimulators untersucht.
Design and construction of a rainfall simulator to test metal runoff at atmospheric conditions
(2023)
A rainfall simulator was presented as an environmental assessment tool to quantify wash-off concentrations from metallic materials. It is part of the RUNOFF-project, which studies and re-assesses the durability of roofing and facade materials under current atmospheric conditions in Germany.
Studying building materials is important as they have a significant impact on achieving a variety of goals and targets within the sustainable developments goals (SDGs). The durability of materials is essential to reach sustainability. However, the durability of metallic materials is strongly depended on climate conditions, which have changed as a result of technical measures in industry, climate change and increasing urbanisation. In Germany at least, the data base is not up-to-date leading to prediction models regarding corrosion resistance and durability of metallic materials which can no longer be trusted and therefore need to be re-assessed and updated. Also, not only the demand for sustainable but also environmentally friendly building materials has increased dramatically. A number of construction materials produce chemical hazards, and therefore have negative impacts on water quality, soils health and ecosystems. To limit these impacts, environmental assessment methods and tools are needed to measure and quantify the inputs and outputs of building materials throughout their lifetime.
Die Präsentation stellt das Runoff-Projekt in seiner Gesamtheit vor. Dabei liegt der Fokus vor allem auf die verschiedenen Untersuchungsverfahren zur Neubewertung der Dauerhaftigkeit von Dach- und Fassadenmaterialien. Dazu zählen elektrochemische Untersuchungen der Deckschichtstabilität, die Bestimmung der Korrosionsprodukte sowie des Massenverlustes und die Identifikation wichtiger Einflussfaktoren.
Radiation biophysics
(2023)
X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. Furthermore, first data about the degradation of single-stranded DNA binding-proteins (G5P / GV5 and hmtSSB) under vacuum and NAP-XPS conditions are presented.
We give an overview about recent work concerning ionizing radiation damage to Oligonucleotides, plasmid DNA, DNA binding proteins (G5P), and DNA-protein complexes.
We focus on combining new experimental setups with Geant4/TOPAS particle scattering simulations to understand the effets of ionizing radiation.
X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further.
Die Bezeichnung „Tinte auf Papier“ bietet einen guten Einstieg in die Beschreibung der Materialität von Musikhandschriften; so haben sich zahlreiche Manuskripte erhalten, die mit Eisengallustinte auf Hadernpapier verfasst wurden.
Das Papier besteht aus Fasern meist pflanzlicher Herkunft und wird durch Entwässerung einer Fasersuspension auf einem Sieb gebildet. Der Abdruck des Schöpfsiebes (die Papierstruktur) und ein vorhandenes Wasserzeichen bieten Anhaltspunkte für Provenienz und Datierung; daneben erlaubt die Analyse der Fasern, der Füllstoffe und der Leimung eine weitere Charakterisierung des Schriftträgers.
Spätestens seit dem Mittelalter sind es Eisengallustinten, die das schwarze bis bräunliche Erscheinungsbild vieler Manuskripte auf Papier hervorrufen. Daneben lassen sich auch schwarze Rußtuschen oder farbige Auszeichnungstuschen nachweisen. Eisengallustinten werden durch Mischung einer eisenhaltigen Komponente mit Gerbstoffen hergestellt. Eisensulfat ist die am häufigsten genannte Eisen liefernde Zutat, daneben sind aber auch eisenhaltige Minerale, Nägel oder Rost denkbar. Die Gallussäure leitet sich ab aus den Galläpfeln, der krankhaften Veränderung einzelner Planzenteile verschiedener Eichenarten. Diese werden durch die Eiablage von Schlupfwespen hervorgerufen.
Wie schon beim Papier ermöglicht der materialanalytische Nachweis charakteristischer Beimischungen oder Verunreinigungen innerhalb der Tinten die Beantwortung kulturhistorischer Fragestellungen – gemeint sind hier die Unterscheidung von Original und Korrektur oder die Sichtbarmachung späterer Ergänzungen.
Der Vortrag widmet sich der materialwissenschaftlichen Analyse von Zeichnungen einiger Bauhausschülerinnen und Bauhausschüler und legt besonderen Fokus auf die verwendeten Farbmittel. Die Objekte werden mit nicht-invasiven bildgebenden Verfahren untersucht, in dem die Wechselwirkung zwischen Röntgen-, sichtbarem und infraroten Licht und den Zeichnungen studiert wird.
Dier Analysen liefern nicht nur generell Erkenntnisse über die Art und Zusammensetzung und damit das Alter der verwendeten Farbmittel. Durch die Auffindung von Vorzeichnungen, die Bestimmung von Überarbeitungen und Korrekturen werden Erkenntnisse über die Genese von Zeichnungen gewonnen. Auf der Basis dieser materialwissenschaftlichen Erkenntnisse werden die Begriffe Original, Kopie, Fälschung diskutiert.
Da die nicht-invasiven Untersuchungen einen umfassenden Einblick in die Materialität der – überwiegend aus Papier bestehenden – Objekte erlauben, bilden sie die Grundlage für die Erstellung nachhaltiger Konservierungs- und Restaurierungskampagnen und deren dauerhaften Erhalt.
Nondestructive testing of gas turbine blades is essential for their maintenance and service process which is critical to ensure both safety and efficiency of these highly stressed parts. In this presentation, a novel ultrasonic testing method is explored in order to acquire part thickness information in the turbine blade’s airfoil. In established industry processes, the measurements are mainly carried out manually and only at a few specific positions of the inspected parts. The proposed method scans the part using a robot arm guiding an ultrasonic array sensor. For ultrasonic coupling to the complex-shaped surface geometry, the inspected part and sensor are immersed into water. A two-step TFM[1, 2] (Total Focusing Method) approach is used to reconstruct the outer and inner surfaces subsequently from the ultrasonic raw data, which are acquired using the FMC[3] (Full Matrix Capture) measurement principle. For each sensor position, the location and geometry of the outer surface is first identified and then used to create an image of an area inside the material. From that image, the inner surface is reconstructed. Finally, part thickness information is deducted from merging location data of inner and outer surface. The result is a high resolution, high precision mapping of the inspected part’s wall thickness.
The progress in the VAMAS Project #15" Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension" within TWA 34 Nanoparticle Populations is presented with highlight of the following points:
- Determine and compare particle size and shape distribution by means of:
• electron microscopy (SEM, TEM, STEM-in-SEM)
• atomic force microscopy (AFM)
• small angle X-ray scattering (SAXS)
- Determine uncertainty induced by deposition protocol from liquid suspension with comparison to known values from a prior ILC with already deposited nanoparticles on TEM grids.
- Provide comparative validation of protocols for the techniques other than TEM.
The progress of the VAMAS Project 16 "Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension" in TWA 34 Nanoparticle Populations is presented. Follwowing points are discusssed:
- Validate the performance of imaging methods to measure the relative number concentration
• electron microscopy (SEM, TEM) and atomic force microscopy (AFM)
• two modes of bimodal (30 and 60 nm) silica nanoparticles
- Validate the performance of small angle X-ray scattering (SAXS) for the traceable measurement of the number concentration of the two modes.
Wasserstoff als flexibel einsetzbarer und leicht transportierbarer Energieträger bildet eine Schlüsselkomponente auf dem Weg zu einer klimaneutralen Energiewende. Zur Speicherung von gasförmigem Wasserstoff kommen bei stationären und auch mobilen Anwendungen meist Druckbehälter aus Verbundwerkstoffen zum Einsatz. Dabei ist für den Betrieb der Behälter die Gewährleistung der Sicherheit von großer Relevanz. Structural Health Monitoring (SHM) bietet einen innovativen Ansatz, um sowohl die Sicherheit als auch die Zuverlässigkeit der Druckbehälter zu gewährleisten und kritische Versagensfälle zu vermeiden.
Zur kontinuierlichen Überwachung und Bewertung des Zustands eines Wasserstoffdruckbehälters wird in dem vorliegenden Beitrag eine aktive Methode präsentiert, die auf geführten Ultraschallwellen basiert. Dabei kommt das Pitch-Catch Verfahren zwischen Sender und Empfängern zur Überwachung der strukturellen Integrität zum Einsatz. Auf Grundlage des untersuchten Wellenausbreitungsverhaltens im Druckbehälter sowie der Geometrieeigenschaften wird ein Sensornetzwerk aus piezoelektrischen Flächenwandlern (PZT) zur Abdeckung des zu überwachenden Bereichs entworfen. Ziel ist es mit Hilfe eines Optimierungsalgorithmus eine größtmögliche Abdeckung bei gleichzeitiger Minimierung der Anzahl der Sensoren zu erreichen. Zudem soll eine gleichmäßige und platzsparende Verteilung im Vordergrund stehen, so dass zukünftig weitere Messmethoden auf dem Druckbehälter angewendet werden können (z. B. durch akustische oder faseroptische Sensoren).
Das für die Anwendung optimierte Sensornetzwerk wird anschließend hinsichtlich der Robustheit bei der Schadenserkennung und -lokalisierung durch Aufbringen von künstlichen Schäden evaluiert. Die Ergebnisse zeigen, dass die künstlichen Schäden am Wasserstoffdruckbehälter nachgewiesen werden können.
The application of composite overwrapped pressure vessels (COPV) to store hydrogen and other compressed gases, especially when operating at high pressures, imposed the need for an innovative and reliable approach to ensure the safe operation of the system. Continuous structural health monitoring (SHM) based on ultrasonic guided waves (GWs) is a promising approach due to the ability of the wave to propagate for long distances and go around complex structures, moreover the high sensitivity to various failure modes such as delamination, matrix cracking and debonding. In this study, we scrutinize the behavior of (GWs) within the COPV using a network of PZT elements that are used for excitation and sensing. A laser doppler vibrometer (LDV) was also used to scan the surface of the vessel in various directions. L(0,1) and L(0,2) were observed in the captured signal. The L(0,2) appeared to be a dominant mode in the COPV and was capable of propagating along the entire length and maintaining a good signal-to-noise ratio. The L(0,2) mode maintained the same phase velocity when it is captured at various excitation angles (0, 45, and 90 degrees). The reduced effect of the orthotropy of the materials on the propagating waves is an important result as it will reduce the complexity in data processing when performing damage identification.
While hydrogen is one of the most promising energy carriers, the safety of hydrogen storage technology remains one of the most important factors for technological and societal approval. While the engineering safety factors of the pressure vessels are kept high, the periodic inspection and the limited lifetime are making the application very costly considering manpower, time, money, and material waste. The development of an integrated structural health monitoring system can allow an easy transition from the current situation to cost-effective predictive maintenance. Hence, we propose to integrate three different SHM systems into hydrogen pressure vessels, namely guided wave ultrasonics, acoustic emission, and fibre optic sensing, to continuously monitor the condition and integrity.
In this work, we evaluated the condition of a Type IV composite overwrapped pressure vessel using ultrasonic guided wave propagation. We mounted fifteen piezo-electric wafers on the composite cylinder by shaping three rings containing five sensors each. We acquired data from the sensor network following different boundary conditions with artificial damages on the selected locations. The data were evaluated with guided wave tomography techniques using ultrasonic features (amplitude, frequency, etc.) as well as artificial intelligence (AI). The results suggest that both traditional guided wave fusion techniques and AI-based characterization methods can detect artificial damages. In future work, it is planned to integrate acoustic emission and fibre optic sensing. Moreover, the measurement and the test results will be implemented into a digital twin to derive trends and make predictions on the damage propagation as well as the remaining useful lifetime.
This work has received funding from German Ministry of Economic Affairs and Climate Actions within the QI-Digital initiative (www.qi-digital.de).
An Amorphous Lewis-acidic Zirconium Chloro Fluoride as HF Shuttle: C-F Bond Activation and Formation
(2023)
In this work, we successfully synthesized amorphous zirconium chloro fluoride (ZCF), which exhibits medium lewis acidity. In addition to investigating the local coordination sphere around the Zr atoms and the material properties, we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present a heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorspar has been named among the 30 critical raw materials in the EU. 1 However, the sustainable transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. Herein, we present the heterogeneous catalyst zirconium chloro fluoride (ZCF) that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
Detaillierte Kenntnisse der elastischen Materialeigenschaften sind in vielen ingenieurtechnischen Bereichen von grundlegender Bedeutung. Insbesondere für die Anwendung von Predictive Maintenance und Structural- Health-Monitoring Methoden mit Ultraschall ist die genaue Kenntnis der elastischen Materialkonstanten eine Grundvoraussetzung. Die von den Herstellern zur Verfügung gestellten Angaben zu den elastischen Materialkonstanten, insbesondere für Polymere und faserverstärkte Kunststoffe, sind jedoch oft unzureichend, da diese vom Produktionsprozess abhängig sind und sich zusätzlich aufgrund von Materialabbauprozessen oder Ermüdung ändern können. In der Praxis liegen polymere Werkstoffe, faserverstärkte Kunststoffe und Metalle oft als dünne, plattenförmige Strukturen vor, in welchen sich geführte Ultraschallwellen (UGWs) ausbreiten können. In der aktuellen Forschung sind bereits verschiedene Neuronale Modelle zur Bestimmung der elastischen Konstanten und der Materialcharakterisierung mittels UGWs bekannt. Ein einfaches neuronales Netz, mit aus Dispersionsbildern extrahierten Werten für Frequenz und Wellenzahl ausbeutungsfähiger Moden als Eingabe, zur Vorhersage der elastischen Konstanten wird in verwendet. Ein rekurrentes Neuronales Netz mit einem Zeit-Frequenz Vektor als Eingabe wird in angewandt, während in ein 1D- Convolutional-Neuronal-Networks (CNN) unter Verwendung der zeitlichen Auslenkung der Grundmoden und in ein 2D-CNN unter Verwendung einer polaren Gruppengeschwindigkeitsdarstellung zur Bestimmung der elastischen Konstanten verwendet wird. In diesem Vortrag wird ein Ansatz zur Bestimmung der isotropen elastischen Konstanten von dünnen Platten auf der Grundlage von UGWs unter Verwendung von Dispersionsbildern und 2D-CNNs vorgestellt. Dispersionsabbildungen aus numerischen Simulationen werden mithilfe verschiedener Methoden vorverarbeitet, um realistische Messdaten zu simulieren. Mit den modifizierten Daten wird das Modell trainiert und die Architektur optimiert. Anschließend wird die Genauigkeit des erzeugten Modells mit realen Messdaten validiert. Es wird gezeigt, dass 2D-CNNs in der Lage sind, die isotropen elastischen Konstanten anhand multimodaler Merkmale aus Dispersionsbildern vorherzusagen, ohne dass eine anfängliche Schätzung der Parameter oder manuelle Merkmalsextraktion erforderlich ist.
γ-Hydroxybutyric acid (GHB) is a natural metabolite, which is currently used as a date rape drug. Particularly, GHB is rapidly eliminated and its detection in realistic environments is only possible within 6-12 h after ingestion. Owing to the increasing use of GHB for criminal purposes, a need has arisen to develop simple and in situ efficient assays for its identification in aqueous and alcoholic drinks. Based on the above, we report herein an indicator displacement assay (IDA) for GHB detection that consists of a Cu2+ complex with a tetradentate ligand and the fluorescent dye coumarin 343 (IDA probe 1). Firstly, the tetradentate ligand was synthesized by reductive amination of a 1,2-cyclohexyl diamine with 2-quinoline carboxaldehyde. Subsequently, this ligand was reacted with Cu(CF3SO3)2 to obtain the corresponding copper complex, which generates the final sensing ensemble by coordinating with coumarin 343 (IDA probe 1). The sensing mechanism relies on a displacement of coumarin 343 from the sensing ensemble 1 thus restoring its fluorescence, as a consequence of the higher binding constant between GHB and complex, showing a high sensitivity in MES buffer (50 mM, pH 6.0) (detection limit of 0.03 μM). Likewise, system design and optimization led to a straightforward integration into a lateral-flow assay without further treatment or conditioning of the test strips while guaranteeing fast overall assay times of 1 min (Figure 1). In this way, IDA probe 1 was incorporated into a coated PEG-glass fibre (PEG-GF) membrane to obtain a highly robust and sensitive lateral flow assay for GHB detection in spiked alcoholic drinks with a detection limit of 0.1 μM in less than 1 min coupled to smartphone readout.
The long-term preservation of our infrastructure requires not only intelligent sensor technology and highly developed monitoring procedures, but also innovative digital tools for analyzing, evaluating and utilizing the results. This includes mathematical and, in particular, probabilistic methods for damage detection and tracking as well as for calculating service life and maintenance cycles and data management. The example project Maintal Bridge Gemuenden as part of the AISTEC project shows the workflow for the implementation of structural health monitoring and experimental tests with a train of Deutsche Bahn. The influence lines, as one possible way for damage detection, were measured with a highly accurate GNSS System to locate the trains position when crossing the bridge. The results were compared to measurements from 1987 just before the bridge went in operation.
Ellipsometry is a highly valuable technology for bridging different measurement methods. As a fast, highly sensitive, and non-destructive optical technique with low environmental requirements, it is ideal for transporting measurement accuracy and for up-scaling measurements in the production environment. It can be used for highly precise determination of properties, material identity and correctness confirmation, as well as defect detection.
Comparable, traceable, and accurate electrical measurements, especially at small scales are one of the biggest challenges in the development of the electrical and electronic devices of the future.
In this project, we develop structured thin layer systems of the transparent conductive material indium tin oxide (ITO) to prove the concept of using these systems as standards for conductivity and permittivity. The layers are produced in a reactive magnetron sputtering process from raw ITO targets with additional oxidation achieved by oxygen injection. We present results of a study correlating the coating process conditions with the properties of the final layer material. We found that especially the temperature development during coating is of key importance and determines the layer properties to a large extent. We will discuss questions of homogeneity and reproducibility of the coating processes used. The finished layers undergo lithographic structuring and etching to produce patterns to serve as reference structures for scanning probe electrical measurements. TCOs have a large variety of applications. In this work we also study the usability of ITO for other purposes and investigate the stability of this material under application conditions.
In this workpackage of the ELENA project, we develop a way to express the measurement uncertainty of nanoscale determination of electrical propserties. The method developed aims to be usable for industrial contexts and described in technical documents and standards drafts. Standards and reference samples are used to make traceable measurements available for the end user.
Die Funktionalität von modernen technischen Komponenten liegt meist in der Oberfläche und in Beschichtungen. Das Design und die Herstellungsqualität von Beschichtungen ist essenziell für die optischen, elektrischen, mechanischen und chemischen Eigenschaften von Bauteilen, sowie für den Korrosions- und Verschleißschutz. In diesem Gremium bearbeiten wir Normen für die Qualitätssicherung von dünnen Schichten verschiedener Art. Dabei betrachten wir Eigenschaften wie Schichtdicke, Zusammensetzung, Haltbarkeit, Korrosionsbeständigkeit und physikalische Parameter von dünnen Schichten mit sehr vielfältigen Techniken. Neben klassischen Verfahren aus der Galvanik und Schichtmesstechnik, werden dabei auch neuere spektroskopische Verfahren wie Ellipsometrie und THz-Reflektion bedeutend. Unser Gremium ist offen für neue Mitglieder aus der Oberflächen- und Beschichtungsgemeinschaft.
After describing the basics of distributed fiber optic sensing in general and distributed fiber optic acoustic sensing (DAS) in particular, several currently and previously investigated fields of application of DASin infrastructure monitoring and seismic monitoring are presented. A focus is placed on seismic measurements and DAS measurements determining the dynamic responses of concrete structures to certain stimuli.
Since the function of materials is controlled by properties and processes on the atomic scale, ab initio based high-throughput methods are valuable strategies in materials design. For computational efficiency, they are however often restriction to T=0K calculations, while many technologically relevant materials properties and thermodynamic stabilities change when going from low to high temperatures. On the other hand, the constantly increasing performance of digital tools for simulation and data-driven science enables more targeted material development including these kinds of finite-temperature effects. A flexible infrastructure, including data management and workflow solutions is required to make this symbiosis user-friendly efficient. Within this presentation, examples from ab initio thermodynamics for the design of phase stabilities in hard-magnetic alloys and defect-phases in advanced high-strength steels will be demonstrated. We will discuss physical concepts with a focus at the impact of magnetic excitations. At the same time, the examples will be used to derive requirements and present solutions for a digital infrastructure. An outlook will be given to current strategies with the NDFI initiative NFDI-MatWerk.
Thermodynamic bulk phase diagrams have become the roadmap used by researchers to identify alloy compositions and process conditions that result in novel materials with tailored microstructures. On the other hand, recent progress in experimental atomic-scale characterization techniques allows one to study the local chemical composition at individual defects such as interfaces, grain boundaries, dislocations and surfaces. They show that changes in the alloy composition can drive not only transitions in the bulk phases present in a material, but also in the concentration and type of defects they contain. Defect phase diagrams, using chemical potentials as thermodynamics variables, provide a natural route to study these chemically driven defects. Our results show, however, that the direct application of thermodynamic approaches can fail to reproduce the experimentally observed defect formation.
Therefore, we extend the concept to metastable defect phase diagrams to account for kinetic limitations that prevent the system from reaching equilibrium. We use ab initio calculations based on density functional theory to quantify the extension of regions where defect formation is expected. We successfully applied this concept to explain the formation of large concentrations of planar defects in supersaturated Fe2Nb Laves phases. In addition, we identify in a joint study with experiments conditions and structures in Mg-Al-Ca alloys for defect phase occurrence. The concept offers new avenues for designing materials with tailored defect structures.
Understanding segregation to grain boundaries, and eventually their defect phase diagrams, is critical to enable rational grain boundary engineering for alloys design. Here, we discuss the progress and challenges one may face when generating such a database of defect-solute interactions, in the context of studying of grain boundary segregation of solutes and impurities in Fe GBs. To compute the large number of relevant defect-solute interactions we have performed high-throughput ab initio calculations using efficient and highly automated workflows using pyiron. We study has been performed across a representative set of coincident-site-lattice (CSL) type tilt GBs. Based on the large ab-initio datasets, we extract and analyse the chemical and structural trends observed in the solute segregation behaviour across the periodic table. The features which are most important in evaluating site segregation are presented and discussed.
Thermodynamic bulk phase diagrams have become the roadmap used by researchers to identify alloy compositions and process conditions that result in novel materials with tailored microstructures. On the other hand, recent progress in experimental atomic-scale characterization techniques allows one to study the local chemical composition at individual defects such as interfaces, grain boundaries, dislocations and surfaces. They show that changes in the alloy composition can drive not only transitions in the bulk phases present in a material, but also in the concentration and type of defects they contain. Defect phase diagrams, using chemical potentials as thermodynamics variables, provide a natural route to study these chemically driven defects. Our results show, however, that the direct application of thermodynamic approaches can fail to reproduce the experimentally observed defect formation.
Therefore, we extend the concept to metastable defect phase diagrams to account for kinetic limitations that prevent the system from reaching equilibrium. We use ab initio calculations based on density functional theory to quantify the extension of regions where defect formation is expected. We successfully applied this concept to explain the formation of large concentrations of planar defects in supersaturated Fe2Nb Laves phases. In addition, we identify in a joint study with experiments conditions and structures in Mg-Al-Ca alloys for defect phase occurrence. The concept offers new avenues for designing materials with tailored defect structures.
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable materials data space is therefore crucial in the digital transformation of an industrial branch.
Therefore, the “Innovation Platform MaterialDigital (PMD) funded by the German Federal Ministry of Education and Research (BMBF), aims to develop a sustainable infrastructure for the standardized digital representation of materials science and materials engineering. With its partners (KIT, Fraunhofer IWM, FIZ, Leibnitz IWT, BAM, MPIE), the PMD is committed to build up a materials science data space. To achieve this the PMD provides a prototypical infrastructure for the digitalization of materials implemented by decentralized data servers, standardized data schemas and digital workflows. Following the FAIR principles, it will promote the semantic interoperability across the frontiers of materials classes.
Standards, methods, and tools developed within the platform are deployed and consolidated within the context of currently near 20 BMBF-funded academic and industrial research consortia and made available to the material science community in general. In this context scientific workflows represent a major focus area, represented within the platform by the workflow frameworks pyiron and SimStack. In consequence, the platform is building up a digital library in form of a workflow store along with common standards for the definition and representation of digital workflows.
In this presentation we will describe the status of our Platform MaterialDigital with a focus on the workflow activities. The current status and the vision for dissemination of the solutions developed in the PMD within the community are provided.
Material science problems have intrinsically multiscale and multiphysics characters, and require us to employ a combination of methods on different time and length scales to resolve critical features. Normally creating workflows that connect data in multiple scales and various methods is a cumbersome task. Pyiron, an integrated development environment (IDE) for material science, contains modules for the atomistic as well as continuum scale that make a seamless connection possible. To this end, it provides a high-level coherent language in a unified workflow platform to study materials, for example, with density functional theory (DFT) simulations in the same framework as with the finite element method (FEM). In this work, in addition to the introduction of different features in pyiron and its continuum module, a couple of exemplary workflows are demonstrated, bridging the scales in pyiron. One such workflow is analyzing the elastoplastic response of metallic alloys, where the elastic properties of the system are dependent on the atomistic composition and structure of the alloy. We use pyiron atomistics to model the dependence of elastic moduli on the atomistic composition of Al-Mg alloys. Benefiting from the integration of DAMASK in the continuum module of pyiron, the model can be used as an input to simulate the elastoplastic response of the alloy under various loadings. In addition, finite element simulations using the FEniCS package are currently integrated into the continuum module and will be demonstrated in the presentation.
Since the function of materials is controlled by properties and processes on the atomic scale, ab initio based high-throughput methods are valuable strategies in materials design. For computational efficiency, they are however often restriction to T=0K calculations, while many technologically relevant materials properties and thermodynamic stabilities change when going from low to high temperatures. On the other hand, the constantly increasing performance of digital tools for simulation and data-driven science enables more targeted material development including these kinds of finite-temperature effects. A flexible infrastructure, including data management and workflow solutions is required to make this symbiosis user-friendly efficient. Within this presentation, examples from ab initio thermodynamics for the design of phase stabilities in hard-magnetic alloys and defect-phases in advanced high-strength steels will be demonstrated. We will discuss physical concepts with a focus at the impact of magnetic excitations. At the same time, the examples will be used to derive requirements and present solutions for a digital infrastructure. An outlook will be given to current strategies with the NDFI initiative NFDI-MatWerk.
Thermodynamic bulk phase diagrams have become the roadmap used by researchers to identify alloy compositions and process conditions that result in novel materials with tailored microstructures. Recent experimental studies show that changes in the alloy composition can drive not only transitions in the bulk phases present in a material, but also in the concentration and type of defects they contain. Defect phase diagrams in combination with density functional theory provide a natural route to study these chemically driven defects. Our results show, however, that direct application of thermodynamic approaches can fail to reproduce the experimentally observed defect formation. Therefore, we extend the concept to metastable defect phase diagrams to account for kinetic limitations that prevent the system from reaching equilibrium. We successfully applied this concept to explain the formation of large concentrations of planar defects in supersaturated Fe-Nb solid solutions and to identify in a joint study with experiments conditions in Mg-Al-Ca alloys for defect phase occurrence. The concept offers new avenues for designing materials with tailored defect structures.
Extensive experimental observations indicate the presence of nano-voids and the increase of free volume along the grain boundaries in hydrogen contaminated metals. This rate-dependent phenomenon motivates theoretical investigations of the underlying mechanisms. Here, a hydrogen enhanced cross-slip (HECS) mechanism in the close vicinity of the grain boundaries is demonstrated by direct molecular dynamics simulations. To this end, the interaction of the screw dislocations with a variety of symmetric tilt grain boundaries in H-charged and H-free bicrystalline nickel specimens is examined. The presence of segregated hydrogen atoms at the grain boundaries induces a stress field in their vicinity, and thus the barrier for cross-slip of screw dislocations considerably decreases. The enhanced crossslip of dislocations facilitates the formation of jogs. These jogs can form vacancies during the glide process. This mechanism shows nano-scale evidence of enhanced vacancy formation and subsequent increase in the free volume along the grain boundaries in the presence of H. This increase of the free-volume along the grain boundary dmaages the material and induce further embrittlement in addition to the direct effect of hydrogen in decreasing the fracture energy.
Defect-hydrogen interaction in Al alloys: Challenges and benefits revealed by ab initio calculations
(2023)
Climate change motivates the search for light-weight materials for transportation and energy storage solutions. As one of the challenges, the deleterious effect of hydrogen on the mechanical properties of metallic alloys is known to reduce the applicability of metallic alloys, motivating the characterization and simulation of hydrogen-defect interactions in these materials. In this work, the interaction of hydrogen with planar defects in aluminium has been investigated by means of ab initio simulations.
On the one hand, two distinct types of GBs have been considered – the Σ11(113) [011] with a close-packed interface structure and the Σ5(210) [001] with a more open interface structure – in order to reveal the mechanisms governing the H segregation energetics. The investigations are afterwards extended to the impact of solutes in the Al alloy. Two scenarios are compared: Their segregation to the grain boundaries and their binding in precipitates. We therewith gained insights into the role of the solute size on the structural and chemical embrittlement in absence and presence of hydrogen. A thermodynamic assessment of the impact of solutes onto H chemisorption in the interfacial vicinity is provided by performing a high-throughput analysis for potential alloying candidates. The identified trends of the solute-H interactions are used to examine the relative importance of changes in hydrogen enhanced decohesion as a thermodynamic effect.
On the other hand, the interaction of hydrogen with defects can be beneficial for the formation of metal hydrides. To enhance the formation and stability of such often highly volatile hydrides we have consider a novel concept: tailoring and employing the negative pressure of microstructural and structural defects to enhance H solubility and thus hydride formation. Using systematic ab initio and atomistic simulations, we demonstrate that an enhancement in the formation of hydrides at the negatively pressurized crack tip region is feasible by increasing the mechanical tensile load on the specimen. The theoretical predictions have been used to reassess and interpret atom probe tomography experiments for a high-strength 7XXX-aluminium alloy that show a substantial enhancement of hydrogen concentration at structural defects near a stress-corrosion crack tip. Based on these insights we derive strategies for enhancing the capability of metals as H-storage materials.
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable materials data space is therefore crucial in the digital transformation, both in academia and industry.
Therefore, the consortium NFDI MatWerk aims to develop a sustainable infrastructure for the standardized digital representation of materials science and engineering (MatWerk). The goal is to seamlessly integrate decentralized data and metadata, experimental and computational workflows, and a materials ontology to maximize interoperability and reproducibility of materials data processing. To this end, data use profiles of participant projects from different sub-disciplines are analyzed to identify the most relevant scientific scenarios within MatWerk.
Similarly, the Plattform MaterialDigital (PMD) is committed to provide a prototypical infrastructure for the digitalization of materials in an industrial context implemented by decentralized data servers, semantic data schemas and digital workflows. The standards, methods, and tools developed within the PMD are deployed and consolidated within the context of currently more than 20 BMBF-funded academic and industrial research consortia. Scientific workflow environments represent a major focus area, including efforts to improve the definition and representation of digital workflows, as well as their distribution in form of a workflow store.
In this presentation we will describe the overarching visions behind these initiatives, their status, and progress of dissemination with a focus on the workflow activities. Following the philosophy of both consortia, specific examples will be used to demonstrate innovative and pragmatic solutions.
Suitable material solutions are of key importance in designing and producing components for engineering systems – either for functional or structural applications. Materials data are generated, transferred, and introduced at each step along the complete life cycle of a component. A reliable materials data space is therefore crucial in the digital transformation and an important prerequisite for machine learning in materials science.
Therefore, the consortium NFDI MatWerk aims to develop a sustainable infrastructure for the standardized digital representation of materials science and engineering (MatWerk). The goal is to seamlessly integrate decentralized data and metadata, experimental and computational workflows, and a materials ontology to maximize interoperability and reproducibility of materials data processing. To this end, data use profiles of participant projects from different sub-disciplines are analyzed to identify the most relevant scientific scenarios within MatWerk.
Similarly, the Plattform MaterialDigital (PMD) is committed to provide a prototypical infrastructure for the digitalization of materials in an industrial context implemented by decentralized data servers, semantic data schemas and digital workflows. The standards, methods, and tools developed within the PMD are deployed and consolidated within the context of currently more than 20 BMBF-funded academic and industrial research consortia. Scientific workflow environments represent a major focus area, including efforts to improve the definition and representation of digital workflows, as well as their distribution in form of a workflow store.
In this presentation we will describe the overarching visions behind these initiatives, their status, and progress of dissemination with a focus on the workflow activities and the connection to machine learning applications. Following the philosophy of both consortia, specific examples will be used to demonstrate innovative and pragmatic solutions.
Thermodynamic bulk phase diagrams have become the roadmap used by researchers to identify alloy compositions and process conditions that result in novel materials with tailored microstructures. On the other hand, recent progress in experimental atomic-scale characterization techniques allows one to study the local chemical composition at individual defects such as interfaces, grain boundaries, dislocations and surfaces. They show that changes in the alloy composition can drive not only transitions in the bulk phases present in a material, but also in the concentration and type of defects they contain. Defect phase diagrams, using chemical potentials as thermodynamics variables, provide a natural route to study these chemically driven defects. Our results show, however, that the direct application of thermodynamic approaches can fail to reproduce the experimentally observed defect formation.
Therefore, we extend the concept to metastable defect phase diagrams to account for kinetic limitations that prevent the system from reaching equilibrium. We use ab initio calculations based on density functional theory to quantify the extension of regions where defect formation is expected. We successfully applied this concept to explain the formation of large concentrations of planar defects in supersaturated Fe2Nb Laves phases. In addition, we identify in a joint study with experiments conditions and structures in Mg-Al-Ca alloys for defect phase occurrence. The concept offers new avenues for designing materials with tailored defect structures.
Überblick über die derzeitig wichtigsten additiven Fertigungsverfahren für metallische Werkstoffe in der Industrie (PBF, DED, BJT) und Berücksichtigung der wesentlichen Prozessmerkmale und Nachbearbeitungsschritte. Vorstellung der wichtigsten Defektphänomene und Nennung von Ursachen und Abhilfemaßnahmen.
Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis
(2023)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the identification and launching corresponding VAMAS projects. The ongoing project "FIB sample processing for TEM" is presented in detail.
Regional standardisation activities and how VAMAS can help in any way to promote activities are reported.
Activities related to organisational updates, government initiatives/priorities (especially related to Materials), details of any strategy documents publicly available, networks within Germany and how we engage are presented.
Newly developed methodical approaches with an emphasis on correlative imaging analysis of morphology and chemistry of nanomaterials will be presented. Correlative imaging by high-resolution SEM with STEM-in-SEM as well as with EDS, and further with AFM, or with the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and as embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for the local surface chemistry will be highlighted. Examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy and the highest surface-sensitive methods XPS and ToF-SIMS as advanced surface characterization methods available in the Competence Centre nano@BAM will be showed. Particularly for the spatially resolved analysis of the chemistry of nanostructures, such in-depth and lateral gradients of chemistry within mesoporous thin layers, or the completeness of the shells of core-shell nanoparticles, the latter methods are inherent.
Other dedicated developments like approaches for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM or the quantitative determination of the roughness of particle surface by high-resolution imaging with electron microscopy will be also presented.
Liaison of ISO/TC 202 Microbeam Analysis with VAMAS/TWA 37 Quantitative Microstructural Analysis
(2023)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the identification and launching corresponding VAMAS projects. The ongoing project "FIB sample processing for TEM" is presented in detail.
The basic principles of generation of electrons and X-rays and the operation of SEM/EDS instruments are presented. Examples, recent successes and challenges in the analysis of nano-structures are given. Multi-method analytical approaches with the focus on imaging the nanoscale are highlighted. Details on the sample preparation and persepective on the automated analysis (sample preparation, measurement, data analyis and storage) are given. Metrological aspects, standardisation, and reference materials are also emphasized by examples.
An overview on the VAMAS technical working areas (TWA) and projects where Germany is active has been given. The role of VAMAS as an international pre-standardisation platform, including its intense collaboration with international bodies ISO, CEN, OECD and CCQM and national organizations like DIN has been highlighted.
(Pre)Standardisation and Metrology in Microbeam Analysis – Ongoing Activities and Opportunities
(2023)
The presentation addresses the current ongoing projects as well as the gaps and opportunities in microbeam analysis within ISO/TC 202 Microbeam Analysis standardisation body and in-liaison Technical Working Areas (TWAs) at the pre-standardization platform of VAMAS (Versailles Project on Advanced Materials and Standards).
Following points are presented and discussed: i) nPSize as an EMPIR project on the nanoparticle size and shape distribution of (more) complex particles including sample preparation and machine learning approaches; ii) parallel development of ISO 21363 (PSSD by TEM), ISO 19749 (PSSD by SEM), ISO 22292 (3D TEM), ISO 52408 (NP Prep for AFM and EM), iii) VAMAS and pre-standardisation, TWA 34 „Nanoparticle Populations“ with two nPSize ILC projects P15 & P16 – results to be published and integrated in ISO 21363 (PSSD by TEM); iv) Remaining challenges: platelets, 2D materials (TiO2 and GR2M); v) Reference data sets as part of a complete Characterisation Workflow.
Die Bestimmung der Nanopartikelgrößen- und -formverteilung nach OECD TG 125 mit der Transmission and Scanning Electron Microscopy (SEM/TEM) wird punktuell vorgestellt:
- Generelles Messprinzip
- Beispiele
- Korrelative Mikroskopie
- Welchen Durchmesser misst die Methode?
- Welche Partikel kann diese Methode messen?
- Welche Informationen kann diese Methode liefern?
- Wo stößt die Methode an ihre Grenzen?
- Implementierung und Datenauswertung,
- Reporting.
Anschließend wurde eine Q&A-Session für die Imaging-Methoden organisiert.
The VAMAS/TWA 45 Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods” involving 85 participants around the world is primarily discussed with respect to the results received and a first data evaluation. Status of the Project "Guidelines for defining reference materials for plastic degradation in marine environment" is reported and two new project proposals are presented: "Development of standardized methodologies for characterisation of nanoplastics (starting soon, BAM as leader?) and "Development of analytical protocols for the identification and quantification of microplastics of fibrous shape (still in negotiation)".
The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are highlighted. The implementation of the results into the corresponding ISO technical specification AWI/TS 23879 is also discussed and planned, in relation with the AFM part.
Accurate characterisation of the morphology (size) and chemistry of graphene-related 2D materials (GR2M) is key in understanding their extraordinary functionalities. Hence, not only the tailoring of these functionalities aiming at applications of increased-performance becomes possible, but also the correlation of the physico-chemical properties with the understanding of the potential toxicity eventually enables a safe and sustainable development of the GR2M for new applications. Whilst AFM and Raman Spectroscopy are recommended to measure the thickness of GO flakes, Scanning Electron Microscopy (SEM) is the most suited method to assess their lateral size, which varies between tens of µm down to below 100 nm. In this paper, procedures for the accurate determination of lateral size of graphene oxide (GO) flakes by SEM are presented. The prerequisite for accurate flake size analysis is the proper sample preparation, i.e. deposition of ideally isolated flakes on a substrate, with the flakes being unfolded, non-overlapped, parallel with the substrate, and having a high coverage density. Examples of optimum image caption conditions and image analysis procedures will be presented. The size descriptors and their measurement are described in the context of the corresponding analysis approach: i) length and width of the flakes with a quick and rough, but robust procedure, and ii) exact contouring of the flakes as part of a highly accurate, but more time-consuming measurement approach. The possibility of application of automated image analysis is discussed as the alternative to the manual flakes analysis.
Das EU Projekt EU FireStat SI2.830108, das vom Europäischen Parlament finanziert und von der DG GROW der Europäischen Kommission in Auftrag gegeben wurde, hat aufgearbeitet, welche Terminologie in den europäische Mitgliedsstaaten verwendet wird und die von den Mitgliedstaaten erhobenen Daten über Gebäudebrände zu analysieren. Dabei wurden die Schwierigkeiten bei der Erfassung und die Unterschiede bei der Auslegung ermittelt und eine gemeinsame Terminologie sowie eine Methode zur Erfassung der erforderlichen Daten vorgeschlagen.
Folgende Schwerpunkte wurden bearbeitet: Zunächst erfolgte eine Diagnose von Terminologie-, Datenerhebungs- und Auslegungsproblemen, Erhebung der Terminologie und der Datenerfassung, Identifizierung der für die Entscheidungsfindung benötigten Daten, Analyse der Methoden zur Datenerhebung Definition einer gemeinsamen Terminologie, Methodik der Kosten-/Nutzenbewertung zur Unterstützung politischer Entscheidungen, Fallstudie zur Anwendung der Methode der Kosten-/Nutzenbewertung, Beschreibung einer zukünftigen Datenerhebungsmethode.
Das Ergebnis des Projekts ist eine Empfehlung, welche Daten in den Mitgliedstaaten erhoben werden sollten, um wissensbasierte Entscheidungen in Bezug auf den Brandschutz zu ermöglichen. Damit wird die Grundlage für Maßnahmen und Initiativen geschaffen, die den Brandschutz und die Brandverhütung der Mitgliedstaaten unterstützen, so dass knappe Ressourcen gezielt eingesetzt werden können.
Germany has concluded energy partnerships with various countries, including Japan. During the 3rd meeting of the Hydrogen Working Group, the strategic approach of both countries on developments of hydrogen guidelines, certification and safety was presented and discussed. BAM gave a presentation on important topics in the field of safety research and on safety-related issues along the value chain. Furthermore, the work program and selected projects of the competence center H2Safety@BAM were presented.
A safe supply of energy is a fundamental prerequisite for modern industrial societies. The extent to which the energy turnaround is being shaped in Germany in terms of, for example, energy policy, promotion, but also social development was discussed during the 12th Wildau Science Week. BAM contributed to the topic of safety of energy sources and presented the competence center H2Safety@BAM.
The Gases Advisory Group is organized regularly by the Prevention Division of the German Employer's Liability Insurance Association for Raw Materials and the Chemical Industry. The event serves as an exchange between science and industry on current safety-related issues concerning oxygen and hydrogen. In this context, BAM presented an overview of its various activities of the competence center H2Safety@BAM, which are reflected in the entire hydrogen value chain. In addition, the plans for the expansion of the test infrastructure at BAM's Technical Safety Test Site were presented. The results of the DELFIN project on the safety of pressurized gas storage tanks, the release tests of liquid hydrogen as well as the underfiring of corresponding cryogenic storage tanks and the plans for the ModuH2Pipe@BAM project were also presented. The presentation concluded with the current recommendations of the Hydrogen Research Network.
Hydrogen is a central component of the energy transition and the European Green Deal for a climate-neutral Europe. To be able to achieve the targets defined by 2045, the EU and the German government have drafted a framework for action and are making long-term investments in research, development and the rapid implementation of innovative hydrogen technologies.
The conditions for a successful energy transition and the economic use of green hydrogen as a clean energy carrier are Hydrogen readiness and a rapid market ramp-up, as well as the establishment of the necessary value chains in the national and European framework. Reliable quality and safety standards are the prerequisite for ensuring safety of supply and environmental compatibility and for creating trust in these technologies.
BAM has bundled its expertise in the field of hydrogen technologies into a competence center H2Safety@BAM to create confidence in the technology and to support the hydrogen strategies of the German government and the EU. The topic of hydrogen has been current at BAM for more than one hundred years and is also currently the focus of numerous research and cooperation activities. The competence centre H2Safety@BAM and its vision of “We build trust in hydrogen technologies” will be presented with its many safety-related topics, which can be found throughout the entire hydrogen value chain. Two deep dives will present the results on projects dealing with the design-to-cost issue of classical pressurized gas storage containments and the consequences of the release of liquid hydrogen, which will be roughly compared to the release of ammonia.
Um die Energiewende voranzubringen, wird neben dem Ausbau der Erneuerbaren Energien ein schneller Markthochlauf bei Wasserstoff-Erzeugung, Transport und Anwendung angestrebt. Dieser Markthochlauf geht derzeit insbesondere einher mit Fragen der Wirtschaftlichkeit und der Umsetzung einer Serienfertigung von Elektrolyseuren. Bei Fragen der Sicherheit wird üblicherweise auf das bestehende Regelwerk verwiesen. Da der Umgang mit Wasserstoff und die Technologien zur Wasserstoff- Erzeugung nicht neu sind, geht man davon aus, dass durch die Einhaltung der bestehenden Regelwerke die Anlagen ausreichend sicher sind. Aber ist das wirklich so? Decken die bestehenden technischen Regelwerke alle derzeitigen Entwicklungen im Zusammenhang mit der Wasserstofferzeugung und -nutzung in allen notwendigen Facetten ab, um die Sicherheit zu gewährleisten? Der Experten-Workshop soll die Möglichkeit bieten, sich über die Sicherheit bei Wasserstofferzeugung und -nutzung auszutauschen sowie offene Fragestellungen und Lücken im Regelwerk zu identifizieren. Hierzu sind sowohl Impulsvorträge als auch ein offener Austausch mit allen Teilnehmenden geplant.
Ammonia Safety
(2023)
In order to share the latest technological information in the gas field and develop the gas industry, the Korean Gas Safety Corporation host an international gas safety seminar every year by inviting domestic and foreign experts. In year 2023, the seminar focussed on the latest trends in ammonia safety management and utilization technology. BAM was asked to give a presentation on ammonia safety and its flammability in specific. Based on the international flammability classification the required explosion protection measures were presented,which are defined by the European ATEX rules. As final part of the presentation the German strategy on transformation of existing infrastructure, here especially the transformation of landbased LNG terminals, was shown as well.
Ammonia Safety
(2023)
Ammonia is an energy source that has been produced and used on a large scale for many decades, primarily as a fertilizer or feedstock in nitrogen chemistry. The CAMPFIRE alliance, founded as part of the "WIR!- Wandel durch Innovation in der Region" funding program of the German Federal Ministry of Education and Research (BMBF), aims to research and develop new energy conversion and storage technologies for the future energy system based on green ammonia. The safe handling of ammonia is an important issue along the entire value chain. Therefore, the alliance has organized a webinar to discuss the topic of ammonia safety and in particular its flammability. BAM's contribution presented the topic of flammability in detail, placed the classification of ammonia in an international, European and national context and presented the basic principles of explosion protection that result from this and must be observed during use and application.