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- nein (19855)
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- Korrosion (248)
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Organisationseinheit der BAM
- 8 Zerstörungsfreie Prüfung (911)
- 6 Materialchemie (829)
- 7 Bauwerkssicherheit (811)
- 9 Komponentensicherheit (724)
- 1 Analytische Chemie; Referenzmaterialien (578)
- 4 Material und Umwelt (435)
- 5 Werkstofftechnik (430)
- 3 Gefahrgutumschließungen; Energiespeicher (413)
- 7.6 Korrosion und Korrosionsschutz (350)
- 9.4 Integrität von Schweißverbindungen (342)
In the late 1980s, a new type of corrosion appeared in drinking water installations where galvanized steel pipes failed forming a deep groove with no corrosion at the other surfaces. The reason was discussed quite fiercely between failure analysts and material suppliers. In the end the discussion lead to the solution: inductive welded pipes of a certain sulphur content were prone to selective corrosion. The history of the arguments is discussed using old communications between Wilhelm Schwenk and Wolfgang Stichel, who later published the results in a paper unfortunately only I german.
Thus the knowledge got lost and new cases based on the same material problems are observed in application of so-called C-Steel piping systems. Failure cases are shown.
Die Umstellung der Wirtschaft auf wasserstoffbasierte Energieversorgung soll in Deutschland vor allem auf Basis der Umstellung des bestehenden Erdgasnetzes erfolgen. Dabei sollen ca. 90 % dieser Fernleitungsnetze auf dem bestehenden Erdgasnetz basieren. Die Beimischung von Wasserstoff zum Erdgas als auch der reine Wasserstofftransport werfen jedoch die Frage auf, ob und wie kompatibel die eingesetzten Materialien sind. Die Reparatur- und Erweiterungsfähigkeit von Erdgas-Bestandspipelines ist zu klären, wenn diese auf Wasserstoff umgestellt werden. Denn gerade Gashochdruckleitungen müssen regelmäßig gewartet und erweitert werden, um einen ordnungsgemäßen Betrieb sicherzustellen. Insbesondere das Schweißen unter Betriebsdruck bzw. an in Betrieb befindlichen Gasleitungen ist eine der wichtigsten Instandhaltungstechnologien, unabhängig von der Zusammensetzung des geförderten Mediums. Es ist daher dringend notwendig, eine geeignete Teststrategie zu erarbeiten, welche die nötigen Vorrausetzungen für sicheres Schweißen an in Betrieb befindlichen Druckwasserstoffleitungen schafft und entsprechende Kriterien für die Praxis liefert. Im Projekt H2-SuD - Einfluss des Schweißens auf die Wasserstoffaufnahme und Degradation im Betrieb befindlicher H2-Ferngasleitungen - soll geklärt werden, ob und wie stark mit einer Eigenschaftsdegradation geschweißter Rohrstähle in Gasnetzen in Folge einer Wasserstoffaufnahme zu rechnen ist. Die Präsentation gibt dazu einen kurzen Überblick über den aktuellen Status des Projektes. Die Förderung erfolgt im Rahmen der DVGW-Innovationsprogammes Wasserstoff (Nr. G 202131).
"Hausbock, Holzwurm und Kompanie - Wissen wir wirklich schon Alles über die üblichen Verdächtigen"
(2014)
Die Verwendung pyrotechnischer Gegenstände in Menschenmengen (u. a. in Fußballstadien) hat in den letzten Jahren stark zugenommen. Zur Verwendung gelangen vorrangig sonstige pyrotechnische Gegenstände der Kategorie P1. Diese Gegenstände sind frei verkäuflich für Personen ab einem Alter von 18 Jahren. Am häufigsten werden pyrotechnische Gegenstände verwendet, die Rauch und Licht in verschiedenen Farben erzeugen.
Analytical Sciences has developed from Ostwald’s “unentbehrlichen Dienstmagd” to a chemical discipline at the core of many of today’s fundamental and applied scientific problems and innovations. An atomic or molecular understanding of basic processes in chemistry, soft matter physics, materials and life science is enabled only through new analytical methods and instrumentation. Similar observations can be found for pressing sociopolitical conflicts of the future: A rational discussion of global climate change or new energy sources is only possible with reliable analytical results. Progress in Analytical Sciences is only possible if the underlying interdisciplinary character is acknowledged and valued. The talk will illustrate the scope of modern Analytical Science through examples from process analysis relevant to modern process intensification and industry 4.0 to bioanalysis and the use of synchrotron radiation to elucidate fundamental reactions materials.
Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in welded joints using a thermal conductivity device (TCD) for quantitative measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries and factors that additionally influence hydrogen determination. They are namely: specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PID-furnace controller as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up the reach the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by evaluation of the recorded data. Generally, independent temperature measurement with calibration specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA).
"Online"-Aushärtungskontrolle bei der Verarbeitung von vernetzenden Kunststoffen mit Ultraschall
(2004)
We report on the development of ultra-small core-shell silver nanoparticles synthesized by an up-scaled modification of the polyol process. It is foreseen to use these thoroughly characterized particles as reference material to compare the catalytic and biological properties of functionalized silver nanoparticles. Small-angle X-ray scattering (SAXS) analysis reveal a narrow size distribution of the silver cores with a mean radius of RC = 3.0 nm and a distribution width of 0.6 nm. Dynamic light scattering (DLS) provides a hydrodynamic radius of RH = 10.0 nm and a PDI of 0.09. The particles’ surface is covered with poly(acrylic acid) (PAA) forming a shell with a thickness of 7.0 nm, which provides colloidal stability lasting for more than six months at ambient conditions. The PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione (GSH) and bovine serum albumin (BSA) have been performed as examples. We demonstrate that the particles effectively catalyze the reduction of 4-nitrophenol to 4-aminophenol with sodium borohydride. The tunable catalytic activity of (436 ± 24) L g-1 s-1 is the highest reported in literature for silver nanoparticles.
(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).
Die Präsentation ist der Startschuss für die Wasserstoffkolloquien der BAM. Sie beginnt mit Adolf Martens und zeigt den Weg vom Foresight-Prozess Wasserstoff bis zum Kompetenzzentrum H2Safety@BAM. Es werden die Kompetenzfelder vorgestellt und die handelnden Personen. Dies leitet über zu den drei Vorträgen des Tages und den Vortragenden.
The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed.
In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies!
Tribological profile of hydraulic oils by using SRV. The determination of a set of critical, tribological by using different SRV-based test methods. The SRV-based concept of tribological profile generates the wear volumes on two triboelements (specimen), the extreme pressure properties and friction under different contact pressures.
Thus, the benchmark and validation of hydraulic oils bear on a wider range of tribological properties.
The RR2016 extends with six hydraulic oils to other base oil types including biodegradable fluids, which were all tested according to ASTM D7043 in order to consolidate the correlation between SRV and V104C.
2015 Tianjin explosions
(2016)
In 2015 a series of explosions occurred at a container storage station at the Port of Tianjin, China, on Wednesday, 12 August 2015, that killed over one hundred people and injured hundreds of firemen and others. The first two explosions happened within 30 seconds of each other at the facility. The second explosion was larger and involved the detonation of about 800 tons of ammonium nitrate. The cause of the explosions was not known at first, but an investigation of the Chinese authorities concluded in February 2016 that an overheated container of dry nitrocellulose was the cause of the initial explosion. Colleagues of the Nanjing University of Science and Technology and BAM worked together to analyze the reasons and the process of that incident based on knowledge about the properties of the involved substances, particularly ammonium nitrate and nitrocellulose, and potential mechanism of initiation and propagation.
2015 Tianjin Explosions
(2016)
In 2015 a series of explosions occurred at a container storage station at the Port of Tianjin, China, on Wednesday, 12 August 2015, that killed over one hundred people and injured hundreds of firemen and others. The first two explosions happened within 30 seconds of each other at the facility. The second explosion was larger and involved the detonation of about 800 tons of ammonium nitrate. The cause of the explosions was not known at first, but an investigation of the Chinese authorities concluded in February 2016 that an overheated container of dry nitrocellulose was the cause of the initial explosion. Colleagues of the Nanjing University of Science and Technology and BAM worked together to analyze the reasons and the process of that incident based on knowledge about the properties of the involved substances, particularly ammonium nitrate and nitrocellulose, and potential mechanism of initiation and propagation.
Actions from the meeting in April 2016: 1. Four SAC test methods are in place and were revised: SH/T 0721 (Grease, coefficient of friction and wear), SH/T 0784 (Grease, pass load/O.K. load), SH/T 0847 (Oil, coefficient of friction and wear) and SH/T 0882 released by 11-2014 (Oil, pass load/O.K. load). 2. New test method to evaluate anti-fretting properties of greases based was approved by SAC TC280 and will be released. 3. SAC TC280 accepted the project “Simulation of synchronizer by using SRV”. Draft text to be submitted by 03-2017. Discussions on a parallel ASTM test method. 4. A procedure for “Wear Volume” is under development for SAC TC280.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
In civil engineering the information about the quantitative ingress of harmful species like Cl⁻, Na⁺ and SO²⁻₄ is of great interest to evaluate the remaining life time of structures. These species are triggering different damage processes like the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. For the evaluation of the heterogeneous concrete it is necessary to discriminate between the different phases mainly cement matrix and aggregates. The transport processes are only proceeding in the cement matrix therefore the measured concentrations should be regarded to the cement content. For the 2D evaluation of element distributions different multivariate cluster-algorithms like k-means and Expectation-Maximization-algorithm (EM-algorithm) have been tested. The methods are compared and different figures of merit will be presented. After phase separation non-relevant information of the aggregates can be excluded. The ingress of harmful species is then quantified using chemometrics. Due to concrete cores from a parking deck the methods have been validated and verified with standard methods of wet-chemistry.
Thermographic super resolution techniques allow the spatial resolution of defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. In this work, we re-port on the extension of this approach towards a full frame 2D super resolution technique. The approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample.
The slip-rolling 2Disk tribometer from Optimol Instruments represented the technological evolution in tribotesting of the well-known AMSLER-type tribometer marketed in 1922. Both use two discs with the same outer diameter rolling against each other on their circumference. In the AMSLER, the lower disc dips into an oil reservoir, whereas in the 2Disk the oil is injected into the contact. The oil supply of the 2Disk is controlled by pump and temperature by a heat exchanger.
2PM FlySCAN: Innovative approach for wide field high resolution imaging of skin tissue volumes
(2016)
Two Photon Microscopy (2PM) is an innovative Technology for high resolution imaging of human skin in vivo and ex vivo. Up to now the method is limited by its interdependence between the field of view and the attainable resolution. The new FlySCAN Technology overcomes these boundaries and enable images sizes of many millimeters by resolutions in the submicrometer range revealing very specific information on clinically and biologically relevant tissue and cell structures. The advantages of the new approach are demonstrated by excellent in vivo and ex vivo tissue images.
Das DVS-Vorhaben 01.3211 „Herstellung beanspruchungsgerechter Oberflächen durch Kombination innovativer additiver und abtragender Fertigungsschritte an hochbelasteten Komponenten“ ist ein Kooperationsprojekt der Bundesanstalt für Materialforschung und -prüfung (BAM) und dem Institut für Schweißtechnik und Trennende Fertigungsverfahren (ISAF) der Technischen Universität Clausthal. Das Übergeordnete Projektziel ist das Erlangen von Erkenntnissen für eine sichere und wirtschaftliche, kombinierte additive und abtragende Fertigung aus kostenintensiven Werkstoffen hochbelasteter Komponenten insbesondere für KMU. Dabei stehe die beiden Werkstoffe CoCr26Ni9Mo5W (2.4681) und FeNi36 (1.3912) im Fokus. Mittels Modifikation der Schweißzusätze sind homogen und isotrop ausgeprägte Werkstoffeigenschaften und eine Erhöhung der Prozessstabilität und Fertigungsfreiheitsgrade bei der additiven Fertigung erzielbar. Darüber hinaus wird der Einfluss nachfolgender abtragender Bearbeitungsschritte des ultraschallunterstützen und des konventionellen Fräsprozesses untersucht. Im Laufe der Sitzung des projektbegleitenden Ausschusses (PbA) wurde der aktuelle Bearbeitungsstand sowie der Zeitplan vorgestellt. Darüber hinaus wurde mit dem PbA über die bereits erzielten Ergebnisse diskutiert. Abschließend wurde ein kurzer Ausblick über die zeitnah beginnenden Arbeiten beider Forschungseinrichtungen sowie ein Überblick über die vorhabenbezogenen Aufwendungen der Wirtschaft und des Ergebnistransfers in die Wirtschaft gegeben.
Structure elucidation of complex synthetic copolymers still represents a challenge. A one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Is the coupling of liquid chromatographic separation techniques to mass spectrometry able to fill the gaps to a certain degree?
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases, CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
The lecture will provide a series of examples where LC-MS has been applied to evaluate complex macromolecules and mixtures of these.
On- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed.
Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of complex structures. The quality of the feedstock material receives increasing attention, as it depicts the first part of the L-PBF process chain. The powder quality control in terms of flowability and powder bed packing density is therefore mandatory.
In this work, a workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape for three different powder batches. The polydisperse particle size distribution (PSD) was transformed into a statistically equivalent bidisperse PSD. The ratio of the small and large particles helped to understand the powder particle packing density. While the particle shape had a neglectable influence, the particle size distribution was identified as major contributor for the packing density.
3D Charakterisierung wasserstoffunterstüzter Risse in Stahl mittels Synchrotron-Refraktions-CT
(2016)
Die Fehlertoleranz moderner hochfester Stähle gegenüber Prozessfehlern beim Fügen nimmt stetig ab und erfordert eine immer kritischere Beurteilung der Ergebnisse aus den vorhandenen Prüfverfahren. Deren Aussagekraft ist häufig zu gering und daher muss zum einen das wissenschaftliche Verständnis der Mikrokaltriss-Entstehung in diesen Stählen vertieft werden und zum anderen müssen die Prüfmethoden und Bewertungskriterien angepasst werden. Dies erfordert ein besseres Verständnis insbesondere der Kopplung von Eigenspannungen, Wasserstoffgehalten und der Wirkung äußerer Kräfte auf die Rissentstehung und das Risswachstum.
Erstmals soll mittels 3D-Synchrotron-Refraktions-Topographie an der BAMline am BESSY die Rissentstehung in mit Wasserstoff beladenen Zugproben charakterisiert werden. Diese Kenntnisse sollen in weiteren Untersuchungen auf Schweißnähte übertragen werden.
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, leading to potential efficiency and performance improvements. However, the rapid cooling rates associated with the process consequently leads to the generation of high magnitude residual stresses (RS). Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterization of these RS is essential for safety related engineering application and supporting the development of reliable numerical models. Diffraction-based methods for RS analysis using high energy synchrotron X-rays and neutrons enable non-destructive spatially resolved characterization of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research conducted by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys. Special focus will be given to the challenges posed by textured LPBF materials for the reliable choice of the diffraction elastic constants (DECs), which is crucial to the accurate calculation of the level of RS.
The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning.
Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures.