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Eingeladener Vortrag
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Mass spectrometric Methods MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming.
Optical spectrometric methods are proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry (LAMIS). First, stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated heteronuclear diatomic molecules (MH or MX) in graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. Finally, the application of molecular spectrometry via emission by LAMIS is compared and discussed.
Die vom BMBF unterstütze Forschungsinitiative BonaRes entwickelt Strategien um Boden als nachhaltige Ressource für die Bioökonomie zu nutzen. Das Projekt Intelligence for Soil (I4S) ist ein Teil dieser Initiative und beschäftigt sich mit der Entwicklung eines integrierten Systems zur ortsspezifischen Düngung. Ein Ziel dieses Projektes ist die Etablierung einer mobilen Sensorplattform zur Bodenkartierung. Aufgabe der BAM ist dabei das Installieren und die Optimierung eines RFA Sensors für die online Messung direkt auf dem Feld. Die RFA ist eine zerstörungsfreie Technik, die kaum Probenvorbereitung benötigt und einen schnelle Multielement Analyse ermöglicht. Das schnelle Kartieren des Bodens ermöglicht später eine ortsspezifische Düngung mit Nährstoffen wie z.B. K, Ca und P.
Die vom BMBF unterstütze Forschungsinitiative BonaRes entwickelt Strategien um Boden als nachhaltige Ressource für die Bioökonomie zu nutzen. Das Projekt Intelligence for Soil (I4S) ist ein Teil dieser Initiative und beschäftigt sich mit der Entwicklung eines integrierten Systems zur ortsspezifischen Düngung. Ein Ziel dieses Projektes ist die Etablierung einer mobilen Sensorplattform zur Bodenkartierung. Aufgabe der BAM ist dabei das Installieren und die Optimierung eines RFA Sensors für die online Messung direkt auf dem Feld. Die RFA ist eine zerstörungsfreie Technik, die kaum Probenvorbereitung benötigt und einen schnelle Multielement Analyse ermöglicht. Das schnelle Kartieren des Bodens ermöglicht später eine ortsspezifische Düngung mit Nährstoffen wie z.B. K, Ca und P.
The use of artificial neural networks (ANNs) is demonstrated for efficient real-time data processing in optical fiber sensing applications. Using ANN-based algorithms, two orders of magnitude improved computation time and improved measurement resolution is achieved for distributed strain sensing using the wavelength-scanning coherent optical time domain reflectometry technique.
The distributed measurement of relative humidity is a sought-after capability for a wide range of applications in civil engineering and structural health monitoring. We show that polymethyl methacrylate (PMMA) optical fi-bers can be employed as a sensor medium to conduct distributed humidity measurement by analyzing Rayleigh backscattering traces obtained by OTDR. We make use of the effect that water penetrates the fiber core and directly influences the local fiber attenuation and Rayleigh backscatter coefficient. We conducted distributed backscattering analysis for two different pulse wavelengths: 500 nm and 650 nm. The 650 nm results are susceptible to both, attenuation changes and backscatter changes, whereas backscatter results at 500 nm are not affected by humidity-induced attenuation and only exhibit a change of Rayleigh backscattered power as a function of humidity. The combined measurement and analysis of both parameters at these two wavelengths has the advantage that cross-sensitivities on backscatter change and attenuation, such as strain and tempera-ture changes, could be separated from the humidity response of the fiber. We present laboratory results for a humidity range between 30% and 90% for both pulse wavelengths: including step responses, humidity cycles and hysteresis analysis. In addition to the attenuation and backscatter coefficient dependence, we also analyze optical runtime changes as a function of humidity. POFs have the advantage that they can be directly embed-ded into materials such as concrete or soil to measure water content or localize water ingress. Standard step-index PMMA POFs can be used as a distributed relative humidity sensor up to 200 m distance.
We present our research on the development of a Brillouin optical frequency-domain analysis (BOFDA) using a perfluorinated graded-index polymer optical fiber (PFGI-POF) as a sensing fiber. The described works include investigations both on the selection of the setup components with respect to mode coupling effects and on the impact of the humidity cross-sensitivity. The suitability of the developed POF-based BOFDA is proved by a distributed measurement on an 86 m long PFGI-POF recorded with the spatial resolution of 6 m.
Polytetrafluorethylen (PTFE) ist ein Hochleistungskunststoff, der sich aufgrund seiner einzigartigen Eigenschaften als unverzichtbarer Werkstoff in der modernen Industriegesellschaft etabliert hat. PTFE, modifiziertes PTFE und PTFE-Compounds kommen bevorzugt bei systemtechnischen Lösungen im Umfeld komplexer Regelwerke mit hohen Kompatibilitäts- bzw. regulativen Anforderungen, z.B. im Sauerstoff-, Lebensmittel- bzw. Trinkwasserkontakt, zur Anwendung. Beim Einsatz in Sauerstoffanlagen sollten Verarbeiter eine Reihe von Hinweisen beachten.
Wir laden zum Trainingsworkshop Datenanalyse ein. Angetrieben durch die Digitalisierung und die sogenannte Industrie 4.0 steigt die Erwartungshaltung gegenüber der Nutzung von Daten. Die Unsicherheit, Widersprüchlichkeit und Redundanz separat verarbeiteter einzelner Quellen soll durch die synergetische Zusammenführung heterogener Datensätze überwunden werden. Dabei steht der zunehmenden Aufgabenkomplexität eine ebenso zunehmende Verfügbarkeit an Daten und Analyseverfahren gegenüber.
Der Workshop vermittelt ein konzeptionelles Verständnis für moderne Datenanalyseverfahren (Machine Learning (ML), Multivariate Statistik) und soll durch ein anschließendes Hands-On Training mit Python (https://www.python.org) einen einfachen Einstieg in die Thematik ermöglichen. Der Kurs richtet sich an den wissenschaftlichen Nachwuchs.
Die herkömmliche Bildgebung mit Röntgenstrahlung beruht auf unterschiedlicher Absorption durch verschiedene Materialien im Volumen eines Körpers. Es entsteht ein "Massebild". Die hier vorgestellten Verfahren benutzen die Brechung und Beugung von Röntgenstrahlen, um innere Oberflächen oder die Molekulartextur von Materialien und Bauteilen abzubilden. Im Vortrag werden die entsprechenden Messtechniken an der BAM im Labormaßstab sowie an Großforschungseinrichtungen vorgestellt und anhand einiger Anwendungsbeispiele die zusätzlichen Informationen zur herkömmlichen Durchstrahlung diskutiert.
Degradation of thermal barrier coatings (TBCs) in gas‐turbine engines due to calcium–magnesium–aluminosilicate (CMAS) glassy deposits from various sources has been a persistent issue since many years. In this study, state of the art electron microscopy was correlated with X‐ray refraction techniques to elucidate the intrusion of CMAS into the porous structure of atmospheric plasma sprayed (APS) TBCs and the formation and growth of cracks under thermal cycling in a burner rig. Results indicate that the sparse nature of the infiltration as well as kinetics in the burner rig are majorly influenced by the wetting behavior of the CMAS. Despite the obvious attack of CMAS on grain boundaries, the interaction of yttria‐stabilized zirconia (YSZ) with intruded CMAS has no immediate impact on structure and density of internal surfaces. At a later stage the formation of horizontal cracks is observed in a wider zone of the TBC layer.
Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds.
Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications.
In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals.
Biocide mitigation strategies of microbiologically influenced corrosion (MIC) in the oil and gas industry have been primarily used to eliminate the growths of sulfate-reducing microorganisms (SRM). However, methanogenic Archaea (MA) can also be highly corrosive by using iron as an electron source for methanogenesis. Because of the fundamental physiological differences between archaea and bacteria, responses of MA towards SRM-specific biocides cannot be deduced using SRM. Due to the lack of information available on the effect of biocides on corrosive MA, we selected THPS, glutaraldehyde, nitrate and perchlorate to compare against corrosive SRM.
Preliminary results showed that at low concentrations of THPS (0-10 ppm), growth of MA was not affected, methane production and corrosion rates (0.1 mm/yr) were comparable between the different THPS concentrations. On the contrary, the SRM strain showed decreased corrosion rates (0.18 mm/yr to 0.03 mm/yr) with increasing THPS concentrations. Further corrosion tests including electrochemical measurements of different biocides on the growth of MA and SRM will be conducted. Such knowledge not only provide important insights on the physiological response of MA to biocides but also contribute to more effective mitigation strategies that can be both economic and environmentally beneficial.
Composite pressure vessels for transporting dangerous goods and for hydrogen and natural gas vehicles consist of a load-bearing composite and a gas-tight, metallic or polymeric barrier layer (liner). To investigate the aging behavior of such composite pressure vessels, BAM carried out the interdisciplinary project COD-AGE. The aim of the project was the development of methods and models for the description and determination of the aging behavior of carbon fiber composites using the example of pressure vessels in order to better predict aging and safe working life. One focus of this project was the provision of suitable NDT methods. These included both test-related tests and the possible development of test equipment for later practical use.
In the lecture, test results of the age-related eddy current test on composite pressure vessels are presented.
In aging tests, pressure vessels made of an approximately 4 mm thick aluminum liner and approx. 8 mm thick CFRP layer were examined. Typical application of such pressure vessels are respiratory protective devices of the fire department. The pressure vessels were tested using conventional eddy current technology from the outer and inner side as well as with high-frequency eddy current technology. Both damage to the metallic liner and structures of the CFRP could be detected. A particular mechanical challenge was the inspection of the inside of the liners, since a cylindrical surface with an inside diameter of 150 mm has to be tested with an access of only 15 mm diameter.
Multiple sclerosis (MS) is the most common acquired neurological disease affecting Young adults. It leads to myelin destruction and formation of lesions in the brain and permeabilization of the blood-brain barrier (BBB).
Gadolinium based contrast agents (GBCA), used for diagnosis and monitoring by MRI, might accumulate in tissue, including brain. Using an animal model, application of linear and macrocyclic GBCA was investigated. Analysis was performed by laser ablation inductively coupled plasma (LA-ICP) MS. This method works as a bioimaging tool for sample thin sections and allows to identify regions of accumulated Gd in the samples.
In healthy and diseased mice, inflammationmediated changes in the brain were investigated by application of GBCA. The mean objective is to understand the changes in inflamed tissue and correlate alterations of the BBB by LA-ICP-MS (Imaging Mass Cytometry).
Mg is a very promising material for lightweight construction and biomedical applications. However, the applicability of Mg and its alloys is hindered by its high corrosion susceptibility. Moreover, due to the toxicity of most inorganic conversion coating systems, the development of novel pre-treatment strategies for technical alloys are of vital importance. Recently, the application of intrinsically conducting polymers (ICPs) have been introduced as an alternative approach for corrosion protection of Mg alloys. ICPs with electronic conductivity are known to be able to passivate small defects, however they fail in the presence of large defects due to fast coating reduction and increased cation transport if macroscopically extended percolation networks exist.
The aim of this study is to develop graphene-polymer nanocomposite thin films for corrosion protection of Mg-alloys. As polymer matrix, poly(4-vinyl pyridine) (P4VP) was selected due to its semiconducting properties and protonic conductivity. In contrast to ICPs with electronic conductivity, the pH-dependant, reversible protonation/de-protonation capability of the P4VP has been utilized to synthesize environment-responsive coatings. The presentation summarizes our recent results on the synthesis and characterization of this novel coating system with a special focus on their interfacial stability and corrosion protection properties.
Mg is a very promising material for lightweight construction and biomedical applications. However, the applicability of Mg and its alloys is hindered by its high corrosion susceptibility. Moreover, due to the toxicity of most inorganic conversion coating systems, the development of novel pre-treatment strategies for technical alloys are of vital importance. The aim of this study is to develop polymeric bilayer thin films for corrosion protection of Mg-alloys. As polymer matrix, poly(4-vinyl pyridine) (P4VP) was selected due to its semiconducting properties and protonic conductivity. In contrast to ICPs with electronic conductivity, the pH-dependant, reversible protonation/de-protonation capability of the P4VP has been utilized to synthesize environment-responsive coatings. Polyacrylicacid (PAA) was tested as crosslinking layers to improve interfacial interactions between the polymeric layers. The macroscopic corrosion properties of the bilayer coatings were investigated by means of electrochemical methods such as linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS) in corrosive media simulating technical and biomedical applications. The presentation summarizes our recent results on the synthesis and characterization of this novel coating system with a special focus on their interfacial stability and corrosion protection properties.
Für moderne Hochleistungswerkstoffe scheinen Standardparameter der Erstarrungsrissprüfung mittels MVT-Test in vielen Fällen ungeeignet. Dieser Vortrag erläutert die charakteristischen Besonderheiten der betrachteten Werkstoffe, und zeigt überdies alternative Analysemethoden auf, mit denen fehlerhafte Einschätzungen von Erstarrungsrissanfälligkeiten vermieden werden können.
Konventionelle und innovative Hochtemperaturwerkstoffe sind im technischen Betrieb einer Vielzahl an Belastungen ausgesetzt. Neben mechanischen Beanspruchungen stellt die chemische Belastung durch das Vorhandensein von aggressiven und korrosiven Medien (SO2, CO2, O2, H2O…) bei hoher Temperatur einen Schlüsselfaktor dar, der die Langlebigkeit der Materialien im Einsatz beeinflusst. Neben konventionellen, mikroskopischen Analyseverfahren bieten röntgenbasierte Techniken Möglichkeiten, die Grenzflächenreaktionen zwischen dem Werkstoff und den Medien während der chemischen Belastung (in situ) zu untersuchen. Neuartige Einblicke in die zugrunde liegenden Prozesse der Schädigungsmechanismen werden anhand von klassischen ferritischen Legierungen beschrieben. Das Verständnis von Schlüsselfaktoren zur Induzierung eines Schutzmechanismus ist insbesondere für die Entwicklung von neuartigen Materialklassen wie Hochentropie- und chemisch komplexe Legierungen notwendig. Erste Einblicke in Schädigungsmechanismen durch Gaskorrosion dieser innovativen Materialsysteme werden vorgestellt.
Rail inspection performed by ultrasonic rail inspection trains is a complex and challenging process. A large number of variables and parameters given by the environment, the track and the testing-system have an influence on the overall performance of the inspection and the inspection result. Typically the parameter vary in a combination depending on the track condition.
To evaluate the individual influence of each relevant variable, simulation tools can be used. Therefore the entire inspection process has to be transferred into a model using combined modelling techniques.
The goal of this work is to model an instrumented ultrasonic test run with a rail inspection train with the parameters varied by a script over a virtually driven distance.
Der Implant-Test nach ISO 17642-3 gehört zur Gruppe der fremdbeanspruchten Kaltrisstests, bei dem eine äußere Beanspruchung auf einen zylindrischen Stab (Implant-Probe) definiert aufgebracht wird. Mit dieser Kaltrissprüfung wurde vergleichende Analysen zur Kaltrissempfindlichkeit der modernen hochfesten Feinkornbaustähle S960MC und S960QL durchgeführt.
Asymmetrical laser-induced plasmas were investigated by a tomography approach based on the inverse Radon transform. Two distinct sources of asymmetricity were investigated: double-pulsed laser-induced plasmas in the orthogonal configuration and single-pulsed laser-induced plasmas under an inclined incidence angle. Both cases were observed at various delay times. The optical thinness of the laser-induced plasmas was achieved by appropriately adjusting the pulse energies. High temporal resolution is achieved by a gated intensified charge-coupled-device camera. The asymmetrical laser-induced plasmas are investigated in terms of their total emissivity, spectrally resolved emissivity, and temperature. The latter is obtained by the Saha–Boltzmann plot method. The images required for the inverse Radon transform technique were obtained with a high angular accuracy and reproducibility provided by mounting the spectrometer on a high-precision nano-positioning rotary stage. The plasmas were induced in the center of rotation of the stage. This arrangement allows the reconstruction of emissivity, which is integrated over a full spectral range (200-800 nm) or over a desired spectral range selected by a bandpass filter (~10 nm). It also allows for the reconstruction of spectrally-resolved emissivity in each cross sectional plasma slice by scanning the plasma across a spectrometer slit. The 3D maps of temperature and electron density are thus obtained for different types of asymmetric plasmas.
CEQAT-DGHS Interlaboratory tests for method validation and measurement uncertainty determination
(2019)
An explosion in a chemical plant or a fire on a dangerous goods vessel - the reason for such accidents can be numerous. Prevention starts in the laboratory where chemicals are tested for their hazardous properties in order to be able to assess the risks involved in their handling. For this purpose, test methods have been developed and published. They are applied globally nowadays. Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory.
Interlaboratory tests play a decisive role in assessing the reliability of test results. Participation in interlaboratory tests is not only a crucial element of the quality assurance of laboratories; as such it is explicitly recommended in DIN EN ISO/IEC 17025. In addition, interlaboratory tests are also used to develop and validate test methods and can be used for the determination of the measurement uncertainty.
Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method (see interlaboratory test reports of the CEQAT-DGHS Centre for quality assurance for testing of dangerous goods and hazardous substances: www.ceqat-dghs.bam.de).
In view of the interlaboratory test results the following conclusions can be drawn:
• To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty.
• A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods (including the determination of the measurement uncertainty) and not on proficiency tests.
• The laboratory management and the practical execution of the tests need to be improved in many laboratories.
• The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results.
Chemical compositions of the welds have significant effect on weld quality. Current inspection methods for the weld seams employ mostly post factum methods and cannot prevent weld defects.Elemental burn offs may significantly affect solidification leading to embrittlement or cracking. Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects.
In situ ED XRD und Radiographie während eines Zugversuchs an wasserstoffbeladenem Supermartensit
(2019)
Die Ergebnisse von in-situ Experimenten am Berliner Elektronenspeicherring (BESSY II) werden vorgestellt. Es wurden Zugversuche an wasserstoffbeladenen und wasserstofffreien supermartensitischen Proben durchgeführt und Diffraktionsspektren und radiographische Bilder aufgenommen. Die energiedispersive Röntgendiffraktion ermöglichte dabei die dehnungsinduzierte Phasenumwandlung von Restaustenit zu Martensit in-situ zu beobachten. Die Radiographiebilder der zerreisenden Probe gaben Einblicke in das Bruchverhalten in Abhängigkeit vom Wasserstoffgehalt des Supermartensits.
aRTist is an easy-to-use and practical simulation tool to generate realistic radiographic images from CAD objects. A dedicated add-on module makes CT simulation easy (virtual computer tomography). Just choose the number of projections.
Unlike in the practice, simulation can separately image the primary and scatter radiation. This allows studying the scattering artefacts in CT (gray-level variations in regions of homogeneous material).
Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen.
Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungskooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Im Zuge der Fallstudien wurde gezeigt, wie Niederfeld-NMR-Spektroskopie die Möglichkeiten der Konzentrationsmessung auf neue Anwendungsgebiete erweitert, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können.
Fallstudie 1: Oligomerisierung
Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit einer geeigneten Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen.
Fallstudie 2: Spaltung von cyclischen Silanverbindungen
In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine vollständig automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht.
Fallstudie 3: Qualitätskontrolle für Produktmischungen von Trialkoxysilanen
Für Produktmischungen eines Trialkoxysilans und weiteren Bestandteilen wie u. a. org. Stabilisatoren, Organozinnverbindungen, eines aromatischen Amins und org. Peroxide wurden quantitative 1H-Spektren akquiriert und eine automatische Auswertungsmethode basierend auf Indirect Hard Modeling (IHM) entwickelt. Für die Nebenkomponenten, deren Stoffmengenanteile bis zu 3 Mol-% betragen, wurden durch die zugrunde gelegte Methode typischerweise korrekte experimentelle Stoffmengenanteile gefunden, die weniger als 0,2 Mol-% vom Referenzwert abweichen.
An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies.
Residual stresses in Laser Beam Melting (LBM) – Critical Review and outlook of activities at BAM
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, which is coupled with the knowledge about the resulting material properties and performance. In particular, residual stress (RS) was soon recognized as an important issue in AM parts, such that parts are usually subjected to a post build-heat-treated. Significant effort has been spent on simulations of RS in AM, especially using finite element methods. As a consequence, the experimental determination of RS has thereby become increasingly important as a validation tool for simulations, as well as a method for assessing the influence of process parameters. In particular, diffraction methods, which are fundamentally non-destructive, offer enormous possibilities to gain knowledge on the residual stress state in real components, since synchrotron radiation and neutrons can penetrate even heavy metals up to several millimeters or centimeters, respectively. Indeed, significant progress has been achieved, in the understanding of the origins of the RS fields as a function of process parameters, as well as their stability under thermal and/or mechanical exposure.
In this paper, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with the focus on those produced by laser powder bed fusion) has even revealed that process parameters that were previously considered unimportant (e.g. the position and orientation on the base plate) play a major role in the onset of residual stress accumulation.
However, while RS characterization is starting to be considered in the component design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigates about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even those which to date are unclear, will also be discussed. These include the determination of the stress-free reference and of the principal axes of stress. All of these aspects will lead towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Traditional innovation indicators often lack coverage, granularity as well as timeliness and involve high data collection costs, especially when conducted at a large scale. Based on the assumption that firms publish information about their products and services on their own websites, the Centre for European Economic Research in Mannheim (ZEW) has developed a framework to extract information from German firm websites applying Web Mining using a free-to-use web-scraping tool.
Categorized as an intraorganizational procedural innovation, management system standards often lack research especially during the early stages of their diffusion mainly due to low data availability. Therefore, we introduce Web Mining to study the diffusion of the international management system standard ISO/IEC 27001 in Germany. Using the Mannheim Enterprise panel dataset, we first apply Web Mining to identify firms that refer to these and other common management system standards, followed by manual categorization. Second, we estimate a probit model to identify drivers for its implementation. Finally, we derive recommendations for policy makers.
Antifoulingmittel im Wasser
(2019)
Es wurden Prüfkörper aus additiver Fertigung mittels Laser Sinter Verfahren (Polyamid 12, PA 12) und Fused Layer Modeling (Acrylnitril-Butadien-Styrol, ABS) sowie Prüfkörper aus dem Kunststoff-Spritzguss Verfahren (PA 12 und ABS) über 2000 Stunden künstlich bewittert. Vor, während und nach der Bewitterung erfolgte eine zerstörungsfreie Prüfung mittels Thermografie, optischer Mikroskopie und spektralen Methoden (UV/VIS-Spektroskopie und spektrale Reflexion), um den Alterungsfortschritt zu untersuchen und Schäden durch die künstliche Bewitterung sowie eingedruckte Defekte zu identifizieren und zu detektieren.
Zusätzlich wurden zerstörende Zugprüfungen vorgenommen, welche mit einer IR-Kamera verfolgt wurden. Auf diese Weise konnten lokale Temperaturänderungen, hervorgerufen durch elastische sowie plastische Verformungen, zeitaufgelöst erfasst und ausgewertet werden.
Eleventh canSAS Meeting: International Cooperation and Collaboration in Small-Angle Scattering
(2019)
The eleventh canSAS workshop was held in Freising, Germany, July 8–10, 2019.
These international meetings, promoting collective action for nomadic small-angle scatterers, have been taking place since 1998 and act as forums to catalyze cooperation amongst the SAS community in order to provide better facilities and equipment, combined with reliable data interpretation and analysis. The meeting attracted over 60 participants from major neutron and X-ray laboratories, as well as manufacturers of SAXS equipment, and users from academia and industry. There was also a wide geographical spread with participants from Australia, Asia, and North America joining European colleagues.
Welding residual stress engineering by means of an adjusted martensite phase transformation would be highly attractive as detrimental tensile residual stresses may be prevented already during welding without time and cost intensive post processing. The present study shows a synchrotron diffraction analysis of a martensitic steel subjected to thermo-mechanical load cycles. Experiments were conducted regarding the microstructural strain response during the austenite to martensite transformation. The strains are a function of the temperature and the specific loads applied during cooling. The relation between the transformation plasticity of the material, the amount of martensite formed and the arising strains can thus be assessed. The lattice plane specific strains were compared to experimental findings from (macro) dilatation tests. It is shown that the microscopic material behavior differs remarkably from the one observed on the macroscopic scale, what leads to characteristic residual stresses in the material.
In traditional NDT, human is seen as the main source of error. The advances in NDT 4.0 lead to believe that by increased automation, people, and therefore human error, can be diminished. The research on human-automation interaction shows that increased automation does not necessarily lead to a decrease of human error, a phenomenon dubbed as “automation ironies”, introduced by Bainbridge in 1987. The research shows that whereas with automation the known human error can be prevented, there is still room for new risks and error sources, which are unknown. As we advance from automation to industry 4.0 concepts, the possibility for human error shifts slightly to the developers of systems but remains in the interaction with systems as well, as the tasks and task demands change and give rise for possible failure at different stages of the NDT process, as once known.
In der traditionellen zerstörungsfreien Prüfung wird der Mensch als Hauptfehlerquelle angesehen. Die Fortschritte bei der zerstörungsfreien Prüfung 4.0 lassen vermuten, dass durch eine verstärkte Automatisierung Menschen und damit menschliche Fehler verringert werden können. Die Untersuchung der Mensch-Automatisierungs-Interaktion zeigt, dass eine zunehmende Automatisierung nicht unbedingt zu einer Verringerung des menschlichen Fehlers führt, ein Phänomen, das 1987 von Bainbridge als „Automatisierungs-Ironien“ bezeichnet wurde. Die Untersuchungen zeigten, dass obwohl bei der Automatisierung bekannte menschliche Fehler verhindert werden können, gibt es noch Raum für neue Risiken und Fehlerquellen, die unbekannt sind. Während wir von der Automatisierung zu Industrie-4.0-Konzepten übergehen, verlagert sich die Möglichkeit menschlicher Fehler geringfügig auf die Entwickler von Systemen, bleibt jedoch auch in der Interaktion mit Systemen erhalten, da sich die Aufgaben und Aufgabenanforderungen ändern und es zu möglichen Fehlern in verschiedenen Phasen von ZfP-Prozessen kommen kann.
It is known that human factors (HF) affect the reliability of non-destructive testing (NDT). However, reliability is often expressed in probability of detection (POD) curves, obtained in practical trials, where human and organisational factors are considered only indirectly, through the few people taking part in the trials. Recently, we have observed an increase in the use of numerical modelling to obtain POD curves outside of practical trials. The so-called model-assisted POD(MAPOD) approaches have so far only very rarely included some kind of variation to account for HF. This talk presents different possibilities to include HF in MAPOD and discusses the advantages and disadvantages of each approach.
This presentation discusses industry 4.0 from the perspective of human machine interaction (HMI). Based on available literature the changes, new demands and possible problems related to people’s jobs as a result of increased digitisation and use of artificial intelligence are addressed. Combining literature with own experience in non-destructive testing (NDT), the author addresses the possible challenges and chances for the NDT personnel in the era of NDT 4.0.
Aufgrund der stark korrosiven Atmosphäre in Tunnelbauwerken kommt es aufgrund von Reinigungs- und Sanierungsmaßnahmen an Ein- und Anbauteilen aus nichtrostendem Stahl häufig zu wartungsbedingten Verkehrsbeeinflussungen und Tunnelsperrungen. Bislang ist nur eine kleine Gruppe rostfreier Edelstähle für die Verwendung in Tunnelbauwerken zugelassen. Im Sinne einer mittel- bis langfristigen Reduktion von Wartungsarbeiten besteht jedoch großes Interesse, die Einsatzmöglichkeiten alternativer nichtrostender Stähle zu erhöhen.
Um dies zu ermöglichen, entwickelten die Bundesanstalt für Materialforschung und -prüfung (BAM), gemeinsam mit dem Landesbetrieb Straßenbau NRW, in Zusammenarbeit mit der Informationsstelle Edelstahl Rostfrei (ISER), mit Unterstützung des Edelstahlherstellers Outokumpu und der Wilhelm Modersohn GmbH & Co. KG ein Forschungsprojekt zur Auslagerung von nichtrostenden Duplexstählen in Straßentunnel. Im Oktober 2019 beteiligte sich der Landesbetrieb Straßen, Brücken und Gewässer in Hamburg und ermöglichte die Auslagerung im Elbtunnel auszuweiten.
Im weitverbreiteten Fall der thermografischen ZfP sollen Defekte im Probeninneren detektiert werden. Da diese eine Inhomogenität darstellen, genügt jegliche Mess- und Datenverarbeitungstechnik, die diese Inhomogenität als Kontrast in der transienten Temperaturverteilung herausarbeitet. Ein üblicher Ansatz ist eine extrem kurze und intensive Blitzlampenbeleuchtung zusammen mit einer nachträglichen Fourier-Transformation zu verwenden. Für die zusätzliche Tiefenbestimmung werden entweder rein phänomenologische Ansätze, semi-analytische Ansätze mit Kalibrationsmessungen oder Fits an analytische bzw. numerische Modelle verwendet. Ein üblicher semi-analytischer Ansatz ist z.B. die Analyse des Abknickens der transienten Abkühlkurve. Problematisch ist das schnelle Abklingen der Amplitude auf Rauschniveau und damit die inhärente Beschränkung der Tiefenreichweite. Eine äquivalente Beschreibung der Wärmeleitung ist über sehr stark gedämpfte thermische Diffusionswellen möglich. Die Eindringtiefe ist dann gleich der thermischen Diffusionslänge. Der semi-analytische Ansatz über normales Least-Squares-Fitting funktioniert für 1D-Schicht-Systeme sehr gut, versagt aber für höherdimensionale Messprobleme. Genau hier setzt eine seit Kurzem bekannte Transformation der diffusen Temperaturentwicklung (bzw. des Realteils der Diffusionswelle) in eine propagierende virtuelle Temperaturwelle an. Dieses sog. Virtual-Wave-Konzept stellt sich selbst als ein weiteres inverses Problem dar. Der Nutzen dieser in einer linearen virtuellen Zeitdomäne propagierenden Welle überkompensiert den numerischen Mehraufwand jedoch deutlich. Zusammen mit neuen Technologien in der Erwärmung durch Hochleistungs-Laser-Arrays und in der Datenakquisition durch kHz-Kameras erlaubt dieser Ansatz eine signifikante Verbesserung der Tiefenreichweite in der Impuls-Thermografie. Im Beitrag werden experimentelle Ergebnisse an einer additiv hergestellten Metallprobe mit überdeckten Schlitzen vorgestellt, die eine Detektion dieser Defekte bis zu einem Seitenverhältnis von Defektbreite/Defekttiefe ~ 0,25 erlauben, also ca. 4 mal tiefer als die übliche Faustformel.
The spatial heterodyne spectrometer (SHS) concept, which is based on an interferometricoptical setup, boasts both the Fellgett and Jacquinot advantages. Theoretically it can provideboosted sensitivity and spectral resolution with respect to dispersion spectrometers in acompact, reasonably cheap arrangement without any moving components – this set ofcharacteristics can be attractive to a number of industrial, space and other field applications. The potential of SHS has already been demonstrated in IR and Raman spectroscopies(e.g.), and more recently also in LIBS. The scientific goal of our present project is toapply the SHS concept to the development of an optimized, but practical dual-grating,tunable SH-LIBS setup, which would possess appealing spectroscopic characteristics.During this development, we extensively rely on the computer-based simulation of theoptical setup, which is an efficient approach that we found to have been missing from earlierSHS efforts published. It can provide application-specific optimization of the SHS systemand predict the performance of the final system. In particular, we use optical simulation tostudy the effect of various important parameters on the relevant spectroscopic figures ofmerits of the system. We used the non-sequential ray-tracing mode of the Zemax/OpticStudio software for optical modelling of the SH-LIBS setup (Optical distortions were studiedin sequential mode). Characteristics of the setup and interferograms were calculated with atleast one million rays. All calculations were carried out for the visible spectral range(400-700 nm), using stepwise extension of monochromatic simulations with 5 nm steps.Wherever applicable, characteristic discrete visible wavelengths from the emissionspectrum of Hg discharge lamps (404.7 nm, 435.8 nm, 546.1 nm, 579.0 nm) were used for thecalculation of spectroscopy figures of merit and for the validation of simulation.
Asymmetrical laser-induced plasmas were investigated by a tomography approach based onthe inverse Radon transform. Two distinct sources of asymmetricity were investigated:double-pulsed laser-induced plasmas in the orthogonal configuration and single-pulsedlaser-induced plasmas under an inclined incidence angle. Both cases were observed atvarious delay times. The optical thinness of the laser-induced plasmas was achieved byappropriately adjusting the pulse energies. High temporal resolution was achieved by agated intensified charge-coupled-device camera. The asymmetrical laser-induced plasmaswere investigated in terms of their total emissivity, spectrally resolved emissivity, andtemperature. The latter was obtained by the Saha–Boltzmann plot method. The imagesrequired for the inverse Radon transform technique were obtained with a high angularaccuracy and reproducibility provided by mounting the spectrometer on a high-precisionnano-positioning rotary stage. The plasmas were induced in the center of rotation of thestage. This arrangement enabled the reconstruction of emissivity which was integrated overthe full spectral range (200–800 nm) or over a desired spectral range selected by a bandpassfilter (~10 nm). It also allowed for the reconstruction of spectrally-resolved emissivity ineach cross-sectional plasma slice by scanning the plasma across a spectrometer slit. The 3Dmaps of the temperature and electron density were thus obtained for different types ofasymmetric plasmas. The work will provide a more detailed description of the twoasymmetrical laser-induced plasmas. This might help with the development of LIBSinstrumentation using the orthogonal double-pulse geometry, or remote LIBS applicationswhich inherently rely on inclined-angle ablation.
Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured (AM) parts and important factors for residual stress formation which have implications on structural integrity. This study examined the influence of heat input on the distribution of residual stresses in two prisms produced by laser powder bed fusion (L-PBF) of austenitic stainless steel 316L.
The layers of the prisms were exposed using two distinct helix scanning strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. Residual stresses were characterised at one plane perpendicular to the building direction at half of its build height using neutron diffraction. In addition, the defect distribution was analysed via micro X-ray computed tomography (µCT) in a twin specimen.
Both scanning strategies reveal residual stress distributions typical for AM: compressive stresses in the bulk and tensile stresses at the surface. However, temperature gradients and maximum stress levels differ due to the different heat input. Regarding the X-ray µCT results, they show an accumulation of defects at the corners where the laser direction turned through 90°.
The results demonstrate that neutron diffraction and X-ray µCT can be successfully used as non-destructive methods to analyse through-thickness residual stress and defect distribution in AM parts, and in the presented case, illustrate the influence of scanning strategies. This approach contributes to deeper assessment of structural integrity of AM materials and components.
Laser based Powder Bed Fusion (L-PBF) is an additive manufacturing technique that has been continuously developed in the past years. It offers unparalleled design freedom and the resulting mechanical properties match, in some cases even exceed, those of materials processed by conventional manufacturing techniques. Nonetheless the process is prone to create Residual Stresses (RS) resulting from the sequential melting and solidification of the material. RS can reduce load bearing capacity and generate unwanted distortions thus diminishing the potential of L-PBF. This research activity aimed at characterizing the RS state in Inconel 718 L-PBF specimens using multiple diffraction methods. The microstructure as well as the surface and bulk residual stresses were investigated. The RS analysis was performed using X-ray, synchrotron and neutron diffraction methods to provide information at different depths within the specimen. The measurements were performed at the Bundesanstalt für Materialforschung und –prüfung (BAM), the EDDI beamline at BESSY II synchrotron and E3 line at BER II neutron reactor of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results revealed a depth depending RS state. The longitudinal and transverse stress components measured by X-ray and synchrotron at the surface agree well, exhibiting stress values around the yield strength of the material. In addition, synchrotron mapping showed gradients along the width and length of the sample for the longitudinal and transverse stress components. Lower RS values compared to surface RS were measured in the bulk of the material using neutron diffraction. The longitudinal stress component in the bulk was tensile and gradually decreased towards the edge of the specimen. The normal component however did not change significantly along the specimen dimensions and was of compressive nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers, which has to be further investigated.