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Paper des Monats
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In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
High quality tubular products are essential to the oil and gas industry. Quality control during their production focuses on the non-destructive detection of surface defects. The structured light technique is a candidate for the challenge to detect, monitor and evaluate such defects in real-time.
In the present study the automatic processing of structured light measurements is performed and validated. The algorithm for the automatic Analysis of inspection data has an advantage over current data evaluation methods based on individual assessments of operators.
This paper focuses on the scandium speciation in bauxite residues of different origin. Insights into mineralchemical similarities and differences of these materials will be presented and links to their natural geological background discussed. The presented research should provide fundamental knowledge for the future development of efficient and viable technologies for Sc-recovery from bauxite residues derived from different bauxites and accumulating at different localities. In total, five bauxite residues were investigated which originated from Greece, Germany, Hungary and Russia (North Ural & North Timan) using a combination of different analytical tools. Those included: laser ablation inductively coupled plasma mass spectrometry, X-ray absorption near Edge structure (XANES) spectroscopy, μ-Raman spectroscopy as well as scanning electron microscopy and electron microprobe analyses. X-ray fluorescence and inductively coupled plasma mass spectrometry were used to determine the overall chemical composition. The investigated samples were found to exhibit a relatively homogenous distribution of Sc between the larger mineral particles and the fine-grained matrix except for Al-phases like diaspore, boehmite and gibbsite. These phases were found to be particularly low in Sc. The only sample where Sc mass fractions in Al-phases exceeded 50 mg/kg was the Russian sample from North Ural. Fe-phases such as goethite, hematite and chamosite (for Russian samples) were more enriched in Sc than the Al-phases.
In fact, in Greek samples goethite showed a higher capacity to incorporate or adsorb Sc than hematite. Accessory minerals like zircon, rutile/anatase and ilmenite were found to incorporate higher mass fractions of Sc (>150 mg/kg), however, those minerals are only present in small amounts and do not represent major host phases for Sc. In Russian samples from North Ural an additional Ca–Mg rich phase was found to contain significant mass fractions of Sc (>500 mg/kg). μ-XANES spectroscopy was able to show that Sc in bauxite residue occurs adsorbed onto mineral surfaces as well as incorporated into the crystal lattice of certain Fe-phases. According to our observations the bauxite type, i.e. karstic or lateritic, the atmospheric conditions during bauxitization, i.e. oxidizing or reducing, and consequently the dominant Sc-bearing species in the primary Bauxite influence the occurrence of Sc in bauxite residues. In karstic bauxites, underlying carbonate rocks can work as a pH-barrier and stabilize Sc. This prevents the Sc from being mobilized and removed during bauxitization. Hence, karstic bauxites are more prone to show a Sc enrichment than lateritic bauxites. Reducing conditions during bauxitization support the incorporation of Sc into clay minerals such as chamosite, which can dissolve and reprecipitate during Bayer processing causing Sc to be redistributed and primarily adsorb onto mineral surfaces in the bauxite residue. Oxidizing conditions support the incorporation of Sc into the crystal lattice of Fe-oxides and hydroxides, which are not affected in the Bayer process. The genetic history of the bauxite is therefore the major influential factor for the Sc occurrence in bauxite residues.
High spatially resolved quantitative bioimaging of CdSe/ZnS Quantum Dots uptake in two kinds of cells is investigated combining laser ablation inductively coupled plasma mass spectrometry and the spatially resolved analysis of dried pL-droplets from a solution with a known concentration of Quantum Dots. Single cells and dried pL-droplets are morphologically characterized by Atomic Force Microscopy. A number concentration of CdSe/ZnS QDs between 3.5 104 and 48 104 is estimated to be uptaken by several selected single cells, after being incubated in the presence of a QDs suspension added to a standard cell culture medium. Mono-elemental bioimaging at subcellular resolution seems to show a higher number concentration of the CdSe/ZnS QDs in the cytosol around the cell nucleus.
Liquefied Natural Gas (LNG) aus regenerativen Quellen, stellt einen potenziellen Kraftstoff für den Schwer- und Fernverkehr des Straßenverkehrs dar. Gegenüber seinen positiven Eigenschaften zu dem in diesem Verkehrssektor häufig verwendeten Kraftstoff Diesel birgt der Kraftstoff aber auch Gefahren für Personen und Bauwerke durch seine sehr niedrige Temperatur bei der Speicherung von ca. -160 °C und seine Explosionsfähigkeit in der Gas-Phase. In der Arbeit wurde sich mit der Gefährdung von Personen und Bauwerken hinsichtlich der von LNG ausgehenden Gefahren in Tunneln auseinandergesetzt.
Tunnel stellen besonders schützenswerte Bauwerke dar, da aus vorhergehenden Störfällen in Tunneln bekannt ist, dass diese mit hohen Personen-, Bauwerks-, und Volkswirtschaftlichen-Schäden einhergehen können.
Untersuchungsschwerpunkt bei der Bewertung von Gefährdungen durch LNG stellte eine Ereigniskaskade bestehend aus Freisetzung, Verdampfung, Stoffausbreitung und Zündung des sich gebildeten explosionsfähigen LNG-Gas/Luft-Gemisches dar. Mit dem Ziel eine solche Ereigniskaskade realitätsnah vorhersagen und zukünftig hierzu Risikoanalysen durchführen zu können wurden innerhalb der Arbeit Parameterstudien sowie Kalibrierungen und Validierungen gegenüber experimentellen Untersuchungen durchgeführt.
Mit den Modellen wurden in der Arbeit exemplarische Fallbeispiele zu Störfällen untersucht. Ergebnisse dieser waren, dass Gefährdungen insbesondere von flüssigem LNG nach dessen Freisetzung und der Verbrennung von LNG-Gas/Luft-Gemischen ausgingen.zeige weniger
Liquefied Natural Gas (LNG) aus regenerativen Quellen, stellt einen potenziellen Kraftstoff für den Schwer- und Fernverkehr des Straßenverkehrs dar. Gegenüber seinen positiven Eigenschaften zu dem in diesem Verkehrssektor häufig verwendeten Kraftstoff Diesel birgt der Kraftstoff aber auch Gefahren für Personen und Bauwerke durch seine sehr niedrige Temperatur bei der Speicherung von ca. -160 °C und seine Explosionsfähigkeit in der Gas-Phase. In der Arbeit wurde sich mit der Gefährdung von Personen und Bauwerken hinsichtlich der von LNG ausgehenden Gefahren in Tunneln auseinandergesetzt.
Tunnel stellen besonders schützenswerte Bauwerke dar, da aus vorhergehenden Störfällen in Tunneln bekannt ist, dass diese mit hohen Personen-, Bauwerks-, und Volkswirtschaftlichen-Schäden einhergehen können.
Untersuchungsschwerpunkt bei der Bewertung von Gefährdungen durch LNG stellte eine Ereigniskaskade bestehend aus Freisetzung, Verdampfung, Stoffausbreitung und Zündung des sich gebildeten explosionsfähigen LNG-Gas/Luft-Gemisches dar. Mit dem Ziel eine solche Ereigniskaskade realitätsnah vorhersagen und zukünftig hierzu Risikoanalysen durchführen zu können wurden innerhalb der Arbeit Parameterstudien sowie Kalibrierungen und Validierungen gegenüber experimentellen Untersuchungen durchgeführt.
Mit den Modellen wurden in der Arbeit exemplarische Fallbeispiele zu Störfällen untersucht. Ergebnisse dieser waren, dass Gefährdungen insbesondere von flüssigem LNG nach dessen Freisetzung und der Verbrennung von LNG-Gas/Luft-Gemischen ausgingen.
Der Vortrag stellt potentielle sicherheitstechnische Fragestellungen beim weiterten Ausbau der stationären elektrischen Energiespeicher (EES) in Deutschland dar. Darüber hinaus werden aktuelle Aktivitäten und Projekte der BAM mit Bezug zur Sicherheit von Lithiumbatterien und stationären elektrischen Energiespeichern vorstellt.
Faseroptische Strahlungssensoren ermöglichen ein räumlich verteiltes Online-Monitoring entlang der gesamten Sensorfaser. Verschiedene Messverfahren nutzen überwiegend zwei durch die ionisierende Strahlung in optischen Fasern induzierte Effekte, d. h. die Erhöhung der optischen Dämpfung und die damit verbundene Veränderung des Brechungsindex des Fasermaterials. Die Sensitivität der Strahlungssensoren lässt sich je nach Anwendung durch die Wahl der Dotierstoffe im Glasfaserkern sowie der Art des Polymermaterials des POF-Sensors beeinflussen. Ferner ist die Sensitivität auch durch den Betrieb bei geeigneten Wellenlängen einstellbar. Bei dem sensorischen Einsatz von faseroptischen Sensoren muss auch die vorhandene Ausheilung des Sensors sowie die Abhängigkeit der erfassten Messsignale von der Temperatur und der Dosisleistung berücksichtigt werden.
Faseroptische Strahlungssensoren ermöglichen ein räumlich verteiltes Online-Monitoring entlang der gesamten Sensorfaser. Verschiedene Messverfahren nutzen überwiegend zwei durch die ionisierende Strahlung in optischen Fasern induzierte Effekte, d. h. die Erhöhung der optischen Dämpfung und die damit verbundene Veränderung des Brechungsindex des Fasermaterials. Die Sensitivität der Strahlungssensoren lässt sich je nach Anwendung durch die Wahl der Dotierstoffe im Glasfaserkern sowie der Art des Polymermaterials des POF-Sensors beeinflussen. Ferner ist die Sensitivität auch durch den Betrieb bei geeigneten Wellenlängen einstellbar. Bei dem sensorischen Einsatz von faseroptischen Sensoren muss auch die vorhandene Ausheilung des Sensors sowie die Abhängigkeit der erfassten Messsignale von der Temperatur und der Dosisleistung berücksichtigt werden.
Zerstörungsfreie Prüfverfahren liefern wichtige Informationen zur Beurteilung von Bauwerken. Mit ihnen können Materialeigenschaften bestimmt oder die innere Struktur von Bauteilen beschrieben werden. Für letzteres werden in der Regel Volumenverfahren angewandt. Einen besonderen Stellenwert haben in der Praxis die Radar- und die Ultraschall-Echoverfahren.
Ihre Anwendung erfordert lediglich eine einseitige Zugänglichkeit
zum Bauteil. Zudem lassen sich zahlreiche unterschiedliche Prüfaufgaben lösen. Zum Stand der Technik gehören beispielsweise die Ortung von Bewehrung und Spannkanälen, die Bestimmung der Dicke von Bauteilen oder die Fehlerlokalisierung.
In diesem Beitrag wird gezeigt, wie mithilfe von Ultraschall-Echomessungen gesammelte Messwerte in ein quantitatives Messergebnis überführt werden können, das wiederum in ingenieurtechnische Berechnungen einfließen kann. Einleitend werden die Prüfmethode und die Messtechnik erläutert. Anschließend wird das Vorgehen von der Auswertung der Messergebnisse bis zur Bestimmung der bautechnischen
Kenngröße – Bauteildicke – gezeigt. Abschließend wird die Methodik an einem Referenzprüfkörper aus Polyamid demonstriert und den Ergebnissen von Messungen an Beton gegenübergestellt.
Bei Gefahrstoffen wird oft zuerst an gefährliche Chemikalien in der verarbeitenden Industrie gedacht. Gefährliche Stoffe werden aber in nahezu jedem Betrieb und auch in Privathaushalten verwendet. Ein typisches Beispiel sind Wasch- und Reinigungsmittel, von denen viele nach der europäischen Verordnung zur Einstufung und Kennzeichnung von Chemikalien (CLP-Verordnung) als gefährlich eingestuft und gekennzeichnet sind. Darüber hinaus ist aber zu beachten, dass nicht jeder Gefahrstoff als gefährlich gekennzeichnet ist. Die Gründe dafür können mannigfaltig sein: Der Stoff oder das Gemisch werden erst durch eine bestimmte Tätigkeit zu einer Gefährdung; als Beispiele seien Wasser an Feuchtarbeitsplätzen oder aufgewirbelter, explosionsfähiger Mehlstaub genannt. Oder der Gefahrstoff wird erst durch eine Tätigkeit freigesetzt oder gebildet; als Beispiele seien aus Aerosolpackungen, wie Bauschaum oder Reinigern freigesetzte Lösemittel (siehe dazu z.B. die Fälle 9, 10, 12 und 26) oder bei Bautätigkeiten freigesetzte asbesthaltige Stäube (siehe dazu Teil 8 "Sanierung und Rückbau") genannt. Gefährdungen durch Tätigkeiten mit Gefahrstoffen können also jeden und jede betreffen.
Dementsprechend weit ist der Begriff Gefahrstoff in diesem Buch zu verstehen. Ein wesentlicher Fokus liegt zwar auf dem Gefahrstoffrecht im Sinne der Gefahrstoffverordnung (GefStoffV), die ja für Tätigkeiten von Beschäftigten gilt und Pflichten der Arbeitgeber enthält, sowie auf Unfallverhütungsrecht mit Unternehmerpflichten. Darüber hinaus beschäftigen wir uns aber auch mit Gefahrstoffen im weiteren Sinne und berühren damit auch den Privatbereich oder das Umweltrecht. Dabei stützen sich Gerichtsurteile auf allgemeine Rechtsprinzipen – etwa die in Schadensersatzprozessen einschlägige Verkehrssicherungspflicht, die in Strafverfahren relevante Frage der Fahrlässigkeit und der Garantenposition oder Grundsätze der kaufrechtlichen Sachmängelhaftung und das Produkthaftungsrecht. Auch das Zivilrecht und das Strafrecht beinhalten also gefahrstoffrechtlich relevante Vorschriften.
Zur Verbesserung gehört immer auch das Lernen aus Erfahrung und Fehlern. Dabei ist es natürlich von Vorteil, wenn man die Fehler nicht selbst machen muss, sondern die Möglichkeit hat, aus den Fehlern anderer zu lernen. Auch die Technische Regel für Gefahrstoffe TRGS 400 "Gefährdungsbeurteilung für Tätigkeiten mit Gefahrstoffen" weist darauf hin, dass "Aufzeichnungen über Unfälle, Störungen des Betriebsablaufes und 'Beinahe-Unfälle' (innerbetrieblich oder aus einschlägigen Veröffentlichungen)" bei der Ermittlung von Gefährdungen zu berücksichtigen sind und "Anlass für die Überprüfung und ggf. Überarbeitung der Gefährdungsbeurteilung sein können".
Landet ein Fall vor Gericht, dann ist etwas "schief" gelaufen und häufig hat jemand (anderes) einen Fehler gemacht, aus dem sich hoffentlich lernen lässt. Diesen Ansatz verfolgen wir, indem wir Gerichtsurteile mit Bezug zum Gefahrstoffrecht vorstellen, erläutern und analysieren. Wörtliche Zitate aus den besprochenen Urteilen haben wir dabei jeweils in kursiver Schrift kenntlich gemacht. Anhand ihrer wichtigsten Aspekte haben wir die Fälle verschiedenen Themen bzw. Stadien im "Lebenszyklus" der Gefahrstoffe zugeordnet und das Buch entsprechend unterteilt, so dass es von der Abgabe bis hin zur Entsorgung reicht. Das Buch enthält folgende Kapitel:
Teil 1 Inverkehrbringen, Verkauf und Abgabe,
Teil 2 Kennzeichnung und Verwechslungsgefahren,
Teil 3 Brand- und Explosionsgefährdungen,
Teil 4 Betriebsanweisung und Unterweisung,
Teil 5 Persönliche Schutzausrüstung (PSA),
Teil 6 An Schule und Hochschule,
Teil 7 Jugendschutz und jugendlicher Leichtsinn,
Teil 8 Sanierung und Rückbau,
Teil 9 Umweltstrafrecht,
Teil 10 Entsorgung,
Teil 11 (Neben-) Wirkungen von gefahrstoffrechtlichen Regelungen.
Teil 11 ist insofern speziell, als dass er sich nicht in den "Lebenszyklus" des Gefahrstoffs einordnen lässt, sondern andere interessante Aspekte aufgreift, wie den Nachbarschutz oder eine Klage auf Beseitigung des Eintrags von Holzstaub als krebserzeugend in einer TRGS.
The dynamic behaviour of slab and ballast tracks has been investigated by measurements and calculations. Hammer impacts and train passages have been analysed. Measurements have been performed by geophones (velocity transducers) which have been time-integrated to displacements. The calculations are done in frequency-wavenumber domain for multi-beam-on-continuous soil models. The characteristics of the different tracks and track elements have been established in theory and experiment. The frequency-dependent compliances (displacement transfer functions) show clear rail-on-rail-pad resonances or highly damped track-soil resonances. Compared to the rail and sleeper, the track plate has much lower amplitudes. The slab track has usually the highest rail amplitudes due to soft rail pads. The train passage yields track displacements which are a superposition of the axle loads from the two neighbouring axles of a bogie and from the two bogies of two neighbouring carriages. This global behaviour is characteristic for the track plate of the slab track whereas the rails of the slab and the ballast track behave more local with only one bogie of influence. The measurements agree very well with the theory of the continuous soil in case of the six measured slab tracks and acceptably well for the six measured ballast tracks. The measurements allow to find appropriate model parameters and to check the models, for example the Winkler model of the soil has been found less appropriate as it reacts more locally.
Cyclic polylactides were prepared in bulk at 170 °C, crystallized at 120 °C and then annealed at temperatures between 130 and 170 C with variation of catalyst, catalyst concentration and annealing time. The transformation of the initially formed low melting (LTm) crystallites, having melting temperatures (Tm) <180 °C into high melting (HTm) crystallites having Tm values > 189 °C was monitored by means of DSC measurements and characterized in selected cases by SAXS measurements. It was confirmed that the formation of HTm crystallites involves a significant growth of the thickness of the lamellar crystallites along with smoothing of their surface. Annealing at 170 °C for 1 d or longer causes thermal degradation with lowering of the molecular weights, a gradual transition of cyclic into linear chains and a moderate decrease of lamellar thickness. An unexpected result revealed by MALDI TOF mass spectrometry is a partial reorganization of the molecular weight distribution driven by a gain of crystallization enthalpy.
Dieser Vortrag erläutert die verschiedenen Korrosionsschutzmethoden, welche sich aus den grundlegendem Verständnis der Korrosion ableiten lassen. So werden korrosionsschutzgerechte Kontruktionen, die Asuwahl geeigneter Werkstoffe und die Vermeidung von galvanischen Elementen erläutert. Unterstützt werden die verschiedenen Themengebiete mit Praxisbeispielen.
Dieser Vortrag behandelt die Grundlagen der Korrosion metallener Werkstoffe. Es wird die Triebkraft der Korrosion, die Teilreaktionen sowie die messtechnische Bestimmung der Korrosionsgeschwindigkeit beschrieben. Weiterhin werden Korrosionselemente wie Konzentrationselemente und Bimetallkorrosion näher erläutert.
A phenomenological criterion for an optical assessment of PE-HD fracture surfaces obtained from FNCT
(2021)
The full-notch creep test (FNCT) is a common test method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD), e.g. for container materials. The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of PE-HD specimens under constant mechanical load in a well-defined liquid test environment. Since the craze-crack damage mechanism underlying the ESC phenomenon is associated with brittle failure, the occurrence of a predominantly brittle fracture surface is a prerequisite to consider an FNCT measurement as representative for ESC, i.e. a time to failure dominated by craze-crack propagation.
The craze-crack propagation continuously reduces the effective residual cross-sectional area of the specimen during the test, which results in a corresponding increase of the effective mechanical stress. Thus, a transition to ductile shear deformation is inevitable at later stages of the test, leading usually to a pronounced central ligament.
Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. An enhanced imaging analysis of FNCT fracture surfaces enables a detailed assessment of craze-crack Propagation during ESC. In this study, laser scanning microscopy (LSM) was employed to evaluate whether FNCT fracture surfaces are representative with respect to craze-crack propagation and ESC. Based on LSM height data, a phenomenological criterion is proposed to assess the validity of distinct FNCT measurements. This criterion is
supposed to facilitate a quick evaluation of FNCT results in practical routine testing. Its applicability is verified on a sample basis for seven different commercial PE-HD container materials.
Surface-supported metal-organic frameworks HKUST-1 (Hong Kong University of Science and Technology) were used as a model system for a development of a near ambient pressure (NAP) XPS based approach to investigate interaction with atmospheres of water, methanol or pyridine at pressures ranging from 1 to 4 mbar. The films were grown on a gold substrate functionalized with a COOH-terminated self-assembled monolayer using liquidphase epitaxy in a step-by-step fashion. Measurement protocols were developed and optimised for different gases in order to obtain spectra of similar quality in terms of signal intensity, noise and shape. Peak shapes were found to depend on the efficiency of charge compensation. Reference measurements in argon proved to be a useful strategy not only for the evaluation of the Cu(II)-fraction in pristine samples, but also to identify the contributions by the respective gas atmosphere to the C 1s and O 1s photoelectron spectra. Reduced copper was found during the exposition of HKUST-1 to water vapour and pyridine, but this effect was not observed in case of methanol. Additionally, it was established that there are no changes in relative Cu(II) percentage with increasing exposure time. This indicates that saturation was reached already at the lowest time of gas exposure. A detailed elucidation of the mechanism of Cu(II) reduction to Cu(I) in HKUST-1 mediated by water and pyridine is part of ongoing work and not in the scope of the present paper.
The demand for miniaturized analytical devices monitoring important parameters in the food and medical industry has increased strongly in the past decades. With fast progress, smart technologies are finding their way into our everyday life. For the future, it is, therefore, a major goal to also link analytical methods with smart technologies to create user-friendly on-site devices. In food industry the monitoring of harmful substances such as dioxins, heavy metals or mycotoxins plays a key role, since the European Commission prescribes legal limits for various food products and beverages. Therefore, companies often have their own laboratories and trained personnel. For one of the most abundant and toxic mycotoxins, Ochratoxin A (OTA) we want to present an electrochemical detection system in which the read-out can be performed with a smartphone connected via Bluetooth to a miniaturized potentiostat. The recognition of OTA is performed with specific antibodies in a competitive assay format. Anti-OTA-antibodies were captured on magnetic beads on which the competitive binding between OTA and an OTA horseradish peroxidase (HRP) tracer was performed. To quantify OTA, the enzymatic reaction of the tracer with 3,3′,5,5′-tetramethylbenzidine (TMB) and H2O2 is employed. Oxidized TMB, which is enzymatically produced by the reduction of H2O2, is quantified by amperometry with screen-printed electrodes in a custom-made flow system. Since it is well-known that oxidized TMB can precipitate on electrode surfaces, we have studied pitfalls of the electrochemical detection of TMB. By cyclic voltammetry we have compared the stability of the electrochemistry of TMB at different electrode materials (gold and carbon) and pH values (pH 1 and pH 4). It was found that a stable response of the electrode could be achieved at pH 1 on gold electrodes. Thus, we applied these reaction conditions for amperometric detection of TMB in the OTA assay. The results of the electrochemical detection method are in good correlation with the photometric detection of TMB. To demonstrate the applicability, we tested our system with OTA-spiked beer and performed the measurement via smartphone.
The elastic properties of the single-crystal nickel-base superalloy CMSX-4 used as a blade material in gas turbines were investigated by the sonic resonance method in the temperature interval between room temperature and 1300 °C. Elastic constants at such high temperatures are needed to model the mechanical behavior of blade material during manufacturing (hot isostatic pressing) as well as during technical accidents which may happen in service (overheating). High reliability of the results was achieved using specimens of different crystallographic orientations, exciting various vibration modes as well as precise measurement of the material density and thermal Expansion required for modeling the resonance frequencies by finite element method. Combining the results measured in this work and literature data the elastic constants of the gamma and gamma' phases were predicted.
This prediction was supported by measurement of the temperature dependence of the gamma'fraction.
All data obtained in this work are given in numerical or analytical forms and can be easily used for different scientific and engineering calculations.
This presentation deals with the influence of the counterface materials on the sliding behaviour of some polymer materials in hydrogen. Polyimide (PI), polyetheretherketone (PEEK) and Polytetrafluoroethylene (PTFE) materials were investigated against hardened 52100 martensitic bearing steel and 304 austenitic stainless steel with similar roughness (Ra = 0.2 μm). Results indicate that the friction and wear of PI and PEEK materials depend on the counterface material. This effect wasn’t observed for PTFE composites.
While the tribological performance of polyimide is better against 52100 in hydrogen, improved sliding behaviour of PEEK materials is observed with 304 counterface, particularly at higher sliding speed. Surface analyses of the transfer film reveal that the influence of the counterface is primarily related to the chemical nature of the steel for PI and to the thermal conductivity of the disc for PEEK materials.
Electrochemical impedance spectroscopy (EIS) is a well-established method to analyze a polymer electrolyte membrane fuel cell (PEMFC). However, without further data processing, the impedance spectrum yields only qualitative insight into the mechanism and individual contribution of transport, kinetics, and ohmic losses to the overall fuel cell limitations. The distribution of relaxation times (DRT) method allows quantifying each of these polarization losses and evaluates their contribution to a given electrocatalyst's depreciated performances. We coupled this method with a detailed morphology study to investigate the impact of the 3D-structure on the processes occurring inside a high-temperature polymer electrolyte membrane fuel cell (HT-PEMFC). We tested a platinum catalyst (Pt/C), a platinum-cobalt alloy catalyst (Pt3Co/C), and a platinum group metal-free iron-nitrogen-carbon (Fe–N–C) catalyst. We found that the hampered mass transport in the latter is mainly responsible for its low performance in the MEA (along with its decreased intrinsic performances for the ORR reaction). The better performance of the alloy catalyst can be explained by both improved mass transport and a lower ORR resistance. Furthermore, single-cell tests show that the catalyst layer morphology influences the distribution of phosphoric acid during conditioning.
The absorption and emission properties of organic dyes are generally tuned by altering the substitution pattern. However, tuning the fluorescence lifetimes over a range of several 10 ns while barely affecting the spectral features and maintaining a moderate fluorescence quantum yield is challenging. Such properties are required for lifetime multiplexing and barcoding applications. Here, we show how this can be achieved for the class of fluoranthene dyes, which have substitution-dependent lifetimes between 6 and 33 ns for single wavelength excitation and emission. We explore the substitution-dependent emissive properties in the crystalline solid state that would prevent applications.
Furthermore, by analyzing dye mixtures and embedding the dyes in carboxyfunctionalized 8 μm-sized polystyrene particles, the unprecedented potential of these dyes as labels and encoding fluorophores for time-resolved fluorescence detection techniques is demonstrated.
Search of new strategies for the inhibition of respiratory viruses is one of the urgent health challenges worldwide, as most of the current therapeutic agents and treatments are inefficient. Severe acute respiratory syndrome coronavirus 2 (SARSCoV-2) has caused a pandemic and has taken lives of approximately two Million people to date. Even though various vaccines are currently under development, virus, and especially its spike glycoprotein can mutate, which highlights a Need for a broad-spectrum inhibitor. In this work, inhibition of SARS-CoV-2 by graphene platforms with precise dual sulfate/alkyl functionalities is investigated. A series of graphene derivatives with different lengths of aliphatic chains is synthesized and is investigated for their ability to inhibit SARS-CoV-2 and feline coronavirus.
Graphene derivatives with long alkyl chains (>C9) inhibit coronavirus replication by virtue of disrupting viral envelope. The ability of these graphene platforms to rupture viruses is visualized by atomic force microscopy and cryogenic electron microscopy. A large concentration window (10 to 100-fold) where graphene platforms display strongly antiviral activity against native SARS-CoV-2 without significant toxicity against human cells is found. In this concentration range, the synthesized graphene platforms inhibit the infection of enveloped viruses efficiently, opening new therapeutic and metaphylactic avenues against SARS-CoV-2.
Antimicrobials can exert specific physiological effects when used in combination that are different from those when applied alone. While combination effects have been extensively mapped for antibiotic-antibiotic combinations, the combination effects of antibiotics with antimicrobials used as biocides or antiseptics have not been systematically investigated. Here, we investigated the effects of combinations of antibiotics (meropenem, gentamicin, and ciprofloxacin) and substances used as biocides or antiseptics [octenidine, benzalkonium chloride, cetrimonium bromide, chlorhexidine, Povidone-iodine, silver nitrate (AgNO3), and Ag-nanoparticles] on the planktonic growth rate of Pseudomonas aeruginosa. Combination effects were investigated in growth experiments in microtiter plates at different concentrations and the Bliss interaction scores were calculated. Among the 21 screened combinations, we find prevalent combination effects with synergy occurring six times and antagonism occurring 10 times. The effects are specific to the antibiotic-biocide combination with meropenem showing a tendency for antagonism with biocides (6 of 7), while gentamicin has a tendency for synergy (5 of 7). In conclusion, antibiotics and biocides or antiseptics exert physiological combination effects on the pathogen P. aeruginosa. These effects have consequences for the efficacy of both types of substances and potentially for the selection of antimicrobial resistant strains in clinical applications with combined exposure (e.g., wound care and coated biomaterials).
The catalytic potential of tin(II)acetate, tin(IV)acetate, dibutyltin-bis-acetate and dioctyl tin-bis-acetate was compared based on polymerizations of L-lactide conducted in bulk at 160 or 130C. With SnAc2 low-Lac/Cat ratios (15/1–50/1) were studied and linear chains having one acetate and one carboxyl end group almost free of cyclics were obtained. Higher monomer/catalyst ratios and lower temperatures favored formation of cycles that reached weight average molecular weights (Mw's) between 100,000 and 2,500,000. SnAc4 yielded mixtures of cycles and linear species under all reaction conditions. Dibutyltin- and dioctyl tin bis-acetate yielded cyclic polylactides under most reaction conditions with Mw's in the range of 20,000–80,000. Ring-opening polymerizations performed with ε-caprolactone showed similar trends, but the formation of COOH-terminated linear chains was significantly more favored compared to analogous experiments with lactide. The reactivity of the acetate catalysts decreased in the following order: SnAc2> SnAc4>Bu2SnAc2 Oct2SnAc2.
Brazil nut (Bertholletia excelsa) fruits are capable of resisting high mechanical forces when released from trees as tall as 50 m, as well as during animal dispersal by sharp-teethed rodents. Thick mesocarp plays a crucial part in seed protection. We investigated the role of microstructure and how sclereids, fibers, and voids affect nutshell performance using compression, tensile and fracture toughness tests. Fractured specimens were analyzed through scanning electron microscopy (SEM) and microtomography (microCT). Mesocarp showed high deformability (strain at max. stress of ~30%) under compression loading, a critical tensile strength of ~24.9 MPa, a Weibull modulus of ~3, and an elastic modulus of ~2 GPa in the tensile test. The fracture toughness, estimated through the work of fracture of SENB tests, reached ~2 kJ/m2. The thick and strong walls of mesocarp cells, with a weaker boundary between them (compound middle lamella), promote a tortuous intercellular crack path. Several toughening mechanisms, such as crack deflection, breaking of fiber bundles, fiber pullout and bridging as well as crack branching, occur depending on how fiber bundles and voids are oriented.
Background. Post-menopausal osteoporosis is a common health problem worldwide, most commonly caused by estrogen deficiency. Most of the information regarding the skeletal effects of this disease relates to trabecular bone, while cortical bone is less studied. The purpose of this study was to evaluate the influence of estrogen deficiency on the structure and mechanical properties of cortical bone.
Methods. Eight ovariectomized (OVH) and eight intact (control) Sprague Dawley rats were used. Structural features of femoral cortical bone were studied by light microscopy, scanning electron microscopy and synchrotron-based microcomputer-tomography and their mechanical properties determined by nano-indentation.
Results. Cortical bone of both study groups contains two distinct regions: organized
circumferential lamellae and disordered bone with highly mineralized cartilaginous islands. Lacunar volume was lower in the OVH group both in the lamellar and disorganized regions (182 ± 75 µm3 vs 232 ± 106 µm3 , P < 0.001 and 195 ± 86 µm3 vs. 247 ± 106 µm3 , P < 0.001, respectively). Lacunar density was also lower in both bone regions of the OVH group (40 ± 18 ×103 lacunae/mm3 vs. 47 ± 9×103 lacunae/mm3
in the lamellar region, P = 0.003 and 63 ± 18×103 lacunae/mm3
vs. 75 ± 13×103 lacunae/mm3 in the disorganized region, P < 0.001). Vascular canal volume was lower in the disorganized region of the bone in the OVH group compared to the same Region in the control group (P < 0.001). Indentation moduli were not different between the study groups in both bone regions.
Discussion. Changes to cortical bone associated with estrogen deficiency in rats require high-resolution methods for detection. Caution is required in the application of These results to humans due to major structural differences between human and rat bone.
Zinc phosphate, an important pigment in phosphate conversion coatings, forms protective films on rubbing surfaces.
We have simulated the underlying reactions under shear by ball-milling zinc phosphate and monitored the reaction of hopeite (Zn3(PO4)2·4H2O) and the retarded recrystallization of the amorphous reaction product by powder X-ray diffraction (PXRD) and quantitative infrared (IR) spectroscopy. Abrasion of stainless steel was simulated by addition of pure 57Fe. The results provide insight into the chemistry of phosphate conversion coatings or during battery cycling of metal phosphates and give theoretical guidance for the preparation of amorphous phosphates. Thermal analysis revealed that the release of structural water is a key step during the reaction of hopeite under shear to ball-milled amorphous zinc phosphate. The back-reaction and associated recrystallization kinetics of amorphous zinc phosphate show a classical Langmuir behavior. Fe impurities inhibit the recrystallization of ball-milled amorphous zinc phosphate strongly. 57Fe Mössbauer spectroscopy and PXRD revealed that Fe is oxidized to Fe2+ and Fe3+ during ball-milling and incorporated locally at the tetrahedral and octahedral sites of the structure. Ball-milled amorphous zinc phosphate is metastable as γ-Zn3−xFex(PO4)2. EPR studies showed the incorporation of Fe3+ to be coupled with the formation of Zn2+ vacancies. The Fe3+ defect sites bind water because of their higher Pearson hardness (compared to Fe2+ and Zn2+), thereby reducing water mobility and inhibiting further reactions like the recrystallization to hopeite. Our findings reveal the amorphization mechanism of Zn3(PO4)2·4H2O in stainless steel ball mills at the atomic scale and highlight how the reactivity of amorphous products is affected by impurities associated with the processing method.
Rationale: (Eco-)toxicological effects are mostly derived empirically and are notcorrelated with metal uptake. Furthermore, if the metal content is determined,mostly bulk analysis of the whole organism population is conducted; thus, biologicalvariability is completely disregarded, and this may lead to misleading results. Toovercome this issue, we compared two different solid sampling techniques for theanalysis of single organisms.Methods: In this study, complementary electrothermal vaporization/inductivelycoupled plasma mass spectrometry (ETV/ICP-MS) , laser ablation/inductivelycoupled plasma mass spectrometry (LA/ICP-MS)-based methods for the analysisof individual organisms were developed and the results obtained were comparedwith the concentrations obtained after digestion and measured using ICP-MS.For this purpose, a common (eco-)toxicological test organism, the mud shrimpCorophium volutator, was selected. As proof-of-concept application, these organismswere incubated with environmentally relevant metals from galvanic anodes, whichare often used for protection against metal corrosion in, for example, offshorewind farms.Results: The bulk analysis revealed that large quantities of the incubated elementswere detectable. Using the ETV/ICP-MS method, we could identify a highbiovariability within the population of organisms tested. Using the LA/ICP-MSmethod, it could be determined that the large quantities of the elements detectedwere due to adsorption of the metals and not due to uptake, which correlates wellwith the absence of (eco-)toxicological effects.Conclusions: The results obtained imply the efficiency of complementary methods toexplain the absence or presence of (eco-)toxicological effects. In particular, methodsthat allow for single-organism analysis or provide even a spatial resolution supportthe interpretation of ecotoxicological findings.
Mixed copper and titanium hydride powder was hot-pressed and characterized by Carrier Gas Hot Extraction, XRay Diffraction, Thermal Gravimetric Analysis coupled with Mass Spectrometry, and Scanning Electron Microscopy.
The hot-pressed and five conventional samples were applied for calibration of hydrogen in Glow Discharge Optical Emission and Mass Spectrometry. Up to the introduction of 15 ng/s hydrogen the Emission yield model is useful in Glow Discharge Optical Emission Spectrometry. A correlation between saturation and even reversal of the emission yield of the spectral lines H121, H486 and H656 and low sputtering rates was found. Hydrogen effects exist for the spectral lines of Cu(II) 219 and Ti(I) 399. In Glow Discharge Mass Spectrometry, a linear dependency of the 1H ion current on the sputtered mass per time exists over the total range of hydrogen content investigated. Hydrogen effects also exist for the sensitivity of 48Ti and 63Cu. The sputtering rate of two-phase materials depends linearly on the sputtered mass per time of one phase, which allows the sputtering rate of two-phase materials with known composition to be predicted.
With a goal to improve our understanding of the relationships between microstructural features and ultrasonic signal behavior, concrete specimens of varying water-to-cement ratio were imaged using X-ray computed tomography (CT), and subsequently subjected to ultrasonic testing. From the CT scans, measurements were made of cement paste density and number of interfaces. Ultrasonic signals produced using a through-transmission configuration were analyzed and fit to a diffusion model to separate absorption from scattering attenuation. The results showed that at the frequencies tested, ultrasonic dissipation rate correlated weakly with paste density, while diffusivity correlated well with number of interfaces, but only if entrained air is considered separately. Cement paste density was found to be very well predicted by diffusivity, leading to a clear power-law relationship between diffusivity and compressive strength.
Numerical Analysis for an Electro‐Magneto‐Mechanical Phenomenon with High‐Order Accurate Methods
(2021)
This paper establishes an axisymmetric model for a levitation device. Therein, the Maxwell equations are combined with the balance of linear momentum. Different possible formulations to describe the MAXWELL equations are presented and compared and discussed in the example. A high order finite element discretization using GALERKIN's method in space and the generalized NEWMARK‐α method in time are developed for the electro‐magneto‐mechanical approach. Several studies on spatial and temporal discretization with respect to convergence will be investigated. In addition, the boundary influences and the domain size with respect to the levitation device are also examined.
Objectives. There is concern that the integrity of fiberglass dental posts may be affected by chairside trimming during treatment. We hypothesize that hard X-ray methods of phase contrast-enhanced micro-CT (PCE-CT) and synchrotron based X-ray refraction (SXRR) can reliably identify and help characterize the extent of damage.
Methods. Fiberglass posts were imaged both as manufactured and following trimming with a diamond bur. Each of the posts was imaged by SXRR and by PCE-CT. Datasets from PCE-CT were used to visualize and quantify 2D and 3D morphological characteristics of intact and of damage-affected regions caused by trimming. Results. The SXRR images revealed fiber inhomogeneities from manufacturing with a significant increase in internal surfaces in sample regions corresponding to damage from trimming. PCE-CT volumes unveiled the micromorphology of single fibers in the posts and some damage in the trimmed area (e.g. fractures, splinters and cracks). Area, perimeter, circularity, roundness, volume and thickness of the glass fibers in the trimmed area were statistically different from the control (p < 0.01).
Significance. The integrity of single fibers in the post is critical for bending resistance and for long-term adhesion to the cement in the root canals. Damage to the fibers causes substantial structural weakening across the post diameter. Glass fragments produced due to contact with the dental bur may separate from the post and may significantly reduce bond capacity. The above mentioned synchrotron-based imaging techniques can further facilitate assessment of the structural integrity and the appearance of defects in posts (e.g. after mechanical load).
Specific control on the mid-infrared (mid-IR) Emission properties is attracting increasing attention for thermal camouflage and passive cooling applications. Metal−dielectric−metal (MDM) structures are well known to support strong magnetic polariton resonances in the optical and near-infrared range. We extend the current understanding of such an MDM structure by specifically designing Au disc arrays on top of ZnS−Au−Si substrates and pushing their resonances to the mid-IR regime. Therefore, we combine fabrication via lift-off photolithography with the finite element method and an inductance−capacitance model.
With this combination of techniques, we demonstrate that the magnetic polariton resonance of the first order strongly depends on the individual disc diameter. Furthermore, the fabrication of multiple discs within one unit cell allows a linear combination of the fundamental resonances to conceive broadband absorptance. Quite importantly, even in mixed resonator cases, the absorptance spectra can be fully described by a superposition of the individual disc properties. Our contribution provides rational guidance to deterministically design mid-IR emitting materials with specific narrow- or broadband properties.
When applying Ground Penetrating Radar (GPR) to assess the moisture content of building materials, different medium properties, dimensions, interfaces and other unknown influences may require specific strategies to achieve useful results. Hence, we present an overview of the various approaches to carry out moisture measurements with GPR in civil engineering (CE). We especially focus on the applied Signal features such as time, amplitude and frequency features and discuss their limitations. Since the majority of publications rely on one single feature when applying moisture measurements, we also hope to encourage the consideration of approaches that combine different signal features for further developments.
The determination of residual stresses becomes more complicated with increasing complexity of the structures investigated. Additive manufacturing techniques generally allow the production of ‘lattice structures’ without any additional manufacturing step. These lattice structures consist of thin struts and are thus susceptible to internal stress-induced distortion and even cracks. In most cases, internal stresses remain locked in the structures as residual stress.
The determination of the residual stress in lattice structures through nondestructive neutron diffraction is described in this work. It is shown how two difficulties can be overcome: (a) the correct alignment of the lattice structures within the neutron beam and (b) the correct determination of the residual stress field in a representative part of the structure. The magnitude and the direction of residual stress are discussed. The residual stress in the strut was found to be uniaxial and to follow the orientation of the strut, while the residual stress in the knots was more hydrostatic. Additionally, it is shown that strain measurements in at least seven independent directions are necessary for the estimation of the principal stress directions. The measurement directions should be chosen according to the sample geometry and an informed choice on the possible strain field. If the most prominent direction is not measured, the error in the calculated stress magnitude increases considerably.
Reference Materials at BAM
(2021)
Grouted connections are intensively used in offshore rigs, platforms as well as jacket and monopile offshore wind turbine structures. Being located in remote offshore conditions, these connections can experience considerable adverse loading during their lifetimes. Degradation was reported inside similar connections, which were installed in the last three decades. Grouting in the offshore sites may often be proven difficult, which eventually leads to reduced load-bearing capacity of connections in the long run. Thus, repair and rehabilitation of such connections should be planned ahead to minimize operational delays and costs. In this study, scaled grouted connections were manufactured using a novel mould, whose integrity were monitored using digital image correlation (DIC). The connections were loaded under static load to visualize the main failure pattern using distributed fibre optic sensors and acoustic emission (AE) analysis. Grouted connections were then repaired using a cementitious injectable grout. The effectiveness of the grout injection was monitored using dye penetration technique. Finally, specimens are reloaded to identify the potential of such repair for grouted connections.
Geosynthetic materials are applied in measures for coastal protection. Weathering or any damage of constructions, as shown by a field study in Kaliningrad Oblast (Russia), could lead to the littering of the beach or the sea (marine littering) and the discharge of possibly harmful additives into the marine environment. The ageing behavior of a widely used geotextile made of polypropylene was studied by artificial accelerated ageing in water-filled autoclaves at temperatures of 30 to 80 °C and pressures of 10 to 50 bar. Tensile strength tests were used to evaluate the progress of ageing, concluding that temperature rather than pressure was the main factor influencing the ageing of geotextiles. Using a modified Arrhenius equation, it was possible to calculate the half-life for the loss of 50% of the strain, which corresponds to approximately 330 years. Dynamic surface leaching and ecotoxicological tests were performed to determine the possible release of contaminants. No harmful effects on the test organisms were observed.
In this study, a multi-proxy approach combining 29Si, 27Al and 1H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO4·5H2O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects.
Additive manufacturing (AM) of alkali-activated materials is a promising method for producing ceramic precursors, construction elements and other parts. A recently introduced AM process is laser-induced slip casting of lithium aluminate/microsilica slurries, which yields parts with excellent mechanical strengths. To clarify the underlying mechanisms, μ-Raman spectroscopy was applied to parts produced by the process, and the dissolution and hydration of lithium aluminate was studied inter alia using conventional and in-situ X-ray diffraction. The results show that significant dissolution of lithium aluminate occurs, particularly at increased temperatures during laser interaction, which leads to an increase of pH and precipitation of an akopovaite-like Li-Al-CO3 layered double hydroxide. The increase of the pH is likely to induce dissolution of the microsilica and possibly formation of a hydrous lithium aluminosilicate gel. These observations explain the strength evolution of the studied parts and can also aid the development and improvement of related AM methods.
Throughout their life cycle—from production, via usage, through to disposal—materials and products interact with the environment (water, soil, air). At the same time, they are exposed to environmental influences and, through their emissions, have an impact on the environment, people, and health. Accelerated experimental testing processes can be used to predict the long-term environmental consequences of innovative products before these actually enter the environment.
The aim of this Special Issue of the journal Materials is to publish original research and review articles as well as short communications tackling the problem of reliable environmental measurement methods and reporting exemplary case studies.
One aim of this work was the development of a new setup for time- and laterally resolved XAFS measurements, based on the pronciple of dispersive XAFS. This setup is scanning free, stable, inexpensive, and straightforward to adjust for probing different elements. The second part of this work describes the impelemntation of a method for full-field X-ray fluorescence imaging with coded apertures. Expensive and complicated X-ray otpics, that are usually used for full-field imaging, are replaced with a coded aperture that consists of many pinholes drilled in an X-ray opaque material. Coded apertures are inexpensive to fabricate, energy independent and easy to use. The working principle is the same as with a pinhole camera, but the multiple holes allow a higher photon flux compared to a single pinhole or even a polycalippary optic, thus alowwing the reduction of measurement time.
News from NDT@BAM
(2021)
The presentation summarizes some recent research at BAM in the field of NDT in civil engineering. the firste xample decribes lab experiments on the degardation of concrete during tunnel fires. Radar measuremenst were sucessfully used to detect interior damage. The second example decribes the first ever experiment on using muon imaging to evaluate concrete constructions.
Reinforced concrete bridges are iconic parts of modern infrastructure. They are designed for a minimum service life of 100 years. However, environmental factors and/or inappropriate use might cause overload and accelerate the deterioration of bridges. In extreme cases, bridges could collapse when necessary maintenance lacks. Thus, the permanent monitoring for structure health assessment has been proposed, which is the aim of structural health monitoring (SHM). Studies in laboratories have shown that ultrasonic (US) coda wave interferometry (CWI) using diffuse waves has high sensitivity and reliability to detect subtle changes in concrete structures. The creation of micro-cracks might be recognized at an early stage. Moreover, large-volume structures can be monitored with a relatively small number of US transducers. However, it is still a challenge to implement the CWI method in real SHM practical applications in an outdoor environment because of the complex external factors, such as various noise sources that interfere with the recorded signals. In this paper, monitoring data from a 36-m long bridge girder in Gliwice, Poland, instrumented with embedded US transducers, thermistors, and vibrating wire strain gauges, is presented. Noise estimation and reductionmethods are discussed, and the influence of traffic, as well as temperature variation, are studied. As a result, the relative velocity variation of US waves following the temperature change with a very high precision of 10−4% is shown, and a good bridge health condition is inferred. The influence of lightweight real traffic is negligible. The study verified the feasibility of the implementation of the CWI method on real bridge structures.
Polymerizations of L-lactide catalyzed either by neat SnCl2 or by SnCl2 + difunctional cocatalysts were conducted in bulk at 180, 160 and 140 °C with variation of the Lac/Cat ratio and time. With neat SnCl2 poly(L-lactide) having weight average molecular weights (uncorrected Mw’s) up to 190 000 g mol−1 were obtained mainly consisting of linear chains. Addition of salicylic acid or 1,1-bisphenol yielded a higher fraction of cyclic polylactides but lower molecular weights. Furthermore, SnCl2 was compared with Bu2SnCl2 and various other metal chlorides and the best results were obtained with SnCl2. With ethyl L-lactate as initiator SnCl2-catalyzed ROPs were performed at 120 °C and the lac/initiator ratio was varied. All these experiments were conducted under conditions allowing for comparison with ROPs catalyzed with neat Sn(II)-2-ethyhexanoate. Such a comparison was also performed with ε-caprolactone as monomer.
Design challenges for Offshore wind-farms. From foundation mechanics to wind-farm aerodynamics
(2021)
This talk provides a brief introduction on general engineering design challenges for the offshore wind energy production. Some general features of the offshore wind-energy field from a civil engineering perspective are firstly presented, followed by a brief discussion of some of the main geomechanical issues for the foundation of the offshore turbines into the seabed.
In the following part, an overview of relevant fluid-structure interactions and some options for an efficient numerical analysis are provided, where the hydromechanical Wave–Tower interaction is firstly discussed. Then, some general aspects of the windfarm aerodynamics are introduced. On the one hand, some modelling possibilities for the wake analysis of single turbines and turbine groups are discussed. And on the other hand the relevance of such analyses for a proper windfarm layout optimization is pointed out.
In particular, this talk shows that: i) The bearing capacity of turbine multi-pile foundations can degrade under cyclic loading (waves, wind, …), while for monopile foundations cyclic hydromechanical coupling effects may take place, which may lead to a foundation softening; ii) Numerical analysis of a turbine’s interaction with wind/waves is useful and affordable, while simplified models can already provide a useful insight into the windfarm aerodynamics. iii) Turbulent wake analysis is very relevant for the windfarm layout.
The thermodynamic behavior of thin PVME films including the irreversible adsorbed layer on the substrate is investigated. In a first step, the growth kinetics of the adsorbed layer was studied combining a leaching technique and atomic force microscopy. Further, it was shown that there is a critical initial film thickness for the formation of a surface-filling adsorbed layer. Additionally, spectroscopic ellipsometry measurements were carried out to investigate the influence of the adsorbed layer on the glass transition temperature of the thin films. For 30 nm films and below, the influence of the adsorbed layer percolates strongly to the bulk-like layer of the film. Finally, the molecular dynamics of the adsorbed layer was studied by broadband dielectric spectroscopy, employing nanostructured-electrode systems. One process was revealed, which was assigned either to molecular fluctuations taking place in a loosely-bounded the part of the adsorbed layer, or to the desorption/adsorption of segments at the substrate.
Lithium ion batteries (LIBs) are prone to spontaneous and subsequent fire or explosion resulting from thermal runaway. The vented gases are not only toxic and flammable, their emission can also raise the surrounding pressure rapidly. In this study, characteristic variations of explosion pressure rise, rate of explosion pressure rise and 𝐾(sT)-value have been evaluated. The characteristic 𝐾(𝑠𝑇)-values were determined to evaluate the explosive behavior of LIBs during thermal runaway. The estimated values were compared to that of other explosive substances.
BAM Inside #1/2021
(2021)
Although in the last decades epoxy-based nanocomposites have been successfully adopted by the marine, automotive and aerospace industries they are still rarely studied on a fundamental level. This work deals with an in-depth comparative investigation of the structure, molecular mobility and vitrification kinetics of three bisphenol A diglycidyl ether (DGEBA)-based materials with different nanofillers: I) taurine-modified layered double hydroxide (T-LDH), II) boehmite (BNPs) and III) halloysite nanotubes (HNTs). Moreover, the effect of different hardeners (diethylene triamine and methyl tetrahydrophtalic acid anhydride) on the unfilled epoxy matrix is addressed as well. The chosen methodology comprises I) small – and wide – angle X-ray scattering (SAXS/WAXS) II) calorimetry in the forms of a) conventional DSC and b) static fast scanning calorimetry (FSC), III) broadband dielectric spectroscopy (BDS), as well as IV) specific heat spectroscopy in the forms of a) temperature modulated DSC, and b) temperature modulated FSC. The combination of these techniques proved an intrinsic spatial heterogeneity of epoxy-based materials, evidenced by two separate segmental relaxation processes. Although, depending on the hardener the response of the systems to calorimetric and dielectric investigations was different, in a broader sense similar conclusions can be extracted on the structural heterogeneity. As expected from the two distinct α-processes, it was shown that, in parallel to the main glass transition, epoxy-based materials can exhibit an additional low temperature vitrification mechanism, which was not discussed in prior studies for an unfilled network former. Furthermore, the interfacial region (so-called rigid amorphous fraction) was qualitatively and quantitatively addressed, in dependence of the employed nanofiller structure.
Lanthanide-doped NaYF4 upconversion nano- and microcrystals were synthesized via a facile solvothermal approach. Thereby, the influence of volume ratios of ethylene glycol (EG)/H2O, molar ratios of NH4F/RE3+ (RE3+ represents the total amount of Y3+ and rare-earth dopant ions), Gd3+ ion contents, types of activator dopant ions, and different organic co-solvents on the crystal phase, size, and morphology of the resulting particles were studied systematically. A possible formation mechanism for the growth of crystals of different morphology is discussed. Our results show that the transition from the α- to the β-phase mainly depends on the volume ratio of EG/H2O and the molar ratio of NH4F/RE3+, while the morphology and size could be controlled by the type of organic co-solvent and Gd3+ dopant ions. Furthermore, the reaction time has to be long enough to convert α-NaYF4 into β-NaYF4 during the growth process to optimize the upconversion luminescence. The formation of larger β-NaYF4 crystals, which possess a higher upconversion luminescence than smaller particles, proceeds via intermediates of smaller crystals of cubic structure. In summary, our synthetic approach presents a facile route to tailor the size, Crystal phase, morphology, and luminescence features of upconversion
materials.
Im Jahr 2011 hat der Bundestag in Deutschland den Ausstieg aus der Kernenergie beschlossen. Der angefallene Abfall wird mehr als hunderttausend Jahre eine derartig hohe Aktivität besitzen, dass er eine erhebliche Gefahr für nachfolgende Generationen darstellen kann. Dieser radioaktive Abfall soll in tiefen geologischen Formationen (z.B. Salz, Ton oder Kristallin) sicher endgelagert werden. Die Endlager werden mittels sogenannter geotechnischer Abdichtbauwerke (Schachtbzw. Streckenverschlüsse) verschlossen, wofür u.a. Zement- oder Sorel-basierte Baustoffe (Betone) in Frage kommen. Die Beschreibung des Dichtvermögens dieser Bauwerke ist unabdingbar. In der Forschungsphase werden verschiedene Werkstoffe untersucht und Methoden für die zerstörungsfreie Untersuchung der Bauwerke als Mittel der Qualitätsprüfung entwickelt. Hierbei ist der Nachweis der Rissfreiheit bzw. die Detektion möglicher Risse ein vorrangiges Thema. In den letzten Jahren konnten bereits umfangreiche Erfahrungen mit der Untersuchung von in-situ-Versuchsobjekten in Realmaßstab gesammelt werden. Die Messungen wurden im Endlager für radioaktive Abfälle Morsleben am in-situ-Versuch “Abdichtbauwerk im Steinsalz” und in der Grube Teutschenthal am Großversuch GV2 durchgeführt. Es ist gelungen mit einem neu entwickelten Ultraschall-Messsystem Eindringtiefen bis ca. 9,0 m zu realisieren. Die Messungen mit dem Large Aperture Ultrasonic System in Kombination mit der Rekonstruktion-Methode Synthetic Aperture Focusing Technique zeigen, dass die zerstörungsfreie Prüfung von Abdichtbauwerken möglich und die Nutzung des Messsystems zur Qualitätssicherung bei der Erstellung der Verschlussbauwerke vielversprechend ist.
1:1 Copolymerizations of glycolide (GL) and L-lactide (LA) is performed in bulk at 100°C and at 160°C with four cyclic tin catalysts. The resulting copolyesters are characterized by SEC measurements, 1H and 13C NMR spectroscopy and by MALDI TOF mass spectrometry. At 160°C and longer reaction time (22 h) nearly complete conversion of both monomers is achieved, and cyclic copolymers with nearly random sequences are formed. At shorter times (0.5-3.0 h, depending on catalyst) the conversion of LA is incomplete, and only cyclics having even numbers of lactyl units are obtained. At 100°C at 22 h again cycles mainly consisting of even numbered lactyl units are formed, but with even and odd numbers of glycolyl units. Copolymerization of lactide at 160°C with small amounts of GL show that formation of high Tm crystallites (Tm > 190°C) is hindered even when only > 2% of GL is added. For polyglycolide containing a smaller amount of lactide complete solubility in hexafluoroisopropanol is only observed around and above 20 mol% of lactide.
Alzheimer’s disease (AD) is characterized by accumulation of tau and amyloid-beta in the brain, and recent evidence suggests a correlation between associated protein aggregates and trace elements, such as copper, iron and zinc. In AD, distorted brain redox homeostasis and complexation by amyloid-beta and hyperphosphorylated tau May alter the isotopic composition of essential mineral elements. Therefore, high-precision isotopic analysis may reveal changes in the homeostasis of these elements. We used inductively coupled plasma-mass spectrometry (ICP-MS)-based techniques to determine the total Cu, Fe and Zn contents in the brain, as well as their isotopic compositions in both mouse brain and serum.
Results for male transgenic tau (Line 66, L66) and amyloid/presenilin (5xFAD) mice were compared to those for the corresponding age- and gendermatched wild-type control mice (WT). Our data show that L66 brains showed significantly higher Fe levels than the corresponding WT. Significantly less Cu, but more Zn was found in 5xFAD brains. We observed significantly lighter isotopic compositions of Fe (enrichment in the lighter isotopes) in the brain, and in serum of L66 mice compared to WT. For 5xFAD mice, Zn exhibited a trend towards a lighter isotopic composition in brain and a heavier isotopic composition in serum compared to WT. Neither mouse model yielded differences in the isotopic composition of Cu. Our findings indicate significant pathology-specific alterations of Fe and Zn brain homeostasis in mouse models of AD. The associated changes in isotopic composition May serve as a marker for proteinopathies Underlying AD and other types of dementia.
Covid 19 stellt Gesellschaft und Wirtschaft vor immense Herausforderungen – auch die Konformitätsbewertungsbranche ist betroffen. Die Bundesanstalt für Materialforschung und -prüfung (BAM) hat gemeinsam mit der TU Berlin und
dem Fraunhofer ISI die Auswirkungen der Pandemie auf die wirtschaftliche und operative Lage von Konformitätsbewertungsstellen in Deutschland untersucht. Dabei standen auch die Digitalisierung sowie die Resilienz der Branche im
Fokus.
Formaldehyde is considered as carcinogenic and is emitted from particleboards and plywood used in toy manufacturing. Currently, the flask method is frequently used in Europe for market surveillance purposes to assess formaldehyde release from toys, but its concordance to Levels measured in emission test chambers is poor. Surveillance laboratories are unable to afford laborious and expensive emission chamber testing to comply with a new amendment of the European Toy Directive; they need an alternative method that can provide reliable results. Therefore, the application of miniaturised emission test chambers was tested. Comparisons between a 1 m3 emission test chamber and 44 mL microchambers with two particleboards over 28 days and between a 24 L desiccator chamber and the microchambers with three puzzle samples over 10 days resulted in a correlation coefficient r2 of 0.834 for formaldehyde at steady state. The correlation between the results obtained in microchambers vs. flask showed a high variability over 10 samples (r2: 0.145),
thereby demonstrating the error-proneness of the flask method in comparison to methods carried out under ambient parameters. An exposure assessment was also performed for three toy puzzles: indoor formaldehyde concentrations caused by puzzles were not negligible (up to 8 µg/m3), especially when more conservative exposure scenarios were considered.
A key application of atomic force microscopy (AFM) is the measurement of physical properties at sub-micrometer resolution. Methods such as force–distance curves (FDCs) or dynamic variants (such as intermodulation AFM (ImAFM)) are able to measure mechanical properties (such as the local stiffness, kr) of nanoscopic heterogeneous materials. For a complete structure–property correlation, these mechanical measurements are considered to lack the ability to identify the chemical structure of the materials. In this study, the measured attractive force, Fattr, acting between the AFM tip and the sample is shown to be an independent measurement for the local chemical composition and hence a complete structure–property correlation can be obtained. A proof of concept is provided by two model samples comprised of (1) epoxy/polycarbonate and (2) epoxy/boehmite. The preparation of the model samples allowed for the assignment of material phases based on AFM topography. Additional chemical characterization on the nanoscale is performed by an AFM/infrared-spectroscopy hybrid method. Mechanical properties (kr) and attractive forces (Fattr) are calculated and a structure–property correlation is obtained by a manual principle component analysis (mPCA) from a kr/Fattr diagram. A third sample comprised of (3) epoxy/polycarbonate/boehmite is measured by ImAFM. The measurement of a 2 × 2 µm cross section yields 128 × 128 force curves which are successfully evaluated by a kr/Fattr diagram and the nanoscopic heterogeneity of the sample is determined.
A systematic approach was used to investigate the weathering-induced degradation of a common water–based intumescent coating. In this study, the coatings are intended for humid indoor applications on steel substrates. The coating contains ammonium polyphosphate, pentaerythritol, melamine, and polyvinyl acetate. By replacing each ingredient with a less water-soluble substance, the most vulnerable substances, polyvinyl acetate and pentaerythritol, were identified. Furthermore, the weathering resistance of the system was improved by exchanging the ingredients. The coatings were stressed by artificial weathering tests and evaluated by fire tests. Thermogravimetry and Fourier-transform infrared spectroscopy were used to study the thermal decomposition. This study lays the foundation for the development of a new generation of water-based intumescent coatings.
Subfloors are layered structures, consisting largely of porous building materials, such as screed. They are often suffering damage from tap water leakage, which is a typical problem in buildings, and which has largely contributed to repair costs of almost 3 billion Euro in 2018 alone in Germany. In this context, especially mould plays a role, which is both destroying the structure and posing severe health risks.
To determine the damaging effects of moisture, it is necessary to know the respective processes occurring in building materials, especially to quantify the amount of moisture and its progress in the material. In this study, humidity sensors are used to derive the material moisture experimentally.
Capacitive sensors recording the relative humidity are embedded into the screed and in the insulation materials such as expanded polystyrene, extruded polystyrene, perlite and glass wool. For the application in screed, the sensors need to be shielded against the aggressive alkaline materials. To ensure an appropriate exchange with the environment, a permeable membrane is requested. Different membrane materials have been investigated regarding their robustness and their permeability.
In the first experimental setup, two humidity sensor arrays with seven individual sensors are embedded in homogeneous screed samples. The measured corresponding relative humidity of the screed is converted to the material moisture based on the approach of Hillerborg. In a second experimental setup, a layered structure of a complete subfloor is built in a box of 0.8 m times 0.8 m. The humidity sensors are positioned in the different insulation materials of various thicknesses. By adding water, leakage damage is simulated and its progress and effect is investigated experimentally.
The investigations point at the question if the observed moisture is able to generate damage such as mould. The moisture and corresponding humidity values are discussed. It will be shown that this low-cost hygrometric approach can be used easily for moisture monitoring of screed and insulation materials as well
Due to the importance of reinforced concrete structures for modern society, damage assessment during the entire life-cycle of such structures has become a special interest in non-destructive testing. Using embedded ultrasound sensors in combination with other measurement methods, numerical modeling and self-made data collectors, tailored specifically for monitoring tasks, the German research group DFG FOR CoDA aims to investigate and develop novel methods for damage detection and rapid model updating in reinforced concrete structures. In the first stage of the project, besides the development of custom-built, low-cost data collectors, ultrasonic transducers are embedded in a large, reinforced concrete specimen on a BAM test site near Berlin. In this experiment, the influence of changing environmental conditions (mainly temperature) on the ultrasound signal is investigated using coda-wave interferometry. The results show a correlation between changes in temperature and ultrasonic velocity. Such changes must be taken into consideration in a long-term monitoring setup to distinguish between reversible and permanent changes. By correcting the data using a linear relation between concrete temperature and velocity change to remove the seasonal trends and by low-pass filtering the data to remove daily variations can remove most of the temperature influence on the ultrasound measurements.
The purpose of this contribution is to introduce and to apply the developed approach of incorporating non-destructively gathered measurement results (instead of deterministic information and assumptions) into a reassessment model of a typical prestressed concrete road bridge and to outline the advantages. An essential part is the quality evaluation of the non-destructively measured information, that deals primarily with two questions. Could the object or parameter to be obtained reliably detected and if, how accurate are the inspection results achieved? Therefore, the importance of the combination of a probability of detection (POD)-approach and measurement uncertainty calculations is emphasized. With regard to the introduced case-study it is shown, for which structure parameters an assumption deviating from the actual (and measurable) situation has a particularly strong (and possibly arithmetically unfavorable) influence on the structural reliability. Measurements on such parameters are particularly beneficial for a reliable and robust reassessment. In conclusion, the individual reassessment results without consideration and with consideration of evaluated non-destructive inspection results are compared.
The stability of the keyhole decreases for deep penetrated high-power laser beam welding. The keyhole tends to collapse with increasing laser power and e.g. keyhole induced porosity can occur. This study deals with the observation of the keyhole during high-power laser beam welding in partial penetration mode by means of a high-speed camera. A butt configuration of 25 mm thick structural steel and transparent quartz glass was used for the experiments. An oscillating magnetic field was applied perpendicular to the welding direction on the root side of the steel plate. The keyhole was highlighted with a coaxial diode laser. It was ascertained that the stability of the keyhole and the weld penetration depth were increased by applying an oscillating magnetic field with an oscillating frequency of 1.2 kHz and a magnetic flux density of 50 mT.
Many measurements of train induced ground vibrations show high amplitudes for a certain mid-frequency range. This ground vibration component cannot be well explained by dynamic loads of the train. Many characteristics indicate that the axle impulses, which are scattered by an irregular soil, are the excitation. This new understanding of railway-induced ground vibration is verified by numerical analysis. The response of the regular homogeneous and irregular inhomogeneous soils has been calculated by the finite-element method in frequency domain. A specific superposition of the impulse responses has been invented including time shift, axle sequence, track filter and hanning filter. The superposition yields the quasi-static component of the ground vibration which is restricted to very low frequencies and to the close near-field of the track. In case of an irregular soil of which the stiffness varies randomly in space, the superposition yields a mid-frequency ground vibration component from the scattering of the axle impulses. The existence and the importance of this component can thus be demonstrated by the calculations. Some rules of the influence of distance, train speed, soil stiffness, strength and width of the stiffness variation have been derived from the calculations. Many measurements show the unique explanation of the mid-frequency ground vibration component by the scattered axle impulses.
The choice of solvents influences crystalline solid formed during the crystallization of active pharmaceutical ingredients (API). The underlying effects are not always well understood because of the complexity of the systems. Theoretical models are often insufficient to describe this phenomenon. In this study, the crystallization behavior of the model drug paracetamol in different solvents was studied based on experimental and molecular dynamics data. The crystallization process was followed in situ using time-resolved Raman spectroscopy. Molecular dynamics with simulated annealing algorithm was used for an atomistic understanding of the underlying processes. The experimental and theoretical data indicate that paracetamol molecules adopt a particular geometry in a given solvent predefining the crystallization of certain polymorphs
Der Vortrag behandelt die Passivität von nichtrostenden Stählen. Es werden Ausführungen zur Passivschichtbildung und deren Kinetik gemacht. Weiterhin werden lokale Korrosionsarten näher erläutert und deren Mechanismen erklärt. An praktischen Beispielen werden inner und äussere Einflussfaktoren auf die Passivität und Korrosionsbeständigkeit von nichtrostenden Stählen näher beleuchtet und erklärt.
The purpose of this paper is to investigate the relationship between hydride morphology, in particular the presence of radial hydrides (RHs), stress state and failure mechanisms associated with the ring compression test (RCT). Samples of ZIRLO®cladding were pre-hydrided and subjected to thermo-mechanical treatments to precipitate long radial hydrides. The results show that the reorientation treatment was very successful. A considerable fraction of RHs was generated, the radial hydride continuity factor being around 80 to 90% of the wall thickness. The samples with reoriented hydrides were tested using the RCT at room temperature. Macroscopic brittle failure was observed with sudden load drops for displacements around 0.5 mm, with a calculated “offset strain”between 0.5 and 1%. Crack nucleation occurs in RHs located in regions with the highest values of hoop stress. These locations are the inner diameter of cladding at the vertical plane of the sample (12 and 6 o’clock positions) and the outer diameter at the horizontal plane (3 and 9 o’clock positions). Noticeable load drops in the RCT are associated with unstable crack propagation events through the radial hydride network, the crack front reaching up to 90% of the wall thickness in some cases. The failure micro-mechanism is quasi-cleavage in the hydrides and micro-void nucleation, growth and coalescence in the Zr matrix, with ductile tearing patches connecting neighboring hydrides. The main conclusion is that radial hydride metrics is not the only parameter that determines cladding failure in the presence of RHs, but the interaction between the location and continuity of RHs and the stress normal to the hydride (the hoop stress in this case). Consequently, if a radial hydride is located at a position within the cladding where the hoop stress is small, a crack will not be initiated easily in the RCT.
Geopolymers and alkali-activated materials have emerged as a complement, and partly as an alternative, to traditional materials in various applications, such as traditional ceramics, energy saving, waste management, building construction, and filtration. These new materials can play an important role in mitigating climate change and promoting a circular economy, which is one of the reasons why they are being actively researched in many laboratories around the world.
Open Ceramics, the official, peer-reviewed, Open Access journal of the European Ceramic Society, is dedicated to foster this research and is compiling a Special Issue with the title “Alkali-activated and geopolymer materials in ceramics and various applications”. The aim of this Special Issue is to promote new applications, the use of previously underused raw materials, and in particular a better understanding of the chemical and mechanical behavior of these materials.
The scope of the Special Issue includes, but is not limited to, research on the following topics:
- valorization of previously underused raw materials
- a better understanding of established raw materials
- detailed spectroscopic characterization of alkali-activated materials and geopolymers to elucidate their phase assemblage
- the mechanism of formation of the phase(s) that comprise these binders
- control of their mechanical properties
- the effect of fillers/aggregates on their mechanical properties
- their durability under various conditions and the underlying deterioration mechanisms
- special applications and recycling-related considerations.
The aluminum alloy 2618A is applied for engine components such as radial compressor wheels which operate for long time at elevated temperatures. This results in coarsening of the hardening precipitates and degradation in mechanical properties during the long-term operation, which is not taken into account in the current lifetime prediction models due to the lack of quantitative microstructural and mechanical data. To address this issue, a quantitative investigation on the evolution of precipitates during long-term aging at 190 °C for up to 25,000 h was conducted. Detailed transmission electron microscopy (TEM) was combined with Brinell hardness measurements and thorough differential scanning calorimetry (DSC) experiments. The results showthat GPB zones and S-phase Al2CuMg grow up to < 1,000 h during which the GPB zones dissolve and S-phase precipitates form. For longer aging times, only S-phase precipitates coarsen, which can be well described using the Lifshitz–Slyozov Wagner theory of ripening. A thorough understanding of the underlying microstructural processes is a prerequisite to enable the integration of aging behavior into the established lifetime models for components manufactured from alloy 2618A.
The dispersive properties of Lamb waves can be utilised for material characterisation because the frequency-wavenumber-relationship, as well as the group velocity, depend on material parameters. These dependencies make a non-destructive estimation of an elastic constant possible. This preliminary study investigates the sensitivity of dispersion curves caused by a change in elastic constants. The Scaled Boundary Finite Element Method is used to compute special dispersion curves, which show the sensitivity value of the frequency and group velocity as a colour value. This representation allows for easy identification of patterns and local effects. Two sets of dispersion curves are presented, one set for a steel plate and the other set for a plate made of a carbon fibre reinforced polymer. In general, we notice that the sensitivity often increases with the frequency and that higher-order modes seem to be more suitable for material characterisation. Moreover, specific modes respond to material changes while others are relatively unaffected, which must be taken into consideration for material characterisation.
A simplified methodology is proposed to estimate the dynamic pressures developed within partially filled cylindrical vertical tanks when subjected to earthquake-related horizontal accelerations. The total pressure at the bottom of the tank is calculated as the superposition of vertical and horizontal pressures. While the magnitude of the vertical pressure depends on the free surface height of the liquid, the horizontal pressure depends on the magnitude of the horizontal acceleration and on the diameter of the tank. The liquid free surface oscillation angle is simulated based upon the principles of the simple pendulum analogy for sloshing. The length of the pendulum, however, is set on the basis of a methodology to calculate the free sloshing frequency of partially filled containers. Such a methodology is experimentally verified in this work. The outputs of the model for full scale situations, suggest that the lateral perturbation - sloshing phenomenon (earthquake effect) can generate an increase in the total pressure of 56% above the no lateral perturbation situation, further suggesting that such an overpressure should be taken into account when designing tanks that could be potentially subjected to earthquake-related perturbations.
For reliability and safety issues of injection wells, corrosion resistance of materials used needs to be determined. Herein, representative low-cost materials, including carbon steel X70/1.8977 and low alloyed steel 1.7225, were embedded in mortar to mimic the realistic casing-mortar interface. Two types of cement were investigated: (1) Dyckerhoff Variodur commercial Portland cement, representing a highly acidic resistant cement and (2) Wollastonite, which can react with CO2 and become stable under a CO2 stream due to the carbonation process. Exposure tests were performed under 10 MPa and at 333 K in artificial aquifer fluid for up to 20 weeks, revealing crevice corrosion and uniform corrosion instead of expected pitting corrosion. To clarify the role of cement, simulated pore water was made by dispersing cement powder in aquifer fluid and used as a solution to expose steels. Surface analysis, accompanied by element mapping on exposed specimens and their crosssections, was carried out to trace the chloride intrusion and corrosion process that followed.
Geothermal brines often contain high amounts of lead and copper ions that can precipitate as native Cu and Pb as consequence of galvanic corrosion when brines react with carbon steel materials. This contribution evaluates which materials could overcome the problem of galvanic corrosion at geothermal environment.
The behavior of these materials in water containing high chloride concentration (> 100 g/L NaCl) as well as various amounts of dissolved bCl2 and/or CuCl2 was characterized by electrochemical and exposure measurements.
Both methods reveal carbon steel suffers corrosion susceptibility, accompanied by Cu◦ and/or Pb◦ precipitation on the surface. Electrochemical measurements on stainless steels result in significant difference in corrosion and repassivation potentials (Ecorr = -189 mV, Erep = 70 mV), indicating a good corrosion resistance.
Due to increasing ageing, deterioration and loading , several prestressed concrete bridges bulit in the 1950ies and 1960ies need monitoring. Recently several bridges have sucesssfully equipped with acoustic emission sensing system. BAM works together with several universities on an add onn: Active ultrasonic monitoring combined with coda wave interferometry will help to detect subtle changes and precursors fo failure earlier than other methods.
The Jack Rabbit II (JR II) chlorine field trials in 2015 and 2016 involved nine 5–20 ton releases of pressurized liquefied chlorine from a tank mounted 1 m above a broad flat desert sand surface. A model comparison study was initiated, where 17 widely-used dense-gas dispersion models were run by scientists in seven countries.
Predictions were submitted following specified formats, using specified emissions and meteorology inputs. To compare with the model predictions, sets of observations were defined for the arc-maximum 1–3 s averaged concentrations (arc max C) and for cloud widths and heights (to 20 ppm and 200 ppm contours) at distances from 0.2 to 11.0 km from the release. The initial focus is on the three field trials (1, 6, and 7) that have the highest observed concentrations and that have detailed emissions information. It is found that these models are able to satisfactorily simulate (generally within a factor of two) the observed arc max C’s and their variation with downwind distance at this flat desert site. At each downwind distance, the scatter in the arc max C predictions covers about 1 ½ orders of magnitude, but the observed arc max C is within the range of the predictions. The median of the cloud width predictions is about 50% larger than the observed value for the three trials. The median of the cloud height predictions is within about 10% of the observed value. For both cloud width and/or height, there are a few models with large (factor of 3 or higher) overpredictions. Of the 17 models, when compared to observations, there is a core group of 5 or 6 with consistently (across all three trials and all distances) less mean error and scatter in their predictions of arc max C and cloud width and height. However, as a group, the 17 models are performing adequately (using the “factor of two” rule of thumb). An important caveat is that, at the JR II desert site, chlorine deposition is minimal. At a site with vegetation and/or organic-rich soil, the effects of removal of chlorine by deposition are expected to be significant.
Natural building materials for interior fitting and refurbishment - What about indoor emissions?
(2021)
Indoor air quality can be adversely affected by emissions from building materials, consequently having a negative impact on human health and well-being. In this study, more than 30 natural building materials (earth dry boards and plasters, bio-based insulation materials, and boards made of wood, flax, reed, straw, etc.) used for interior works were investigated as to their emissions of (semi-) volatile organic compounds ((S)VOC), formaldehyde, and radon. The study focused on the emissions from complete wall build-ups as they can be used for internal Partition walls and the internal insulation of external walls. Test chambers were designed, allowing the compounds to release only from the surface of the material facing indoors under testing Parameters that were chosen to simulate model room conditions. The emission test results were evaluated using the AgBB evaluation scheme, a procedure for the health-related evaluation of construction products and currently applied for the approval of specific groups of building materials in Germany.
Seventeen out of 19 sample build-ups tested in this study would have passed this scheme since they generally proved to be low-emitting and although the combined emissions of multiple materials were tested, 50% of the measurements could be terminated before half of the total testing time.
The durability of flame retardancy is a challenge for cables over long lifetimes. The degradation of flame retardance is investigated in two kinds of exposures, artificial weathering and humidity. In this basic study, typical mineral flame retardants in two polymers frequently used in cable jackets are investigated to get the fundamental picture. Aluminum hydroxide (ATH) and magnesium hydroxide (MDH) are compared in ethylene‐vinyl acetate (EVA), and further in EVA and linear low‐density polyethylene (LLDPE) cables containing the same ATH. The changes in chemical structure at the surface are studied through attenuated total reflectance Fourier transform infrared spectroscopy (ATR‐FTIR), the formation of cracks, and changes in color are investigated. The cone calorimeter and a bench scale fire testing cable module are utilized to evaluate the fire behavior of the cables. Although the flame retardancy deteriorated slightly, it survived harsh exposure conditions for 2000 h. Compared to EVA/MDH and LLDPE/ATH, the fire behavior of EVA/ATH is the least sensitive. Taken together, all of the results converge to estimate that there will be no problem with flame retardancy performance, for materials subjected to natural exposure for several years; the durability of fire retardancy is questionable for longer periods, and thus requires further investigation.
This review summarizes recent developments regarding molecular imaging markers for magnetic resonance imaging (MRI) of prostate cancer (PCa). Currently, the clinical standard includes MR imaging using unspecific gadolinium-based contrast agents. Specific molecular probes for the diagnosis of PCa could improve the molecular characterization of the tumor in a non-invasive examination. Furthermore, molecular probes could enable targeted therapies to suppress tumor growth or reduce the tumor size.
Durch die Einbeziehung von gemessenen Daten bei der Bewertung von bestehenden Bauwerken können Unsicherheiten bei der Beurteilung des Tragverhaltens reduziert werden, ohne das normative Zuverlässigkeitsniveau einzuschränken. Informationen sind die wesentliche Grundlage für die Analyse der Zuverlässigkeit von Tragwerken. Umso wichtiger ist die Kenntnis über die Präzision und die Richtigkeit der verwendeten Informationen. Aus messtechnischer Sicht kann ein Messwert, dem keine Messunsicherheit beigeordnet wurde, als wertlos erachtet werden. Liegt ein vollständig dokumentiertes Messergebnis vor, so ist die Qualität der gemessenen Information bekannt und deren Vergleichbarkeit gewährleistet. In diesem Beitrag wird am Beispiel einer Spannbetonbrücke und zweier Grenzzustände gezeigt, wie Messergebnisse aus der zerstörungsfreien Prüfung in probabilistische Nachweise von Bestandsbauwerken einfließen können und welche Auswirkungen die Implementierung von gemessenen Daten bei der Bewertung von Bestandsbauwerken haben kann.
Laser based powder bed fusion additive manufacturing offers the flexibility to incorporate standard and userdefined scan strategies in a layer or in between the layers for the customized fabrication of metallic components. In the present study, four different scan strategies and their impact on the development of microstructure, texture, and residual stresses in laser powder bed fusion additive manufacturing of a nickel-based superalloy Inconel 718 was investigated. Light microscopy, scanning electron microscopy combined with electron backscatter diffraction, and neutron diffraction were used as the characterization tools. Strong textures with epitaxially grown columnar grains were observed along the build direction for the two individual scan strategies. Patterns depicting the respective scan strategies were visible in the build plane, which dictated the microstructure development in the other planes. An alternating strategy combining the individual strategies in the successive layers and a 67◦ rotational strategy weakened the texture by forming finer microstructural features. Von Mises equivalent stress plots revealed lower stress values and gradients, which translates as lower distortions for the alternating and rotational strategies. Overall results confirmed the scope for manipulating the microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing by effectively controlling the scan strategies.
Properties of alkali-activated mortars with salt aggregate for sealing structures in evaporite rock
(2021)
Concrete structures for sealing of tunnels in the host rock are an essential part of systems for nuclear waste storage. However, concretes based on blended cements or magnesium oxychloride cements, which are commonly considered for this application, can deteriorate severely due to a significant heat of hydration and associated deformation and cracking. Alkali-activated materials (AAMs) offer a potential solution to this problem because of their low heat release during hardening. To explore their suitability for the construction of sealing structures in evaporite rock, various AAMs with salt aggregate were studied regarding fresh properties, heat release, mechanical properties and microstructure. The heat of reaction of the AAMs was up to 55% lower than that of a blended cement designed for sealing structures, indicating significant benefits for the intended application. Other relevant properties such as mechanical strength and permeability depended strongly on the mix-design of the AAMs and curing conditions.
Active thermography is a fast, contactless and non-destructive technique that can be used to detect internal defects in different types of material. Volumetric irregularities such as the presence of pores in materials produced by the Additive Manufacturing processes can strongly affect the thermophysical and the mechanical properties of the final component.
In this work, an experimental investigation aimed at detecting different pores in a sample made of stainless AISI 316L produced by Laser Powder Bed Fusion (L-PBF) was carried out using pulsed thermography in reflection mode. The capability of the technique and the adopted setups in terms of geometrical and thermal resolution, acquisition frequency and energy Density of the heating source were assessed to discern two contiguous pores as well as to detect a single pore. Moreover, a quantitative indication about the minimum resolvable pore size among the available and analysed defects was provided. A powerful tool to assess the Limits and the opportunities of the pulsed technique in terms of detectability and localizability was provided by comparing active thermography results to Computed Tomography as well as a related Finite Element Analysis (FEA) to simulate the pulsed heating transfer with Comsol.
The negative effects induced in marine organisms by Climate Change related abiotic factors consequences, namely ocean warming, are well-known. However, few works studied the combined impacts of ocean warming and contaminants, as pharmaceutical drugs. Carbamazepine (CBZ) and cetirizine (CTZ) occur in the marine environment, showing negative effects in marine organisms. This study aimed to evaluate the impacts of Ocean warming on the effects of CBZ and CTZ, when acting individually and combined (drug vs drug), in the edible clam Ruditapes philippinarum. For that, drugs concentration, bioconcentration factors and biochemical parameters, related with clam’s metabolic capacity and oxidative stress, were evaluated after 28 days exposure to environmentally relevant scenarios of these stressors. The results showed limited impacts of the drugs (single and combined) at control and warming condition. Indeed, it appeared that warming improved the oxidative status of contaminated clams (higher reduced to oxidized glutathione ratio, lower lipid peroxidation and Protein carbonylation levels), especially when both drugs were combined. This may result from clam’s defence mechanisms activation and reduced metabolic capacity that, respectively, increased elimination and limited production of reactive oxygen species. At low stress levels, defence mechanisms were not activated which resulted into oxidative stress. The present findings highlighted that under higher stress levels clams may be able to activate defence strategies that were sufficient to avoid cellular damages and loss of redox homeostasis.
Nevertheless, low concentrations were tested in the present study and the observed responses may greatly Change under increased pollution levels or temperatures. Further research on this topic is needed since marine heat waves are increasing in frequency and intensity and pollution levels of some pharmaceuticals are also increasing in coastal systems.
Calibration-Free Chemical Process and Quality Control Units as Enablers for Modular Production
(2021)
Modular chemical production is a tangible translation of the digital transformation of the process industry for specialty chemicals. In particular, it enables the speeding-up of process development and thus a quicker time to market by flexibly connecting and orchestrating standardised physical modules and bringing them to life (i.e., parameterising them) with digitally accumulated process knowledge.
We focus on the specific challenges of chemical process and quality control, which in its current form is not well suited for modular production and provide possible approaches and examples of the change towards direct analytical methods, analytical model transfer or machine-supported processes.
Continuing our study on (CO2 + O2) mixtures, this work reports new experimental (p, rho, T) data for two oxygen-rich mixtures with mole fractions x(O2) = (0.50 and 0.75) mol·mol−1, in the temperature range T = (250–375) K and pressure range p = (0.5–20) MPa, using a single-sinker densimeter. Experimental density data were compared to two well-established equation-of-state models: EOS-CG and GERG-2008. In the p, T-range investigated, the EOS-CG gave a better reproduction for the equimolar mixture (x(O2) = 0.5), whereas the GERG-2008 performed significantly better for the oxygen-rich mixture (x(O2) = 0.75). The EOS-CG generally overestimates the density, while the GERG-2008 underestimates it. This complete set of new experimental data, together with previous measurements, is used to calculate the virial coefficients B(T, x) and C(T, x), as well as the second interaction virial coefficient B12(T) for the (CO2+ O2) system.
Thermoplastic modified thermosets are of great interest especially due to their improved fracture toughness. Comparable enhancements have been achieved by adding different nanofillers including inorganic particles such as nanosized boehmite. Here, we present a nanomechanical study of two composite systems, the first comprising a polycarbonate (PC) layer in contact with epoxy resin (EP) and the second consisting of a PC layer containing boehmite nanoparticles (BNP) which is also in contact with an EP layer. The interaction between PC and EP monomer is tested by in situ Fourier transformed infrared (FT-IR) analysis, from which a reaction induced phase separation of the PC phase is inferred. Both systems are explored by atomic force microscopy (AFM) force spectroscopy. AFM force-distance curves (FDC) show no alteration of the mechanical properties of EP at the interface to PC. However, when a PC phase loaded with BNP is put in contact with an epoxy system during curing, a considerable mechanical improvement exceeding the rule of mixture was detected.
The trend of BNP to agglomerate preferentially around EP dominated regions and the stiffening effect of BNP on EP shown by spatial resolved measurements of Young's modulus, suggest the effective presence of BNP within the EP phase.
This paper focuses on the influence of the counterface materials on the sliding behaviour of polymer materials in hydrogen. Polyimide (PI), polyetheretherketone (PEEK) and Polytetrafluoroethylene (PTFE) materials were investigated against hardened 52100 martensitic bearing steel and 304 austenitic stainless steel with similar roughness (Ra = 0.2 μm). Results indicate that the friction and wear of PI and PEEK materials depend on the counterface material. This effect wasn’t observed for PTFE composites. While the tribological performance of polyimide is better against 52100 in hydrogen, improved sliding behaviour of PEEK materials is observed with 304 counterface, particularly at higher sliding speed. Surface analyses of the transfer film reveal that the influence of the counterface is primarily related to the chemical nature of the steel for PI and to the thermal conductivity of the disc for PEEK materials.
Mussel-inspired multifunctional coating for bacterial infection prevention and osteogenic induction
(2021)
Bacterial infection and osteogenic integration are the two main problems that cause severe complications after surgeries. In this study, the antibacterial and osteogenic properties were simultaneously introduced in biomaterials, where copper nanoparticles (CuNPs) were generated by in situ reductions of Cu ions into a mussel-inspired hyperbranched polyglycerol (MI-hPG) coating via a simple dip-coating method. This hyperbranched polyglycerol with 10 % catechol groups’ modification presents excellent antifouling property, which could effectively reduce bacteria adhesion on the surface. In this work, polycaprolactone (PCL) electrospun fiber membrane was selected as the substrate, which is commonly used in biomedical implants in bone regeneration and cardiovascular stents because of its good biocompatibility and easy post-modification. The as-fabricated CuNPs-incorporated PCL membrane [PCL-(MI-hPG)-CuNPs] was confirmed with effective antibacterial performance via in vitro antibacterial tests against Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), and multi-resistant E. coli. In addition, the in vitro results demonstrated that osteogenic property of PCL-(MI-hPG)-CuNPs was realized by upregulating the osteoblast-related gene expressions and protein activity. This study shows that antibacterial and osteogenic properties can be balanced in a surface coating by introducing CuNPs.
Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS are classified, relevant control parameters are identified, and their material-specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Many microorganisms including free-living and symbiotic fungi weather minerals through the formation of biofilms on their surface. Weathering thus proceeds not only according to the mineral’s chemistry and the environmental conditions but also according to the local biofilm chemistry. These processes can be dissected in experiments with defined environmental settings and by employing genetic tools to modify traits of the fungal biofilm. Biofilms of the rock-inhabiting fungus Knufia petricola strain A95 (wild-type, WT) and its melanin-deficient mutant (ΔKppks) were grown on polished olivine sections in subaerial (air-exposed) and subaquatic (submerged) conditions. After seven months of interaction at pH 6 and 25°C, the fungus-mineral interface and abiotic olivine surface were compared using high resolution transmission electron microscopy (HRTEM). The abiotic, subaquatic olivine section showed a 25 nm thick, continuous amorphous layer, enriched in Fe and depleted in Si compared to the underlying crystalline olivine. This amorphous layer formed either through a coupled interfacial dissolution reprecipitation mechanism or through the adsorption of silicic acid on precipitated ferric hydroxides. Its thickness was likely enhanced by mechanical stresses of polishing. Directly underneath a fungal biofilm (WT and mutant alike), the surface remained mostly crystalline and was strongly etched and weathered, indicating enhanced olivine dissolution. The correlation between enhanced olivine dissolution and the absence of a continuous amorphous layer is a strong indication of the dissolution-inhibiting qualities of the latter. We propose that the fungal biofilm sequesters significant amounts of Fe, preventing formation of the amorphous layer and driving olivine dissolution onwards. The seemingly similar olivine surface underneath both WT and mutant biofilms illustrates the comparably insignificant role of specific biofilm traits in the weathering of olivine once biofilm attachment is imposed. Under subaerial conditions, the absence of water on the abiotic surface prohibited olivine dissolution. This was overcome by the water retention capacities of both the WT and mutant biofilm: the olivine surface underneath subaerial fungal biofilms was as weathered as the corresponding subaquatic olivine surface. Under the studied environmental settings, the effect of fungal biofilms on olivine weathering seems to be universal, independent of the production of melanin, the composition of extracellular polymeric substances (EPS) or air-exposure.