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Eingeladener Vortrag
- nein (443)
The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling.
Everything SAXS
(2019)
This textbook fulfills its dedication of being the “essential reference for the field, featuring protocols, analysis,fundamentals and the latest advances” of impedance spectroscopy to its readers. It really provides an insight in all facets of this powerful technique.
It should not be missed in the bookshelf of electrochemists and all other interested researchers and engineers who want to be on the current state of this technique.
Experimenting on MAUS
(2019)
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals.
The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions.
First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur.
Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals.
For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range.
During the past few years significantly increasing research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical, biological, or chemical surface properties. In this contribution the mechanisms of formation and current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animal integuments, the tailoring of surface colonization by bacterial biofilms, the advancement of medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces.
To arrive to sustainable hydrogen-based energy solutions, the understanding of water-splitting catalysts plays the most crucial role. Herein, state-of-the-art hypotheses are combined on electrocatalytic active metal sites toward the oxygen evolution reaction (OER) to develop a highly efficient catalyst based on Earth-abundant cobalt and zinc oxides.
The precursor catalyst Zn0.35Co0.65O is synthesized via a fast microwaveassisted approach at low temperatures. Subsequently, it transforms in situ from the wurtzite structure to the layered γ-Co(O)OH, while most of its zinc leaches out. This material shows outstanding catalytic Performance and stability toward the OER in 1 m KOH (overpotential at 10 mA cm−2 ηinitial = 306 mV, η98 h = 318 mV). By comparing the electrochemical results and ex situ analyses to today’s literature, clear structureactivity correlations are able to be identified. The findings suggest that coordinately unsaturated cobalt octahedra on the surface are indeed the active centers for the OER.
This talk presents a new application for high-spatial resolution eddy current testing (ET) with magneto resistive (MR) sensor arrays. With rising popularity and availability of additive manufacturing (AM), companies mainly in the aerospace sector, set high requirements on quality control of AM parts, especially produced with selective laser melting (SLM). Since it was shown that those parts are prawn to flaws like pores or cracks, every part needs to be tested. Therefore, NDT Methods, like ET, could help to characterize SLM parts. Research on ET has shown, that offline ET with high spatial resolution MR sensor arrays is possible and that flaws as small as 50 µm could be detected while significantly reducing testing time. In this talk a first approach on automated online ET method for testing SLM parts is proposed. An approach with hundreds of MR sensor is made to maintain spatial resolution and short testing times. Classic signal conditioning methods are used to reduce cost and complexity while maintaining high testing bandwidths. The proposed idea enables further research on automated generation of testing reports, process control or automated flaw curing.
Nanocomposites based on MgAL layered double hydroxides (LDH) and an epoxy resin were prepared and investigated by a combination of complementary methods. As epoxy resin Bisphenol A diglycidyl ether (DGEBA) was used with Diethylenetriamine as curing agent. The LDH was modified with taurine, which acts as an additional crosslinking agent due to its amine groups. The epoxy resin was cured in a presence of the nanofiller, which was added to the system in various concentrations. X-ray scattering, by combination of SAXS and WAXS was used to characterize the morphology of the obtained nanocomposites. These investigations show that the filler is distributed in the matrix as small stacks of ca. 10 layers. The molecular dynamics of the system, as probe for structure, was investigated by broadband dielectric spectroscopy. In addition to the - and -relaxation (dynamic glass transition), characteristic for the unfilled materials, a further process was found which was assigned to localized fluctuations of segments physically adsorbed or chemically bonded to the nanoparticles. The dielectric -relaxation is shifted to higher temperatures for the nanocomposites in comparison to the pure material but depends weakly on the content of nanoparticles. Further, for the first time Flash DSC was employed to a thermosetting system to investigate the glass transition behavior of the nanocomposites. The heating rates were converted in to relaxation rates. For low concentrations of the nanofiller the thermal data overlap more or less with that of the pure epoxy. For higher concentrations the thermal data are shifted significantly to higher temperatures. This is discussed in terms the cooperativity approach to the glass transition.
High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching.
The development of hydrogen technologies is a key strategy to reduce greenhouse gas emission worldwide. Power-to-Gas is a challenging solution, in which hydrogen and methane can be used in mobility, industry, heat supply and electricity generation applications. This presentation deals with the tribological behaviour of polymer materials in hydrogen and methane, both in gas and in liquefied form.
The development of hydrogen technologies is a key strategy to reduce greenhouse gas emission worldwide. Power-to-Gas is a challenging solution, in which hydrogen and methane can be used in mobility, industry, heat supply and electricity generation applications. This presentation deals with the tribological behaviour of polymer materials in hydrogen and methane, both in gas and in liquefied form.
19th and 20th centuries glass paint layers consist of a colour body and a colourless lead silicate flux, in which borax or boric acid was added as further component to improve the paint ability and to reduce the firing temperature for multiple layers of paint. Model glasses were used in laboratory tests to investigate the stability of glass paints with additions of boron oxide. To determine boron in paint layers, a LIBS-system with pulsed NdYAG-laser was used.
Der Implant-Test nach ISO 17642-3 gehört zur Gruppe der fremdbeanspruchten Kaltrisstests, bei dem eine äußere Beanspruchung auf einen zylindrischen Stab (Implant-Probe) definiert aufgebracht wird. Mit dieser Kaltrissprüfung wurde vergleichende Analysen zur Kaltrissempfindlichkeit der modernen hochfesten Feinkornbaustähle S960MC und S960QL durchgeführt.
Heute werden in Stahlkonstruktionen zunehmend hochfeste Baustähle (Streckgrenze ≥ 960 MPa) eingesetzt. Daher sind auch in Schweißnähten solche hohen Festigkeiten gefordert. Jedoch können hohe Eigenspannungen aufgrund geringerer plastischer Dehnungsreserven in diesen Schweißnähten die Sicherheit der Bauteile vermindern. Diese sind insbesondere im Zusammenhang mit Wasserstoff und Härtegefügen risskritisch. Niedrige Bauteilbeanspruchungen und Kosteneinsparungen lassen sich heutzutage mit modernen fokussierten Lichtbogenvarianten und engeren Nahtspalten erreichen. Die vorliegende Studie zeigt allerdings, dass diese modernen Schweißprozesse und die angepasste Nahtgeometrie höhere Wasserstoffkonzentrationen und signifikant gesteigerte oberflächennahe Zugeigenspannungsniveaus bedingen. Anhand mehrlagiger Schweißversuche an S960QL unter Variation von Wärmeführung, Lichtbogenvariante und Nahtöffnungswinkel wurden die Effekte und Wechselwirkungen unter Zuhilfenahme von Eigenspannungsanalytik mittels Röntgendiffraktometrie und Wasserstoffanalytik mittels Trägergasheißextraktion systematisch untersucht. Das Schweißgefüge führte unter kritischer mechanischer Beanspruchung und erhöhtem Gehalt an diffusiblem Wasserstoff insbesondere bei geringem Nahtöffnungswinkel und fokussiertem Lichtbogen zu einer deutlichen Ausbildung von Mikrorissen. Die Mikrorisse führten teils zu einer makroskopischen Ausprägung. Durch Analysen zur Nachwärmung aus der Schweißwärme heraus konnten suffiziente Wärmeführungsparameter für eine effektive Prävention solcher Risse erarbeitet werden. Die vorliegende Arbeit zeigt anhand des Interaktionssystems bei der wasserstoffunterstützten Kaltrissbildung Gefüge-Beanspruchung-Wasserstoff, welche Wärmeführungs- und Schweißparameter sich für die hochfesten Feinkornbaustähle zur Kaltrissvermeidung eignen.
The paper provides an overview on material defects which may serve as fatigue crack initiation sites and can cause final fatigue failure of a component. These comprise nonmetallic inclusions in Steel and aluminum alloys, cavities such as pores, micro-shrinkages and un-welded regions in cast, sinter and additively manufactured alloys, graphite nodules, shrinkages and other items in modular cast iron, regions of defective microstructure, microcracks and secondary notches such as undercuts and surface roughness. Besides their origin, the effect and mechanisms on fatigue crack initiation and propagation are discussed.
The considerations are proceeded and accompanied by a Brief discussion of some Basic aspects such as the stages of crack propagation along their length scale, the overcoming of crack arrest and the question when a secondary notch can be treated as a crack.
What to measure? is a key question in nanoscience, and it is not straightforward to address as different physicochemical properties define a nanoparticle sample. Most prominent among these properties are size, shape, surface charge, and porosity. Today researchers have an unprecedented variety of measurement techniques at their disposal to assign precise numerical values to those parameters. However, methods based on different physical principles probe different aspects, not only of the particles themselves, but also of their preparation history and their environment at the time of measurement. Understanding these connections can be of great value for interpreting characterization results and ultimately controlling the nanoparticle structure–function relationship. Here, the current techniques that enable the precise measurement of these fundamental nanoparticle properties are presented and their practical advantages and disadvantages are discussed. Some recommendations of how the physicochemical parameters of nanoparticles should be investigated and how to fully characterize these properties in different environments according to the intended nanoparticle use are proposed. The intention is to improve comparability of nanoparticle properties and performance to ensure the successful transfer of scientific knowledge to industrial real‐world applications.
Zinc materials are of high importance in the field of corrosion protection. For example, almost half of the annual production of zinc is used as anti-corrosive layer for steel components, particularly under atmospheric conditions. The corrosion protection is frequently ascribed to zinc carbonate species with low solubility which form on the metal surface under atmospheric conditions. Due to the technological importance and wide use of zinc materials, its corrosion behavior and the formation of reaction products has been intensively investigated over decades.
Assuming atmospheric corrosion conditions, an initial native passive film of few nanometers thickness forms spontaneously. It consists of zinc oxide and hydroxide, transforming into various species in dependence of the surrounding atmospheric conditions.
This study focusses on the investigation of corrosion product layers on massive titanium-zinc sheets, formed during short- and mid-term exposure experiments by Fourier-transformed infrared spectroscopy. This method enables the investigation of extremely thin native passive films which form during the initial hours of exposure. Furthermore, aged surface layers are analyzed which were formed by transformation of initial passive layers over the time of several weeks. The spectroscopic investigations are complemented by scanning electron microscopy (SEM/EDX) in order to obtain information on the chemical composition and morphology of the corrosion products. The combination of both methods offers a comprehensive view on the processes occurring in the early stages of zinc corrosion.
The applicability of 1D-quadrupole-model on the depth estimation of overload-induced delaminations is tested in this contribution. While classical 1D-methods like Pulsed Phase Transformation and Thermographic Signal Reconstruction determine the depth of a defect by one parameter, a two-layer quadrupole model provides two parameters: depth and thermal resistance. In addition, the convectional losses at the surfaces may be considered. The defect investigated is a large-scale delamination in glass fibre reinforced polymer generated by tension overload.
The explosion regions of 1-propanol, 2-propanol, acetone and 1-butanol in air were measured in the presence of CO2, He, N2 and Ar in accordance with EN1839 method T at high temperatures and at atmospheric pressure. The experimental results show that 1-propanol, 2-propanol and acetone have very similar lower explosion limits (LELs). 1-Butanol shows a slightly wider explosion area near the LEL line. In addition, the explosion regions of all combustible/inert gas/air mixtures were calculated with the method of constant adiabatic flame temperature profiles (CAFTP), using the flame temperature profile along the explosion region boundary curve of each combustible/N2/air mixture as a reference to determine the explosion regions of combustible/inert gas/air mixtures with inert gases other than N2 at different initial temperatures. To calculate the explosion regions for systems containing He, the calculation method was modified to include the very different physical transport properties of He. Moreover, the procedure for calculating the apexes in the ternary explosion diagrams was modified. The calculation results show good agreement with the experimental results.
Der Vortrag stellt ein neuartiges Korrosionsprüfverfahren für Zinküberzüge auf Basis gelartiger Elektrolyte vor und führt die Vorteile gegenüber konventionellen Prüfverfahren auf. Basierend auf den Ergebnissen wird die Idee für einen IGF-Projektantrag in Kooperation mit dem Fraunhofer IKTS vorgestellt.
Several decades have passed since the initial drafting of the European standards for explosives subject to European Directive 2014/28/EU, and this field as experienced some substantial technical innovations. While at the turn of the millenium the concept of electronic detonators had just been conceived, and it is mentioned in a Technical Specification, today electronic detonators exist in many variants, also regarding communication means between shotfirer and the detonating cap. Questions regarding safe functioning and prevention of inadvertent ignition have to be asked in a quite different way, where delicate electronic circuits are used, and where information is transmitted by radio waves. In addition, the safety of functioning is partly found in software components and the corresponding standards need to be reviewed thoroughly on these grounds.
A different but in recent times more and more popular technology, is the on-site production of explosives, being mostly emulsion explosives, ANFO, or combined products. Also here software in the machinery is starting to play an important role. The on-site produced explosive must fulfil safety requirements and has to be, in addition, quality controlled. This cannot solely be left to the hopefully proper design of the software and machinery, but needs to be made accessible to verification. Since this area seems broader in approach, it is not going to be addressed by a new standard. The state of the art technology shall be described in a Technical Specification with a perspective from requirements of the above mentioned European Directive.
Since the early drafting of the European standards for civil explosives, harmonised under directive 93/15/EEC and 2014/28/EU, blasting technology has developed notably. This is particularly evident for electronic detonators and electronic firing systems, and the EU commission agreed to initiate a standardisation initiative, also noting that the currently existing document on electronic detonators is “only” a Technical Specification (CEN/TS). This paper addresses the current activities in the area of standardisation. The EU is about to launch a formal standardisation request to cover the most recent technological developments not addressed by the current standards. The request would also include various adjustments of references to the new Directive for civil explosives, and in addition the task of developing a Technical Specification for on-site mixed explosives and corresponding manufacturing units. The latter has been included to address the nowadays frequently found mobile production on the basis of ammonium nitrate prills or emulsions.
Im Vortrag wird die Problematik Mikroplastik eingeführt und ein Probenset aus dem Mittelmeer mit ersten Ergebnissen besprochen. Die Alterung von Polymeren im Umweltkontext sowie Möglichkeiten der Analyse von Polymeralterungsfortschritten werden diskutiert. Die thermoanalytische Methode mit Zersetzungsgasanalytik (TED-GC-MS) wird eingeführt und deren Einsatzmöglichkeiten in der Thematik umrissen.
Effect of Inter-Layer Dwell Time on Distortion and Residual Stresses of Laser Metal Deposited Wall
(2019)
The laser metal deposition is an advanced manufacturing technology enabling the production of large-sized parts and partially or completely elimination of machining and welding. The process is characterised by non-uniform local heating of the buildup leading to a stress distribution, which may exceed the yield strength of the material and leads to loss of dimensional accuracy. The interlayer dwell time has a strong influence on the temperature field. The effect of the interlayer dwell time on the distortion and the stress distribution during laser metal deposition of a single-pass wall on the edge of 2 mm thick plate was studied experimentally and numerically. The deposited material was IN625 and the substrate material was AISI 316. A decrease of the residual displacement, due to a uniform shrinkage after the deposition of the last layer and a lower level of the residual compressive longitudinal plastic strain, has been observed in the studies without dwell time. The peak increment of the free edge displacement corresponds to the first layer and hence the subsequent layers will be deposited on the already plastically deformed buildup. The tensile residual longitudinal stress near the top of the buildup and transverse stress near the edges of the buildup is higher than yield strength in the studies with dwell time.
3D microstructures with sub-micron resolution can be manufactured in additive manner applying multi-photon laser structuring technique. This paper is focused on the incorporation of superparamagnetic iron oxide nanoparticles into the photoresist in order to manufacture micrometer-sized devices featuring a magnetic moment. The aim of the project is to achieve untethered actuation of the presented objects through externally applied magnetic fields. Future medical application scenarios such as drug delivery and tissue engineering are targeted by this research.
Die zeitaufgelöste THz-Spektroskopie (THz-TDS) operiert mit elektromagnetischen Impulsen, die ein Amplitudenspektrum im unteren THz-Bereich aufweisen. Die THz-TDS ist in der Lage, dielektrische Volumina zerstörungs- und kontaktfreie zu durchstrahlen. Um eine 3D-THz Bildung zu ermöglichen, wurde für die THz-TDS ein rechnergestütztes Mess- und Rekonstruktionsverfahren (THz-TDSAFT) entwickelt, mit dem es gelingt, unter Verwendung der im Zeitbereich registrierten THz-TDS-Daten das Volumeninnere in Form eines dreidimensionalen Tomogramms zu rekonstruieren. Die THz-TD-SAFT basiert auf die für die Ultraschalltechnik entwickelte Synthetische Apertur Fokussierung (SAFT) bzw. des heuristisch begründeten Algorithmus des Synthetischen Apertur Radars (SAR). Anhand von Beispielen wird die Möglichkeiten der THz-TD-SAFT demonstriert und nachgewiesen, dass mit dem Rekonstruktionsansatz die künstlich eingebauten Fehlstellen bezüglich der Position und Größe geometrisch richtig im Tomogramm abgebildet werden können.
Some zinc coated advanced high strength steels (AHSS), under certain manufacturing conditions, are known to be prone to liquid metal embrittlement (LME) during resistance spot welding. LME is an undesired phenomenon, which can cause both surface and internal cracks in a spot weld, potentially influencing its strength. An effort is made to understand influencing factors of LME better, and evaluate geometry-material combinations regarding their LME susceptibility. Manufacturers benefit from such knowledge because it improves the processing security of the materials. The experimental procedure of welding under external load is performed with samples of multiple AHSS classes with strengths up to 1200 MPa, including dual phase, complex phase and TRIP steels. This way, externally applied tensile load values are determined, which cause liquid metal embrittlement in the samples to occur. In the future, finite element simulation of this procedure gives access to in-situ stress and strain values present during LME formation. The visualization improves the process understanding, while a quantification of local stresses and strains allows an assessment of specific welded geometries.
Der Vortrag behandelt in grundsätzlicher weise die Anwendung bruchmechanischer Methoden auf die rechnerische Ermittlung der Wöhlerkurve. Dabei werden die Besonderheiten des Kurzrisswachstums (Notwendigkeit der elastisch-plastischen Beschreibung der zyklischen Rissspitzenbelastung, gradueller Aufbau des Rissschlißphänomens) ebenso diskutiert wie das Problem des Mehrfachrissewachstums und Rissarrest. Die Ausführungen werden an einem Beispiel illustriert.
Der Vortrag stellt das WIPANO-Vorhaben GELELEK vor. Zu Beginn wird die Problemstellung und Projektidee kurz erläutert. Anschließend wird ein Überblick über die Projektpartner, Projektziele und Arbeitsschritte gegeben, sowie die ausgewählten Probenbleche vorgestellt. Abschließend wurde noch eine Einladung zur Teilnahme am projektbegleitenden Ausschuss ausgesprochen.
Bioanalytical, diagnostic, and security applications require the fast and sensitive determination of a steadily increasing number of analytes or events in parallel in a broad variety of detection formats.[1,2] Ideal candidates for spectral encoding and multiplexing schemes are luminescent nanocrystals like semiconductor quantum dots (QDs), particularly Cd-containing II/VI QDs with their narrow and symmetric emission bands. With the availability of relatively simple and inexpensive instrumentation for time-resolved fluorescence measurements, similar strategies utilizing the compound-specific parameter fluorescence lifetime or fluorescence decay kinetics become increasingly attractive.[3-5] The potential of different types of QDs like II/VI, III/V and Cd-free ternary QDs such as AgInS (AIS) QDs for lifetime-based encoding and multiplexing has been, however, barely utilized, although the lifetimes of these nanocrystals cover a time windows which is barely accessible with other fluorophores. Here we present a brief insight into the photophysics of AIS QDs and show the potential of dye- and QD-encoded beads for lifetime-based encoding and detection schemes in conjunction with flow cytometry and fluorescence lifetime imaging microscopy
Femtosecond laser-induced periodic surface structures: from light localization to applications
(2019)
This presentation reviews the current state in the field of Laser-induced Periodic Surface Structures (LIPSS). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized laser radiation. LIPSS are formed in a “self-ordered” way and are often accompanying material processing applications. They can be produced following a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their structural sizes typically range from several micrometers down to less than 100 nanometers exhibiting a clear correlation with the polarization direction of the laser radiation. Various types of surface structures 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, through time-resolved optical experiments and theoretical simulations. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained.
The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution.
The full-notch creep test (FNCT) is a common method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD) 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 specimens mechanically loaded in a well-defined liquid environment. Since the craze-crack damage mechanism underlying the ESC process is associated with brittle failure, the occurrence of globally brittle fracture surfaces is a prerequisite to consider an FNCT measurement as representative for ESC . Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. Due to the experimental setup, an inevitable increase of the true mechanical stress and the associated appearance of small ductile parts on fracture surfaces is induced in any case. Hence, an FNCT experiment is considered as 'valid', if the corresponding fracture surface is predominantly brittle . Based on laser scanning microscopy (LSM) height data of FNCT fracture surfaces , a universal and easy-to-use phenomenological criterion was developed to assess the validity of distinct FNCT experiments. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
Most knowledge about the structure, function, and evolution of early compound eyes is based on investigations in trilobites. However, these studies dealt mainly with the cuticular lenses and little was known about internal anatomy. Only recently some data on crystalline cones and retinula cells were reported for a Cambrian trilobite species. Here, we describe internal eye structures of two other trilobite genera. The Ordovician Asaphus sp. reveals preserved crystalline cones situated underneath the cuticular lenses. The same is true for the Devonian species Archegonus (Waribole) warsteinensis, which in addition shows the fine structure of the rhabdom in the retinula cells. These results suggest that an apposition eye with a crystalline cone is ancestral for Trilobita. The overall similarity of trilobite eyes to those of myriapods, crustaceans, and hexapods corroborates views of a phylogenetic position of trilobites in the stem lineage of Mandibulata.
Die Additive Fertigung (AM) wird eingesetzt, um komplexe Bauteile für die Luftfahrt-, Medizin- und Automobilindustrie kostengünstig und zeitsparend herzustellen. Der Einsatz von AM in der Industrie erfordert eine strenge Qualitätskontrolle der hergestellten Teile, um die geforderten Normen erfüllen zu können. Aus diesem Grund spielen die Prozessüberwachung und die Anwendung von Methoden der zerstörungsfreien Prüfung eine große Rolle, was im Fokus unserer aktuellen Forschung steht. In dieser Arbeit benutzen wir Röntgenrückstreuung, welche lediglich einen einseitigen Zugang zum Objekt benötigt, um innenliegende, künstlich hergestellte Defekte in additiv gefertigten Stufenkeilen aus Polyamid 12 (PA 12, Laser Sintering) sowie Acrylnitril-Butadien-Styrol (ABS, Fused Layer Modeling) zu untersuchen. Dafür wurde ein von der Firma AS&E (Boston, USA) konstruierter Prototyp verwendet, der ursprünglich für den Sicherheitsbereich entwickelt wurde. Die Messung der Rückstreuung basiert auf der Flying-Spot Technik mit einem stark kollimierten Nadelstrahl, erzeugt von einem rotierenden Kollimator, wobei großflächige Detektoren die rückgestreute Strahlung sammeln. Da die Anforderungen an die räumliche Auflösung sowie die Kontrastempfindlichkeit in der zerstörungsfreien Prüfung (ZfP) über denen im Sicherheitsbereich liegen, ist eine Optimierung des Prototyps notwendig, um eine Bildqualität zu erreichen, wie sie in der ZfP gefordert ist. Darüber hinaus wurden klassische Durchstrahlungsprüfungen durchgeführt, um die Fähigkeit des Rückstreusystems bei der Defekterkennung in den untersuchten Objekten einschließlich innenliegender Defekte vergleichen und bewerten zu können. Die nachweisbaren Poren und Lufteinschlüsse sind in den Durchstrahlungsaufnahmen, besonders bei den PA 12 Proben, kleiner als in den mittels Rückstreuung erzeugten Bildern. Daher ist eine weitere Optimierung des AS&E- Prototypen notwendig und zusätzliche Untersuchungen sind erforderlich, um die ZfP-Anforderungen zu erfüllen und die Anwendungsgrenzen dieses Geräts zu ermitteln. Jedoch zeigen Vergleichsmessungen mit gedruckten Leichtmetallen (Al), dass die Rückstreutechnik eine vielversprechende Methode zur in-situ Qualitätssicherung mehrerer cm großer Bauteile mit inneren Defekten ab ca. 400 μm Größe ist.
Inorganic nanoparticles are used to improve the performance of epoxy as the matrix phase in fiber-reinforced composites used for aerospace applications. The effectiveness of nanofillers on property enhancement of thermosetting polymers depends on many factors including the interaction between the functional groups of nanofillers and the polymer reactants. In the current work, we study the effect of boehmite nanoparticles (BNPs) on properties of anhydride-cured bisphenol-A-diglycidyl ether (DGEBA). Dynamic mechanical thermal analysis (DMTA) and a high-resolution force measurement approach called intermodulation atomic force microscopy (ImAFM) were carried out to investigate the thermomechanical and nanomechanical properties of this material, respectively. It was found that BNPs lead to decrease of glass transition temperature (Tg) and crosslink density of the polymer network meanwhile significantly enhancing the Young’s modulus. Besides formation of a soft interphase near the particles, significant changes in local stiffness of polymer matrix far from the interphase was observed with ImAFM. Thus, boehmite induces long-range chemical alteration on the matrix. This effect has a higher impact on overall composite properties compared to the formation of interphase which is only a short-range effect. The local chemical evaluations on the soft interphase using an infrared-AFM method (NanoIR) revealed the accumulation of anhydride hardener near the boehmite interface. Based on these observations the effect of boehmite on the curing of epoxy is hypothesized to be governed by the strong interaction between boehmite and the anhydride. This interaction causes changes the ratio of reactants in the epoxy mixture and hence alteration of curing pathway and the network architecture. In future studies we examine this hypothesis by measuring the thermomechanical properties of cured epoxies in which the epoxy-hardener ratio is systematically altered and further comparing to those properties of nanocomposites shown in the current study.
Formation of interphases between inorganic nanofillers and thermoplastic matrices are usually correlated to short-range interactions which does not exceed more than tens of nanometers away from the surface of the filler. Nevertheless, in nanocomposites with thermosetting matrices, the effect of nanofillers on the properties of the matrix is not limited to the immediate vicinities, but a long-range property alteration of the bulk polymer may be observed. The interaction between nanofillers and the polymer can disturb the curing reaction and alters the chemical, physical and mechanical properties of the polymer network in the matrix phase. In our studies, we aim to investigate short and long-range interphases of a nanocomposite system consisting of a thermosetting matrix (DGEBA) filled with an inorganic nanoparticle (boehmite). For this purpose, a combination of atomic force microscopy (AFM)-based approaches is implemented. Scanning kelvin probe microscopy (SKPM) was used to map the compositional contrast and the interphase with different electrical properties than the bulk. The mechanical properties of the interphase were probed by high resolution intermodulation AFM. (ImAFM). Furthermore, infrared spectroscopy AFM (AFM-IR) is used to investigate the chemical structure of the matrix at different distances from the nanoparticle. SKPM and (AFM-IR) measurements both show a long-range (to 10 µm) effect of boehmite on the chemical structure and surface potential of the bulk epoxy, respectively, whereas ImAFM force measurements reveals a short-range mechanical interphase between the filler and the matrix. The AFM-IR demonstrated the existence of unreacted anhydride hardener at the interphase. This indicates the preferential absorption of anhydride on the surface of boehmite. The consequence of such a selective interaction between the inorganic filler and the epoxy components is disturbance of the epoxy-hardener stoichiometric ratio, the curing mechanism. and the alteration of bulk properties of the matrix.
A new dual purpose cask design was developed for the safe transport and interim storage of spent fuel elements of German research reactors. In the framework of the safety assessment within the licensing procedure the Bundesanstalt für Materialforschung und –prüfung (BAM) as competent authority performed a series of drop tests according to the IAEA-Regulations. The package consists of a cylindrical thick-walled ductile cast iron cask body closed by a double lid system with metallic seals. A lid and bottom sided impact limiter consisting of a wood/steel construction limit the mechanical impact loading. The full-scale test specimen was equipped with a basket and assembled with dummy-fuel elements. The package and test specimen, respectively have a total mass of approximately 24 metric tons.
The mechanical test program included three 9m free drop tests, in horizontal, vertical and oblique cask orientation onto the lid system. Additionally, a 1m-puncture drop test followed the horizontal drop test to consider an IAEA-test sequence. The horizontal and vertical drop tests were performed at a temperature of minus 40°C. During the oblique drop test the upper impact limiter was heated to +80°C. The tests were conducted onto an unyielding target, fulfilling the requirements of the IAEA regulations.
The test specimen was considerably instrumented with strain gauges and accelerometers. Transient strains at selected locations of the inner and outer container walls, of the primary and secondary lid, as well as of the corresponding lid bolts were measured during the drop tests. Furthermore, decelerations in different locations at the cask body and the lids were measured. The complex geometrical deformation of the impact limiters due to the impact were determined by optical 3d- measurements using the projected fringe method in combination with multi-image photogrammetry. Before and after the drop tests the leakage rate of the lid system was determined by helium leakage testing.
The experimental results contribute to the evaluation of the package response to mechanical tests, demonstrating safety under normal and accident conditions of transport. Especially to the verification of the dynamic finiteelement model of the package used in the package design safety report. The paper describes the performance of the drop tests, selected test results focusing on the lid screws and the cask body and the deformation of the impact limiters as well as impact kinematics, respectively.
Im Europäisches Übereinkommen über die Internationale Beförderung gefährlicher Güter auf Binnenwasserstraßen ist festgelegt, welche gefährlichen Güter unter welchen Bedingungen auf europäischen Binnenwasserstraßen befördert werden dürfen. Tabelle C ‚Verzeichnis der zur Beförderung in Tankschiffen zugelassenen gefährlichen Stoffe in numerischer Reihenfolge’ (ADN 3.2.2) listet für die Stoffe, Gemische und Lösungen, deren Beförderung in Tankschiffen zugelassen ist, die anzuwendenden besonderen Vorschriften entweder in vollständiger Information oder in kodierter Form auf. In dieser Tabelle C werden für die einzelnen Stoffe vor allem die zu verwendenden Tankschifftypen, deren Ausrüstung sowie Anforderungen hinsichtlich des Explosionsschutzes, des Schutzes der aquatischen Umwelt und des Schutzes der Menschen vor längerfristigen gesundheitlichen Schäden festgelegt.
Bei dem Datenmaterial handelt es sich um durch PTB und BAM bewertete, experimentell oder rechnerisch ermittelte sicherheitstechnische Kenngrößen sowie um Angaben zu den aquatoxischen Eigenschaften und zu den längerfristigen gesundheitlichen Wirkungen auf den Menschen. Die Angaben zum Wasserverunreinigungspotential und die Zuordnungen zu den aquatoxischen Gefahren N1, N2, N3 wurden im Rahmen der Arbeiten der Zentralkommission für die Rheinschifffahrt (ZKR) zu Tabelle C vom Umweltbundesamt (UBA, J. Seelisch) zusammengestellt und bewertet. Die Angaben zu den längerfristigen gesundheitlichen Wirkungen auf den Menschen entsprechen den harmonisierten Einstufungen der EU.
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning.
Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures.
Für Bauteile (Komponenten) von Versorgungsanlagen für flüssige Brenn- und Kraftstoffe muss die Beständigkeit der metallenen Werkstoffe und Polymere nachgewiesen werden. Im Anwendungsfall von Heizöl mit 20 % biogenen Anteilen in Form von Rapsölfettsäuremethylester (FAME, Biodiesel) ist es für eine konservative Beurteilung des Korrosionssystems Werkstoff/Medium/Umgebung wichtig, die Alterungseffekte des Mediums einzubeziehen.
Entwicklung eines Prüfverfahrens für die Untersuchung der Beständigkeit von metallenen Werkstoffen und Polymeren in Heizöl und Heizöl-FAME-Blends, das für eine Vorauswahl der Werkstoffe und zum Nachweis der Beständigkeit im Hinblick auf die bauaufsichtlichen Zulassungsverfahren geeignet ist. Ein Schwerpunkt wird bei den metallenen Werkstoffen auf der Erprobung von Messmethoden liegen, mit denen sich in kurzer Versuchszeit ein Korrosionsangriff detektieren lässt.
Die untersuchten Werkstoffe Aluminium, Stahl 1.0037, 1.4301, Kupfer, Messing (CuZn40Pb) und Zink (ZP0410) sind in B0, B20, B100 und in 6 Jahre altem B100 beständig.
Auch in einem Jahr alten B20 und in einem Jahr alten B100 sind die Werkstoffe beständig.
Bei Kupfer blieb die Korrosionsrate in der Flüssigphase sowohl in B20 (0 μ m/ a) als auch in B100 (4 μ m/ a) nach einem Jahr unverändert. Für das 6 Jahre alte B100 stieg die Korrosionsrate des Kupfers an (16 μ m/a). Im Gegensatz dazu sank bei Messing die Korrosionsrate in der Flüssigphase mit dem Alter des Brennstoffs, nach einem Jahr für B20 von 4 μ m/ a auf 1 μ m/a und für B100 von 36 μ m/ a auf 6 μ m/ a, im 6 Jahre alten B100 lag die Korrosionsrate des Messings bei 0 μ m/ a.
In 8 Jahre altem B10 trat bei Zink in der Flüssigphase Flächenkorrosion auf, es ist in dem Medium demnach nicht beständig. Messing zeigte örtliche Korrosion in der Gasphase, es ist folglich unbeständig und für den Einsatz in stark gealterten B10 nicht geeignet.
Aluminium, 1.0037, 1.4301 und Kupfer sind in dem 8 Jahre alten B10 beständig.
Die Änderung der Zugfestigkeit und der Reißdehnung von ACM, HNBR und FKM in Heizöl, B20 und gealterten B10 beträgt < 15 %. Diese Werkstoffe sind in Heizöl, B20 und in gealterten B10 unter Berücksichtigung des von der BAM zur Beurteilung der Beständigkeit festgelegten Grenzwertes von 15 % bei 40 °C als beständig zu bewerten.
PUR ist bei 40 °C nicht beständig in B20 und in gealtertem B10. Bei 70 °C ist HNBR nicht in B20 beständig aufgrund der Verringerung der Zugfestigkeit (40 %) und der Reißdehnung (50 %). FKM ist bei 70 °C in Heizöl und in B20 beständig.
The present work is intended to make a contribution to the monitoring of civil engineering structures. The detection of damage to structures is based on the evaluation of spatially and temporally distributed hybrid measurements. The acquired data can be evaluated purely geometrically or physically. It is preferable to do the latter, since the cause of damage can be determined by means of geometrical-physical laws in order to be able to intervene in time and ensure the further use of the structures. For this reason, the continuum mechanical field equations in conjunction with the finite element method and hybrid measurements are combined into a single evaluation method by the adjustment calculation. This results in two challenges.
The first task deals with the relationship between the finite element method and the method of least squares. The finite element method solves certain problem classes, which are described by a system of elliptical partial differential equations. Whereas the method of least squares solves another class of problems, which is formulated as an overdetermined system of equations. The striking similarity between both methods is known since many decades. However, it remains unresolved why this resemblance exists. The contribution is to clarify this by examining the variational calculus, especially with regard to its methodological procedure. Although the well-known Gauss-Markov model within the method of least squares and the finite element method solve inherently different problem classes, it is shown that both methods can be derived by following the same methodological steps of the variational calculus. From a methodical viewpoint, this implies that both methods are not only similar, but actually the same. In addition, it is pointed out where a possible cross-connection to other methods exists.
The second task introduces a Measurement- and Model-based Structural Analysis (MeMoS) by integrating the finite element method into the adjustment calculation. It is shown in numerical examinations how this integrated analysis can be used for parameter identification of simple as well as arbitrarily shaped structural components. Based on this, it is examined with which observation types, with which precision and at which location of the structure these measurements must be carried out in order to determine the material parameters as precisely as possible. This serves to determine an optimal and economic measurement set-up. With this integrated analysis, a substitute model of a geometrically complex structure can also be determined. The issue of the detection and localisation of damage within a structure is studied by means of this structural analysis. The Measurement and Model-based Structural Analysis is validated using two different test setups, an aluminum model bridge and a bending beam.
For the vast majority of ellipsometric measurements, the application of planar substrates is mandatory and requires a proper sample alignment prior to the measurement. Here, the authors present a generalized approach of how to extract the isotropic ellipsometric sample parameters from an imaging Mueller-matrix measurement even if the sample is significantly misaligned. They validate the method by layer-thickness calculations based on imaging Mueller-matrix measurements of flat crystalline silicon samples that were misaligned on purpose. Furthermore, they also exploit this method’s capabilities to perform spatially resolved layer-thickness measurements of a single-layer indium-tin-oxide coating on a fused-silica microlens without the need of realignment or repositioning of the sample during the measurement.