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Eingeladener Vortrag
- nein (443)
The need for steels with highest mechanical properties is a result of the increasing demands for energy and resource efficiency. In this context, high-strength low-alloyed (HSLA) structural steels are used in machine, steel and crane construction with yield strength up to 960 MPa. HSLA steels enable lightweight construction by thinner necessary plate thickness. However, welding of HSLA steels requires profound knowledge of three factors in terms of avoidance of hydrogen-assisted cracking (HAC): the interaction of (1) microstructure, (2) local stress/strain and (3) local hydrogen concentration. In addition to the three main factors, the used weld-arc process is also important for the performance of the welded joint, especially when using modern arc variants. In the past, the conventional transitional arc process (Conv. A) was mainly used for welding of HSLA grades. In the past decade, the so-called modified spray arc process (Mod. SA) was increasingly used for welding production. This modified arc enables reduced seam opening angles with increased deposition rates compared to the conventional process. Economic benefits of using this arc type are: a reduced number of necessary weld beads and a lower weld seam volume, which result in decreased total welding time and costs. Nonetheless, investigations on a high-strength S960QL showed significantly higher hydrogen concentrations in the weld metal at a reduced seam opening angle with Mod. SA. This indicates an increased risk for the susceptibility of the welded component to HAC. Hence, existing recommendations on HAC-avoidance cannot be transferred directly to the Mod. SA-process.
In the present study, the susceptibility to HAC of the HSLA steel S960QL with same type of filler material was investigated. For that purpose, both Conv. A and Mod. SA were used with same weld heat input at different deposition rates. For assessment of the HAC susceptibility, the externally loaded Implant-test was used. Both conducted test series with Conv. A and Mod. SA showed similar crack critical stress of about 280 MPa. Below this value, no delayed fracture appeared. The welds with Mod. SA showed higher hydrogen concentrations. The fracture occurred in the heat-affected zone (HAZ) or in the weld metal (WM). But in all specimens, cracks initiated at the notch root of the spiral notch of the implants within the coarse-grained HAZ. However, the test series with Mod. SA showed a significant extension of the time-to-failure of several hours compared to tests carried out with Conv. A. The reason is the deeper weld penetration in case of Mod. SA, which causes longer diffusion path for hydrogen. The fracture topography of the ruptured implant specimens with Conv. A was typical ductile in specimen center and quasi-cleavage like at the edge of the specimens. When using Mod. SA, the topography changed to primarily quasi-cleavage fracture topography with shares of intergranular fracture and secondary crack appearance.
Die Messung von Flüssigkeitskonzentrationen in Rohrsystemen ist von großem Interesse für viele unterschiedliche Anwendungen. Die meisten Messsysteme sind jedoch nicht in der Lage, die Flüssigkeit direkt im Rohr zu untersuchen und es muss eine zusätzliche Vorrichtung, wie z.B. einem Bypass, angebracht werden, welche den Kontakt zwischen Flüssigkeit und Sensor ermöglicht.
Um den Einbauaufwand gering zu halten und die Strömungseigenschaften des Rohres nicht zu beeinflussen, wird ein neuartiges Messsystem entwickelt, welches als Teil der Rohrwand ausgeführt werden kann. Dieses neuartige System ist angelehnt an die Idee der phononischen Kristallen (PnK). PnK’s bestehen im Allgemeinen aus einem Matrixmaterial, in welchem Streuzentren periodisch angeordnet sind. Dies führt beim Eintreffen einer akustischen Welle in definierten Frequenz-bereichen, sogenannter Bandlücken, zu zunehmender destruktiven Interferenz. Wird innerhalb einer solchen Bandlücke durch Einbringen einer flüssigkeitsgefüllten Kavität ein Resonanzverhalten erzeugt, kann dies genutzt werden, um die Flüssigkeit zu analysieren.
Im Rahmen von Voruntersuchung wird zunächst das akustische Verhalten des PnK’s, welcher für die Sensorentwicklung genutzt werden soll, unter Vernachlässigung der Flüssigkeit ausführlich untersucht. Hierbei werden zunächst die Bandlücken ermittelt und das Übertragungsverhalten betrachtet. Dieses wird im Anschluss experimentell überprüft. Hierzu werden neben herkömmlichen Fertigungsverfahren auch additive Verfahren zur Herstellung der Proben genutzt.
Forschungsprojekt zum Korrosionsverhalten von Edelstählen - BAM und VSM mit neuen Erkenntnissen
(2019)
Wie kann man verhindern, dass Edelstahl korrodiert? Und welchen Einfluss haben Kornarten und Körnungen von Schleifmitteln auf das Korrosionsverhalten? Diesen Fragen ist die Bundesanstalt für Materialforschung und -prüfung (BAM) mit Unterstützung der VSM AG zwei Jahre lang auf den Grund gegangen. Heute wurden im VSM Technical Center am Hauptsitz von VSM in Hannover die Ergebnisse vorgestellt. Die zentralen Erkenntnisse: Kornarten und Zusätze im Schleifmittel haben keinen Einfluss auf die Korrosion. Aber: Je feiner die Oberfläche geschliffen ist, desto besser ist der Korrosionsschutz. Dabei ist das Einhalten der Schleiffolge besonders wichtig.
We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low.
Understanding the interaction between nanoparticles and the matrix and the properties of interphase is crucial to predict the macroscopic properties of a nanocomposite system. Here, we investigate the interaction between boehmite nanoparticles (BNPs) and epoxy using different atomic force microscopy (AFM) approaches. We demonstrate benefits of using multifrequency intermodulation AFM (ImAFM) to obtain information about conservative, dissipative and van der Waals tip-surface forces and probing local properties of nanoparticles, matrix and the interphase.
We utilize scanning kelvin probe microscopy (SKPM) to probe surface potential as a tool to visualize material contrast with a physical parameter, which is independent from the mechanics of the surface. Combining the information from ImAFM stiffness and SKPM surface potential results in a precise characterization of interfacial region, demonstrating that the interphase is softer than epoxy and boehmite nanoparticles. Further, we investigated the effect of boehmite nanoparticles on the bulk properties of epoxy matrix. ImAFM stiffness maps revealed the significant stiffening effect of boehmite nanoparticles on anhydride-cured epoxy matrix. The energy Dissipation of epoxy Matrix locally measured by ImAFM shows a considerable increase compared to that of neat epoxy. These measurements suggest a substantial alteration of epoxy structure induced by the presence of boehmite.
Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in weld joints using a thermal conductivity detector (TCD) for hydrogen measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries (ISO 3690 type B and small cylindrical samples), and factors that additionally influence hydrogen determination. They are namely specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PI-furnace controller, as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up to the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by Evaluation of the recorded data. Generally, independent temperature measurement with dummy specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA).
Since the early 19th century microorganisms were studied on their capabilities of causing microbiologically influenced corrosion (MIC) of metals. The most studied ones are sulfate-reducing bacteria (SRB), but others can corrode metals as well, e.g. acid-producing bacteria or methanogenic archaea (MA). However, these studies were mostly focused on metals related to the petroleum industry but metals for other industries, e.g. dentistry, are also susceptible to corrosion. The inert Titanium (Ti) is often used as an implant material, but it is a base metal. The formation of a passivating oxide layer allows Ti to be corrosion resistant at normal conditions.
Nonetheless, scanning electron microscope images on dental implants from patients with acute peri-implantitis showed clear signs of corrosion. Currently, the corrosion mechanism of dental implants is unknown, but many indications suggest that oral microorganisms, including MA (Methanobrevibacter oralis) and SRB (Desulfomicrobium orale), could be involved.
To determine if MA or SRB can corrode Ti (pure Ti or Ti-6Al-4V alloy), corrosion rate, methane and sulfide concentrations were analyzed. Electrical potential measurements using in-house developed electrochemical cells indicated a potential change on Ti in the presence of a corrosive MA strain compared to an abiotic control.
Microbial composition comparison will be analyzed using samples from dental pockets of 150 infected patients by considering the quality of the implant and 50 healthy people by means of amplicon sequencing. Enrichments and isolation of pure cultures from the dentals samples are also examined for their corrosion behavior. Overall, this is the first study investigating the susceptibility of dental implant material to corrosion using human related MA.
In the present study, the susceptibility to HAC of the HSLA steel S960QL with same type of filler material was investigated. For that purpose, both Conv. A and Mod. SA were used with same weld heat input at different deposition rates. For assessment of the HAC susceptibility, the externally loaded Implant-test [ ] was used. Both conducted test series with Conv. A and Mod. SA showed similar crack critical stress of about 280 MPa. Below this value, no delayed fracture appeared. The welds with Mod. SA showed higher hydrogen concentrations. The fracture occurred in the heat-affected zone (HAZ) or in the weld metal (WM). But in all specimens, cracks initiated at the notch root of the spiral notch of the implants within the coarse-grained HAZ. However, the test series with Mod. SA showed a significant extension of the time-to-failure of several hours compared to tests carried out with Conv. A, see Fig. 1a. The reason is the deeper weld penetration in case of Mod. SA (Fig. 1b and Fig. 1c), which causes longer diffusion path for hydrogen. The fracture topography of the ruptured implant specimens with Conv. A was typical ductile in specimen center and quasi-cleavage like at the edge of the specimens. When using Mod. SA, the topography changed to primarily quasi-cleavage fracture topography with shares of intergranular fracture and secondary crack appearance.
Die Verwendung von LTT-Zusatzwerkstoffen stellt einen alternativen Ansatz zu den sonst üblichen Verfahren der Schweißnahtnachbehandlung zur Schwingfestigkeitserhöhung geschweißter Stahlkonstruktionen dar. Der wesentliche Wirkmechanismus beruht auf der Beeinflussung des Eigenspannungszustands durch die niedrige Martensitstarttemperatur bereits während des Schweißens. Dadurch werden die Druckeigenspannungen aus der behinderten Volumenausdehnung infolge Phasenumwandlung voll wirksam. Weiter weist die Schweißnaht eine hohe Härte auf, die die Schwingrissbildung verzögern kann, allerdings auch zu einer niedrigen Kerbschlagarbeit führt.
Im ersten Teil dieses Beitrages werden grundlegende Untersuchungen zur schweißtechnischen Verarbeitung eines LTT-Zusatzwerkstoffes präsentiert. Dies beinhaltet zunächst die Sicherstellung der Schweißbarkeit sowie die Charakterisierung der Schweißgefüge und deren Härte mit dem Ziel, reproduzierbare Verbindungseigenschaften für die nachfolgende Schwingfestigkeitsprüfung herzustellen.
Der zweite Teil des Beitrages beschäftigt sich mit den dazugehörigen Schwingfestigkeitsuntersuchungen an den Stählen S355J2 und S960Q unter Verwendung konventioneller Zusatzwerkstoffe im Vergleich zum LTT-Zusatz.
Das verwendete Schweißdetail ist eine Verbindungsschweißung am Stumpfstoß unter Variation der Schweißnahtausführung (DY-Naht und V-Naht). Weitergehend wird eine bauteilähnliche Probe (die Längssteife) untersucht, bei der der LTT-Zusatzwerkstoff als zusätzliche Schweißlage aufgebracht wurde. Neben der Schwingfestigkeit werden die Schweißnähte hinsichtlich der Eigenspannungen, der Eigenspannungsstabilität im Schwingversuch sowie metallografisch charakterisiert. Die Ergebnisse zeigen, dass LTT-Zusatzwerkstoffe unter Einhaltung wesentlicher Konstruktionsrichtlinien zu einem deutlichen Anstieg der Schwingfestigkeit führen. Dadurch kann das Leichtbaupotential hochfester Stahlgüten genutzt werden.
This book provides a comprehensive and thorough guide to those readers who are lost in the often-confusing context of weld fatigue. It presents straightforward information on the fracture mechanics and material background of weld fatigue, starting with fatigue crack initiation and short cracks, before moving on to long cracks, crack closure, crack growth and threshold, residual stress, stress concentration, the stress intensity factor, J-integral, multiple cracks, weld geometries and defects, microstructural parameters including HAZ, and cyclic stress-strain behavior. The book treats all of these essential and mutually interacting parameters using a unique form of analysis.
Laminography is a widely used NDT technique for large flat object which cannot be investigated by traditional computed tomography. However, due to the limited scanning angle of laminography, the reconstructed image has more artifact interference, which seriously affects the reconstructed image quality. Reducing artifacts of the laminography image and enhancing the images have become important research effort. In this paper, we present dual-energy materials characterization methods based on photon counting detectors to reduce artifacts and enhance image for laminography. The photon counting detector used in this study allows the setting of two independent energy thresholds in order to acquire dual-energy images for laminography from a single scan. The dual energy imaging methods of basis material decomposition (BMD) and weighted logarithmic subtraction (WLS) were studied in the paper with respect to laminography image enhancement. A fast decomposition algorithm on laminographic projection domain with approximating the inverse dual-energy equations to calculate the thickness of basic materials was used in the BMD dual-energy imaging methods. The experimental results show that the BMD method can characterize materials and enhance features of the basic material within the laminographic dataset. In the WLS method, a linear operation was applied on dual-energy images reconstruction directly, which can eliminate the attenuation of one specific material in the resultant image by setting an appropriate weighting factor. In our experiments. WLS method was used successfully to eliminate the strong artifacts generated by the special material and enhance the images. Dual-energy materials characterization methods based on photon counting detectors show potential applications in laminography.
Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here the glass transition and glassy dynamics is considered for epoxy-based nanocomposite with Layered Double Hydroxide nanofiller and for thin films of a misicble polymer blend of PVME/PS with thicknesses down to 7 nm. The materials are investigated by spectroscopic techniques (broadband and specific heat spectroscopy), as well as by fast scanning calorimetry and small- and wide-angle X-ray scattering.
For inorganic/polymer nanocomposites a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate into the entire system, affecting the overall nanocomposite properties. A combination of two relaxation spectroscopy techniques (Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS) in a form of Temperature Modulated DSC (TMDSC)) as well as Fast Scanning Calorimetry (FSC) was employed to investigate the structure and molecular mobility of nanocomposites based on Epoxy and Layered Doubled Hydroxides with different nanoparticle content.
First, BDS investigations proved the existence of a process, which is present only for nanocomposites, assigned to the dynamics of polymer segments within RAF. Second, the amount of RAF was quantified by analyzing the change of specific heat capacity step of nanocomposites, comparing to the pure material.
Thirdly, the glass transition of nanocomposites was studied with FSC, applying high heating rates (500-10 000 K/s). Considering that all techniques probe essentially the same molecular process, an activation plot was constructed, delivering a complete picture of the molecular mobility and structure of the polymer nanocomposites including RAF.
Die warmfeste austenitische Gusseisenlegierung EN-GJSA-XNiSiCr35-5-2 (häufig auch als Ni-Resist D-5S bezeichnet) wurde hinsichtlich ihres mechanischen Verhal-tens bei hoher Temperatur charakterisiert. Dazu wurden (isotherme) niederzyklische (LCF-) und (nicht-isotherme) thermomechanische Ermüdungsversuche (TMF) zwischen Raumtemperatur und 900 °C durchgeführt. Diese Ergebnisse dienten (zu-sammen mit weiteren Versuchsdaten) der Kalibrierung werkstoffmechanischer Modelle. Bei den höchsten Prüftemperaturen wurde Schädigung in Form von Kriechen beobachtet und metallographisch dokumentiert.
Metalle
(2019)
Dieses Standardwerk bietet eine Darstellung der Struktur und Eigenschaften der Metalle und ihrer Anwendungen als Werkstoffe. Im ersten, wissenschaftlichen Teil werden der atomare und mikroskopische Aufbau, die thermodynamischen und die grundlegenden physikalischen und mechanischen Eigenschaften der Metalle beschrieben sowie die Grundlagen der thermisch aktivierten Reaktionen und der Phasenumwandlungen. Die wichtigsten experimentellen Untersuchungsmethoden werden erläutert, wobei die mikroskopischen und Beugungsverfahren einen Schwerpunkt bilden.
Im zweiten, technischen Teil werden die Werkstoffgruppen der Metalle und ihre anwendungsbezogenen Eigenschaften behandelt. Dabei wird auf die zugrunde liegenden Legierungen und die Verfahren zur gezielten Einstellung ihrer Eigenschaften eingegangen. Schwerpunkte bei der Darstellung der Werkstoffe sind die Stähle, die teilchengehärteten Legierungen, die Magnetwerkstoffe und die pulvermetallurgisch hergestellten Werkstoffe. Außerdem werden die Oberflächeneigenschaften und die Verfahren zur Oberflächenbehandlung dargestellt.
Overview about the surface initiated microstructure formation in glass surfaces. Samples which are exposed to a temperature treatment, can develop a crystalline microstructure above Tg at the surface. These separated crystals can be preferably oriented towards the surface of the sample. First experiments about the origin of these orientation phenomenon as well as the potentially causing mechanisms are presented and discussed within the presentation.
The aim of this research is to study the influence of moisture absorption at low moisture contents on the creep behaviour of an epoxy adhesive in steel bonded joints. Single lap joints were manufactured using high strength steel adherends and a two-component epoxy adhesive. The single lap joints were tested at load Levels corresponding to average lap shear stresses of±5%, 15%, 30% and 45% of the dry lap shear strength in both 40 °C air and 40 °C distilled water. Specimens were not pre-aged to be able to analyse the coupled effect of moisture and loading. The test results show that an increase in the load level resulted in an increase in the instantaneous strain and in the creep strain rate. The creep strain of single lap joints loaded in water was generally larger than for the ones loaded in air. For joints loaded in water the creep behaviour was found to be dependent on the moisture concentration in the adhesive. At low moisture percentages creep was suppressed, resulting in a lower instantaneous strain. At higher moisture percentages creep was promoted, resulting in a larger strain rate. The suppression of creep at low moisture percentages is attributed to water molecules bonding to the epoxy macromolecules, resulting in a reduction in molecular mobility and a smaller creep strain. At higher moisture percentages the plasticizing effect of the water dominates, resulting in a larger creep strain. The Maxwell threeelement solid model and Kelvin-Voigt three-element solid model were used to simulate the creep behaviour of the single lap joints loaded in air and water. The models gave good representations of the creep Response across the different load levels in both water and air, they were however unable to give a correct representation of the instantaneous strain of the single lap joints loaded in water. This is attributed to the models being unable to account for the present short-term relaxation process that is dependent on the moisture concentration.
Ergebnisse aus dem AiF Forschungsvorhaben IGF 18823 N/1 "Optimierung von Korundschleifprozessen"
Ein Referenzwerkstoff mit einem definierten Oberflächenzustand wurde zunächst umfassend mittels elektrochemischer Korrosionsuntersuchungen, KorroPad-Untersuchungen und oberflächenanalytischer Verfahren charakterisiert. Anhand definierter Schleifversuche an diesem Referenzzustand wurden anschließend verschiedene Schleifparameter variiert, deren Auswirkungen auf die Korrosionsbeständigkeit mit den gleichen Methoden beurteilt wurden. Somit war es möglich, den Einfluss einzelner Schleifparameter auf das Korrosionsverhalten aufzuzeigen.
Elektrochemische Messungen sind für eine moderne Korrosionsforschung und –prüfung unverzichtbar. Aus dem Verständnis der Grundlagen können durch gezielte Modifizierung der Versuchsbedingungen unterschiedliche Fragestellungen beantwortet werden, wodurch bestehende Grenzen der Anwendung immer wieder verschoben werden können. Außerhalb etablierter Anwendungen stellen Auswahl und Einsatz geeigneter Verfahren sowie die Interpretation der Ergebnisse eine anspruchsvolle Aufgabe dar, die zwingend eine ausgewiesenen Fachexpertise voraussetzen.
The phase behavior and molecular ordering of hexakishexyloxy triphenylene (HAT6) DLC under cylindrical nanoconfinement is studied utilizing differential scanning calorimetry (DSC) and dielectric spectroscopy (DS), where cylindrical nanoconfinement is established through embedding HAT6 into the nanopores of anodic aluminum oxide membranes (AAO), and a silica membrane with pore diameters ranging from 161 nm down to 12 nm. Both unmodified and modified pore walls were considered, and in the latter case the pore walls of AAO membranes were chemical treated with n octadecylphosphonic acid (ODPA) resulting in the formation of a 2.2 nm thick layer of grafted alkyl chains. Phase transition enthalpies decrease with decreasing pore size, indicating that a large proportion of the HAT6 molecules within the pores has a disordered structure, which increases with decreasing pore size for both pore walls. In the case of the ODPA modification the amount of ordered HAT6 is increased compared to the unmodified case. The pore size dependencies of the phase transition temperatures were approximated using the Gibbs Thomson equation, where the estimated surface tension is dependent on the molecular ordering of HAT6 molecules within the pores and upon their surface. DS was employed to investigate the molecular ordering of HAT6 within the nanopores. These investigations revealed that with a pore size of around 38 nm, for the samples with the unmodified pore walls, the molecular ordering changes from planar axial to homeotropic radial. However, the planar axial configuration, which is suitable for electronic applications, can be successfully preserved through ODPA modification for most of the pore sizes.
We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics.
Dense ZnO films with a strong c‐axis texture have been deposited on transparent conductive oxide glass, glass, and Si wafers, respectively, with a two‐step pressureless wet chemical method using zinc acetate dihydrate as Zn‐precursor. The crystallographic structure of the films has been studied with XRD and scanning electron microscopy. Optical measurements reveal a high transparency of the ZnO films with a thickness of up to 10 μm. This new cost‐effective route for ZnO film deposition does not require expensive sophisticated equipment and is easily upscaled.
Broadband dielectric spectroscopy in the frequency range from 10-1 to 109 Hz is employed to revisit the segmental dynamics of the miscible blend system poly(vinyl methyl ether)/polystyrene (PVME/PS) in dependence on the composition firstly in the bulk state. Here especially the case of high polystyrene concentrations is considered. It is important to note that only the molecular dynamics of PVME segments as affected by PS is observed because the dipole moment of polystyrene is negligible. Three relaxation processes are found which are due to fluctuations of differently constrained or confined PVME segments. The degree of the confinement of PVME segments due to PS is discussed in dependence on the composition.
Further a spatial confinement is considered by investigating thin films of the PVME/PS blend where the film thickness was varied from 100 nm down to 5 nm. Two concentrations of PVME/PS (50/50 wt% and 25/75 wt%) are investigated. To measure nanometer thick films a novel electrode system based on nanostructured electrodes was employed. Nanostructured electrodes can be considered as a cut-edge technology in dielectric spectroscopy. The relaxation spectra of the films showed multiple processes which are discussed in dependence on the film thickness.
This book provides a state‐of‐the‐art overview on the processing, characterization, and modelling of metallic and ceramic materials used for energy and environmental applications. 17 scientists show a collection of current knowledge in 8 chapters.
This book fulfills its intention to provide a reference book containing a collection of publications on thin films and coatings made of ceramic and metals used for energy and environmental applications. It covers a broad range of this topic and provides a comprehensive insight. Graduate and undergraduate students of materials science and mechanical engineering can find an overview on this topic to step in this interesting field of engineering.
The molecular mobility of the highly asymmetric miscible blend poly(vinyl methyl ether)/polystyrene was investigated by broadband dielectric (frequency range 10^-1 Hz – 10^9 Hz) and specific heat spectroscopy (frequency range 10^1 Hz – 10^4 Hz). The dielectric spectra revealed a complex molecular dynamic behavior, where three different relaxation processes were observed. At temperatures below the glass transition temperature an α´-relaxation was found, with an Arrhenius-like temperature dependence of its relaxation rates. It is assigned to localized fluctuations of the confined PVME segments within a frozen glassy matrix dominated by PS. Above the thermal glass transition temperature two processes with a VFT behavior of their relaxation rates were detected called α1- and α2-relaxation, both originating from PVME dipoles fluctuating in PS-rich environments, however with diverse PS concentrations. The relevant length scales for the processes are assumed to be different, corresponding to the Kuhn segment length for the former relaxation and to the CRR for the latter one. The observed multiple glassy dynamics result from spatial local compositional heterogeneities on a microscopic level. Additionally, SHS investigations were performed for the first time for this system, proving an existence of a fourth relaxation process (α3-relaxation) due to the cooperative fluctuations of both PS and PVME segments. The separation between the thermal α3- and dielectric α2-relaxation increases dramatically with increasing polystyrene concentration, proving that the thermal response is dominated by PS.
The industrial use of ultrashort laser pulses has made considerable progress in recent years. The reasons for this lie in the availability of high average powers at pulse repetition rates in the several 100 kHz range. The advantages of using ultrashort laser pulses in terms of processing precision can thus be fully exploited. However, high laser intensities on the workpiece can also lead to the generation of unwanted X-rays. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose can become significant for high-repetition-rate laser systems so that X-ray exposure safety limits must be considered. The X-ray emission during ultrashort pulse laser processing was investigated for a pulse duration of 925 fs at 1030 nm wavelength and 400 kHz repetition rate. Industrially relevant materials such as steel,aluminum and glass were treated. Tungsten served as reference. X-ray spectra were recorded, and X-ray dose measurements were performed for laser treatment in air. For laser intensities > 2 × 10^13 W/cm2, X-ray doses exceeding the regulatory exposure limits for members of the public were found. Suitable X-ray protection strategies are proposed.
The impact of polyaniline in phosphorus flame retardant ethylene-propylene-diene-rubber (EPDM)
(2019)
Usually elastomers are loaded with high amounts of flame retardants to fulfill fire safety requirements. In this study the potential char precursor polyaniline (PANI) and the established fire retardant pentaerythritol (PER) were implemented in ethylene-propylene-diene monomer rubber (EPDM). PANI and PER were used in low loadings (7 phr) and combined with two phosphorous flame retardants, Ammonium polyphosphate (APP) and a piperazine-pyrophosphate/phosphoric acid compound (FP), to boost their performance. A comprehensive study is presented, explaining the impact of PANI on curing and mechanical properties, including compensation for the plasticizer-like effect of APP in EPDM, and improved flame retardancy. In the cone calorimeter test, the combination of EPDM/FP/PANI reduced the effective heat of combustion by 20%. All nine EPDM rubber compounds were investigated with the LOI and UL 94 tests, cone calorimeter, FMVSS 302 and glow wire testing to quantify fire performance. The PANI containing EPDM rubbers, EPDM/APP/PANI and EPDM/FP/PANI outperformed the corresponding PER containing, EPDM/APP/PER and EPDM/FP/PER rubbers in various tests. Moreover, the study investigated the impact of PANI and PER on the mode of action of the phosphorus species and showed that the addition of PANI increased the amount of phosphorus in the condensed phase. To receive a broader understanding of the flame retardant mode of action of PANI in combination with APP and FP, calculations were carried out to estimate the impact of PANI on the protective layer effect.
Flow-back and produced waters from shale gas and shale oil fields contain high ammonium, which can be formed by methanogenic degradation of methylamines into methane and ammonium. Methylamines are added to fracturing fluid to prevent clay swelling or can originate from metabolism of the osmolyte triglycinebetaine (GB).
We analyzed field samples from a shale gas reservoir in the Duvernay Formation and from a shale oil reservoir in the Bakken formation in Canada to determine the origin of high ammonium. Fresh waters used to make fracturing fluid, early flow-back waters, and late flow back waters from the shale gas reservoir had increasing salinity of 0.01, 0.58, and 2.66 Meq of NaCl, respectively. Microbial community analyses reflected this fresh water to saline transition with halophilic taxa including Halomonas, Halanaerobium, and Methanohalophilus being increasingly present. Early and late flow-back waters had high ammonium concentrations of 32 and 15 mM, respectively.
Such high concentrations had also been found in the Bakken produced waters.
Enrichment cultures of Bakken produced waters in medium containing mono, di-, or trimethylamine, or triglycinebetaine (GB) converted these substrates into ammonium (up to 20 mM) and methane. The methylotrophic methanogen Methanohalophilus, which uses methylamines for its energy metabolism and uses GB as an osmolyte, was a dominant community member in these enrichments. Halanaerobium was also a dominant community member that metabolizes GB into trimethylamine, which is then metabolized further by Methanohalophilus. However, the micromolar concentrations of GB measured in shale reservoirs make them an unlikely source for the 1,000-fold higher ammonium concentrations in flow-back waters. This ammonium either originates directly from the reservoir or is formed from methylamines, which originate from the reservoir, or are added during the hydraulic fracturing process. These methylamines are then converted into ammonium and methane by halophilic methylotrophic methanogens, such as Methanohalophilus, present in flow-back waters.
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.
Additive Fertigung hat in den letzten Jahren aufgrund der hohen Flexibilität stark an Bedeutung gewonnen. Insbesondere in der Luft- und Raumfahrttechnik werden hohe Anforderungen an die Qualitätskontrolle additiv gefertigter Bauteile gestellt. Teile die mit dem selektiven Laserschmelzen (SLM) hergestellt werden, bilden schon währen des Fertigungsprozesses Poren oder Risse aus. Aus diesem Grund ist die zerstörungsfreie Prüfung jedes Bauteils notwendig. Erste Versuche haben gezeigt, dass die ex-situ Wirbelstromprüfung von SLM-Bauteilen mit hochauflösenden MR Sonden möglich ist und dass Fehler im Bereich von einiger µm detektiert werden können. In dem Vortrag wird eine automatisierte in-situ Wirbelstromprüfung von SLM-Bauteilen vorgestellt. Für die Prüfung wird eine Vielzahl hochauflösender MR Sensoren verwendet, um die benötige hohe Ortsauflösung bei gleichzeitig kurzer Prüfzeit zu erreichen. Zusätzlich werden klassische Methoden der Signalverarbeitung verwendet, um die Kosten und die Komplexität des Systems trotz hoher Prüffrequenz zu minimieren. Das vorgestellte System kann in der Zukunft helfen automatisiert Prüfberichte zu generieren, den SLM-Prozess zu kontrollieren oder automatisiert Fehlstellen auszuheilen.
Der Vortrag widmet sich der „CAT-TECHNOLOGIE ZUR BESTIMMUNG DER HAFTFESTIGKEIT DÜNNER SCHICHTEN“ und beschreibt die Punkte „Motivation –CAT-Technologie“ (CAT: Centrifugal Adhesion Testing) und die „Haftfestigkeit von Schichten“, (Ag-Schichten auf N-BK7 Glas, Cr- und Al-Schichten auf Borofloat 33 Glas, Au-Schichten auf N-BK7 Glas und SiO2-Schichten auf CR39 Polymer) im Einzelnen.
A comparison of tributyltin chloride, dibutyltin dichloride,and butyltin trichloride as catalysts of ring-opening polymerizations(ROPs) of l-lactides at 160°C in bulk reveals increasing reactivity in the above order, but only the least reactive catalysts, Bu3SnCl, yield a uniform reaction product, namely cyclic poly(L-lactide)s with weight average molecular weights (Mw ́s) in the range of 40,000–80,000. A comparison of dimethyltin , dibutyltin , and diphenyltin dichlorides resulted in the following order of reactivity: Me2SnCl2<Bu2SnCl2<<Ph2SnCl2. In this series also, the most reactive catalyst yields cyclic polylactides, but the extent of cyclization varies with the molecular weight. The formation of cyclic polylactides is explained by ROP combined with simultaneous polycondensation involving end-to-end cyclization (ROPPOC method). ROP of meso-lactide at 80 or 60°C yields even-numbered linear chains as main products, a result supporting the ROPPOC mechanism.
Virtual CT acquisition and reconstruction of complex and noisy scanning trajectories in aRTist
(2019)
In modern CT imaging, simulation has become an important tool to minimize cost- and time-intensive measurements. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. We extended the CT simulation software ‘aRTist’ with a module to set-up arbitrary trajectories including disturbing influences during the scan. Moreover, such geometric deviations can be compensated by the internal reconstruction tool.
Die Untersuchung von Schallausbreitung in periodischen Strukturen ist aktuell von großem Interesse für eine zielgerichtete Beeinflussung von Schallwellen in einem großen Frequenzbereich. Hierbei liegt der Fokus insbesondere auf den phononische Kristalle (PnK’s), einer periodischen Anordnung von Streuzentren in einer Matrix. PnK’s können neben anderen Anwendungen, wie der Sensoranwendung oder der Nutzung als effektiver Wellenleiter, als Schallisolator dienen. In dieser Arbeit wird ein neuartiger PnK aus einer periodischen Anordnung von Zylindern untersucht, welcher zur Schallisolation verwendet werden kann. Zunächst wird die Struktur simuliert, dabei wird ein achsensymmetrisches Modell mit einem 3D-Modell verglichen. Im Anschluss wird die simulierte Geometrie gefertigt und vermessen.
Presentation of latest develeopements regarding conformity assessments of pyrotechnic articles within the forum of notified bodies according to article 37 of the EU Directive 2013/29/EU OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL of 12 June 2013 on the harmonisation of the laws of the Member States relating to the making available on the market of pyrotechnic articles (recast).
Polymeric core-shell particles were synthesized in a semi-batch emulsion polymerization process. The shell of the particles consist of PVDF with a high amount of beta-phase. Small-angle X-ray scattering (SAXS) was used to quantify the size of the cores of the particles and the thickness of the shell.
Der Vortrag widmet sich der „ CAT-TECHNOLOGIE ZUR BESTIMMUNG DER KLEBFESTIGKEIT“ und beschreibt die Punkte „Motivation –CAT-Technologie (Centrifugal Adhesion Testing), Klebfestigkeit ( Materialscreening verschiedener Werkstoffklassen, Klebstoffscreening fürV2A gegenV2A als Referenz, Klebstoffscreening für Niedrigenergie-Polymere und Oberfächenmodifizierung von Niedrigenergie-Polymeren) und Verbundfestigkeit (“Stirnabzug vs. Zug-Scher-Prüfung an CFK) im Einzelnen.
Defects as a root cause of fatigue failure of metallic components. II: Non-metallic inclusions
(2019)
This second part of the review on defects as root cause of fatigue failure comprises the origin, the nature and the effects of non-metallic inclusions. Topics addressed are the different kinds of inclusions formed during the manufacturing process, various types of mis-match causing local stresses and, as a consequence, fatigue crack initiation, and effects of characteristics such as size, morphology, localization, spatial distribution and orientation of the defects on the fatigue behavior. Methods for inclusion counting and sizing are discussed along with statistical aspects necessary to be considered when evaluating structural components.
Aktuell werden Prozessmonitoringsysteme in der additiven Fertigung (AM) zur Überwachung der Energiequelle, des Bauraums, des Schmelzbades und der Bauteilgeometrie zumindest im metallbasierten AM schon kommerziell angeboten. Weitere Verfahren aus den Bereichen der Optik, Spektroskopie und zerstörungsfreien Prüfung werden in der Literatur als geeignet für die in-situ Anwendung bezeichnet, es finden sich aber nur wenige Berichte über konkrete Umsetzungen in die Praxis.
Die Bundesanstalt für Materialforschung und -prüfung hat ein neues Projekt gestartet, dessen Ziel die Entwicklung von Verfahren des Prozessmonitorings zur in-situ Bewertung der Qualität additiv gefertigter Bauteile in AM-Prozessen mit Laser- bzw. Lichtbogenquellen ist. Verschiedene Verfahren der zerstörungsfreien Prüfung, wie Thermografie, optische Tomografie, optische Emissionsspektroskopie, Wirbelstromprüfung und Laminografie werden in verschiedenen AM-Prozessen zum Einsatz gebracht und die Ergebnisse fusioniert. Die evaluierten Ergebnisse werden mit Referenzverfahren wie Computertomografie und Ultraschall-Tauchtechnik verglichen. Ziel ist eine deutliche Reduzierung aufwändiger und zeitintensiver, zerstörender oder zerstörungsfreier Prüfungen nach der Fertigung des Bauteiles und zugleich eine Verringerung von Ausschussproduktion.
Hier wird das Projekt als Ganzes vorgestellt und der Fokus auf verschiedene Methoden der Temperaturmessung mit Hilfe der Thermografie gelegt. Anforderungen an die Messtechnik für verschiedene AM-Systeme werden diskutiert und erste experimentelle Ergebnisse werden präsentiert.
The fast and accurate detection of disease-related biomarkers and potentially harmful analytes in different matrices is one of the main challenges in the life sciences. In order to achieve high signal-to-background ratios with frequently used photoluminescence techniques, luminescent reporters are required that are either excitable in the first diagnostic window or reveal luminescence lifetimes exceeding that of autofluorescent matrix components. Here, we demonstrate a reporter concept relying on broad band emissive ternary quantum dots (QDs) with luminescence lifetimes of a few hundred nanoseconds utilized for prolongating the lifetimes of organic or inorganic emitters with lifetimes in the order of a very few 10 ns or less through fluorescence resonant energy transfer. Using spectrally resolved and time-resolved measurements of the system optical response we demonstrate the potential of lifetime multiplexing with such systems exemplarily for AgInS2/ZnS and CdSe/ZnS QDs.
Additive Fertigung hat in den letzten Jahren aufgrund der hohen Flexibilität stark an Bedeutung gewonnen. Insbesondere in der Luft- und Raumfahrttechnik werden hohe Anforderungen an die Qualitätskontrolle additiv gefertigter Bauteile gestellt. Teile die mit dem selektiven Laserschmelzen (SLM) hergestellt werden, bilden schon währen des Fertigungsprozesses Poren oder Risse aus. Aus diesem Grund ist die zerstörungsfreie Prüfung jedes Bauteils notwendig. Erste Versuche haben gezeigt, dass die ex-situ Wirbelstromprüfung von SLM-Bauteilen mit hochauflösenden MR Sonden möglich ist und dass Fehler im Bereich von einiger µm detektiert werden können. In dem Vortrag wird eine automatisierte in-situ Wirbelstromprüfung von SLM-Bauteilen vorgestellt. Für die Prüfung wird eine Vielzahl hochauflösender MR Sensoren verwendet, um die benötige hohe Ortsauflösung bei gleichzeitig kurzer Prüfzeit zu erreichen. Zusätzlich werden klassische Methoden der Signalverarbeitung verwendet, um die Kosten und die Komplexität des Systems trotz hoher Prüffrequenz zu minimieren. Das vorgestellte System kann in der Zukunft helfen automatisiert Prüfberichte zu generieren, den SLM-Prozess zu kontrollieren oder automatisiert Fehlstellen auszuheilen.
Subsurface residual stresses (RS) were investigated in Ti-6Al-4V cuboid samples by means of X-ray synchrotron diffraction. The samples were manufactured by laser powder bed fusion (LPBF) applying different processing parameters, not commonly considered in open literature, in order to assess their influence on RS state. While investigating the effect of process parameters used for the calculation of volumetric energy density (such as laser velocity, laser power and hatch distance), we observed that an increase of energy density led to a decrease of RS, although not to the same extent for every parameter variation. Additionally, the effect of support structure, sample roughness and LPBF machine effects potentially coming from Ar flow were studied. We observed no influence of support structure on subsurface RS while the orientation with respect to Ar flow showed to have an impact on RS.We conclude recommending monitoring such parameters to improve part reliability and reproducibility.
T92 steel was oxidized at 650 °C for 1000 h in dry and wet oxyfuel gases. The microstructure of inner oxide layer was investigated using scanning transmission electron microscopy and energy dispersive spectroscopy on thin lamellas of oxide cross-sections. The oxides were composed of fine equiaxed grains and separated into Fe-rich and Cr-rich regions. Fe-rich regions were wustite and iron sulphide while Cr-rich regions consisted of Fe-Cr spinel with different stoichiometries. Precipitates of (W,Mo)-rich oxides were formed within the oxide scale and beneath the oxide/alloy interface. Often iron sulphide and (W,Mo)-rich oxide were surrounded by Cr-rich spinel.
Wepresent here a systematic analysis of the influence of Tm3+ Doping concentrations (xTm) on the excitation power (P)-dependent upconversion luminescence and -performance of hexagonal-Phase NaYF4: 20% Yb3+, xTm%Tm3+ upconversion nanoparticles (UCNPs) for xTm of 0.2, 0.5, 0.8, 1.2, and 2.0, respectively. Our results reveal the influence of these differentTm3+ doping concentrations with respect to optimized upconversion quantum yield (ΦUC) values of the variousTm3+ upconversion emission bands, with the highestΦUC values of theTm3+ emission bands above 700 nmresulting for different xTm values as theTm3+ emission bands below 700 nm. This underlines the potential ofTm3+ dopant concentration for colour tuning. Special emphasis was dedicated to the spectroscopic parameters that can be linked to the (de)population pathways of the variousTm3+ energy levels, like the P- and xTm-dependent slope factors and the intensity ratios of selected emission bands. The evaluation of all parameters indicates that not only energy transfer upconversion-, but also crossrelaxation processes between neighbouringTm3+ ions play a vital role in the (de)population of the excited energy levels of Yb3+, Tm3+ codoped nanocrystals.
We present a series of results that demonstrate that the broadband photoluminescence (PL) of aqueous glutathione-capped Ag−In−S (AIS) nanocrystals (NCs) is an inherent property of each NC, rather than a collective characteristic of an NC ensemble. By analyzing parameters affecting the PL features such as the postsynthesis annealing and the deposition of a passivating ZnS shell, we found no correlation between the spectral width of the PL band of AIS (AIS/ZnS) NCs and the density of the lattice defects. Analysis of the PL spectra of a series of size-selected AIS/ZnS NCs revealed that the PL width of fractionated NCs does not depend on the NC size and size distribution. The PL measurements in a broad temperature window from 320 to 10 K demonstrated that the PL width does not decrease with decreasing temperature as expected for an emission arising from thermally activated detrapping processes. Also, we show that the model of the self-trapped exciton can be versatilely applied to reconstruct the PL spectra of different AIS NCs and can account for the effects typically attributed to variations in defect state energy. Measurements of the PL properties of single AIS/ZnS NCs highlighted the broadband nature of the emission of individual NCs. The presented results show that the broadband PL of ternary NCs most probably does not originate from lattice defects but involves the NC lattice as a whole, and, therefore, by tailoring the NC structure, PL efficiencies as high as those reported for binary cadmium or lead chalcogenide NCs can be potentially reached.
Elastomers are usually reinforced by large amount of fillers like carbon black (CB) or silica in order to improve various mechanical properties, such as Young’s modulus, hardness, tear resistance, abrasion resistance, and gas barrier properties. In recent years, such improvements were also obtained by using nanoparticles at significantly lower filler loadings. Graphene is a twodimensional (2D) sheet of a thickness in the atomic scale, composed of a honeycomb structure of sp2 carbon atoms. Besides significant mechanical reinforcement, graphene harbors the potential to be used as a multifunctional filler, as it can also increase the conductivity and weathering stability of elastomer matrices. Ultraviolet (UV) irradiation and oxidative agents can lead to the degradation of elastomers due to a multistep photooxidative process, including the formation of radicals. Carbon-based fillers have an influence on these reactions, as they can absorb UV radiation and act as radical scavengers.
This chapter summarizes the results of our larger project on multilayer graphene (MLG)/elastomer nanocomposites, previously published, which present a comprehensive case study of MLG as a multifunctional nanofiller in elastomer/graphene nanocomposites. Different elastomeric matrices are compared in order to demonstrate the outstanding impact of MLG as a general benefit. The dependency of this effect on concentration is discussed in detail. Taking into account the key role of dispersion, different mixing procedures are compared, evaluating a facile implementation of graphene nanocomposites into conventional rubber processing. Finally, the most probable commercial uses of MLG nanofillers in combination with conventional CB are studied. The nanocomposites were prepared in the kg scale in order to obtain enough specimens to investigate various properties of the uncured and vulcanized rubbers at the highest quality level, including rheology, curing, morphology, several mechanical properties, abrasion, conductivity, gas permeation, burning behavior, and weathering stability. The structure property relationships are asserted and questioned, for example, by investigating the radical scavenging ability or aspect ratio of the MLG. This chapter illustrates the state of the art of graphene/rubber nanocomposites targeted for commercial mass applications.