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Eingeladener Vortrag
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In this study, the molecular dynamics of a series of dipole functionalized triphenylene-based discotics, forming a columnar mesophase, were investigated by broadband dielectric spectroscopy (BDS). In addition to conductivity and localized dynamics, glassy dynamics were also observed. At higher temperatures an α1-processes and at low temperatures an α2 processes were detected having a completely different temperature dependence of its relaxation times. Different molecular assignments of α1- and α2-processes are suggested. The phase behavior of the material was explored under helium purge down to 100 K by differential scanning calorimetry (DSC). Besides the phase transition temperatures and enthalpies, one or two thermal glass transitions were found for all the materials. Moreover, the glassy dynamics were further investigated by Flash DSC, which is a chip-based calorimetry technique allowing for fast heating and cooling rates as high as 10000K/s.
High performance polymers of intrinsic microporosity (PIMs) have emerged as novel materials with broad applications from gas separation to electronic devices. Sufficiently rigid, even contorted polymer chains show only limited molecular mobility, therefore undergo inefficient packing and give rise to intrinsic microporosity with pore size generally smaller than 1 nm and BET surface areas larger than 700 m2/g. Further performance optimization and long-term stability of devices incorporating PIMs rely on our understanding of structure-processing-property relationships and physical aging, in which glass transition plays a key role. Up to now no glass transition temperature (Tg) of PIMs could be detected with conventional thermal analysis techniques before degradation. Decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this. This was achieved by employing fast scanning calorimetry (FSC) based on a chip sensor, which is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. FSC provides definitive evidence of glass transition of a series of PIMs with a special consideration on the chain rigidity. The determined glass transition temperature of these PIMs follows the order of the rigidity of their backbone structures. FSC provides the first clear-cut experimental evidence of the glass transition of PIM-EA-TB with a Tg of 663 K, PIM-1 of 644 K and PIM-DMDPH-TB of 630 K at a heating rate of 1Χ104 K/s. Local fluctuations are featured in glass transition of highly rigid PIMs. As conformational changes are prevented by the backbone rigidity, the glass transition must rather be assigned to local small scale fluctuations.
Ultrashort laser pulse micromachining features a high precision. By increasing the repetition rate of the applied laser to several 100 kHz, laser processing becomes quick and cost-effective and make this method attractive for industrial applications. Upon exceeding a critical laser intensity, hard X-ray radiation is generated as a side effect. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose becomes significant for high-repetition-rate laser systems so that radiation safety must be considered.
In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. Due to the hard accessibility of these layers, their growth kinetics and molecular dynamics are still not fully understood. Here, the irreversibly adsorbed layers of Poly(2-vinylpyridine) (P2VP) and Poly(vinyl methyl ether) (PVME) thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work.
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 to the entire system, affecting the overall nanocomposite properties. A combination of two relaxation spectroscopy techniques (Broadband Dielectric Spectroscopy (BDS) and 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 (0.5-10 kK/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.
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) in offshore industries, such as the oil and gas pipelines, due to the high concentrations of sulfate in the seawater. SRM act upon the metal by the reactiveness of hydrogen sulfide (HS-), and by withdrawal of the available electrons (Fe --> Fe2+ + 2e-; E° = -0.47 V) in electrical contact with the metal (EMIC). However, methanogenic archaea can also cause MIC. Because they do not produce HS-, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood.
To investigate the corrosion potential of methanogens, we studied the EMIC methanogenic strains isolated from marine sediments (Methanobacterium-affiliated strain IM1) and crude oil tanks (Methanococcus maripaludis Mic1c10), in an in-house developed flow-through cell to simulate a fluctuating environment. A co-culture of M. maripaludis and D. alaskensis was also established to study the effect of syntrophic growth on metal corrosion that may occur in industrial pipelines. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.4 mm/yr) are higher to that caused by the marine SRM Desulfovibrio alaskensis (0.15 mm/yr). Surface analyses of the metal showed severe pitting with high methane production. Genomic analysis of the EMIC methanogen M. maripaludis Mic1c10 will provide an insight on the mechanisms of MIC. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC.
Permitted explosives have a tradition of many decades in Germany and had been designed to the needs of the underground coal mining in the Ruhr. In neighboring countries of Germany similar provisions were made to prevent hazards from fire damp and coal dust explosions in underground coal mines. Due to the termination of coal mining in Germany and most other European countries, also the testing facilities are disappearing. This presentation outlines the current situation of testing regimes and facilities.
During a European convention of the authorities for market surveillance (AdCO) for explosives the activities of the notified bodies are presented, putting a focus on matters concerning market surveillance.
The presentation outlined in detail, which verifications are possible
with explosives, while practical tests involving initiation of
explosives are excluded. Elements of labeling and the conclusions in
view of quality control were explained, and typical failures by
manufacturers to comply were orally described.
The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge.
While today, engineers can choose from a wide range of rheology modifying admixtures, in some parts of the world, these are difficult to access, due to their complex processing. However, alternatives can be bio-based polymers such as polysaccharides from various sources. These are easily accessible all over the world, do not demand for complicated processing, and typically they are more sustainable than many established materials, which are crude oil-based.
The paper presents the effects of acacia gum, cassava starch and the gum of triumfetta pendrata A. Rich on the rheological performance of cementitious systems. It is shown that acacia gum can be as efficient as polycarboxylate based superplasticisers, cassava starch can reduce the yield stress slightly with little effect on the plastic viscosity, and the gum of triumfetta pendrata A. Rich increases the thixotropy of cement pastes with plasticizing polymers significantly.
Thermosetting materials are gaining increasing attention in many structural composite applications. However, the incorporation of inorganic nanoparticles (NPs) into polymer matrix is a promising approach to enhance their functional characteristics, and thus, to enable the development of thermosets advanced application. It has been shown that Boehmite Alumina (BA) used as nanofillers can improve different parameters of polymers. This NPs can be easily tailored enabling desirable interactions with a big range of polymers. However, the overall effect of nanofiller depends on many factors, therefore, making it hard to predict the resulted performance of nanocomposites. In the current contribution we would like to discuss the impact of Boehmite NPs on two different epoxy resin nanocomposite systems with the focus on the possible influence mechanisms of this nanofiller.
As the first system, UV curable Cycloaliphatic-Epoxy Oligosiloxane (CEOS) resin/Boehmite nanocomposites were investigated by FTIR, TGA, DSC and T-SEM. It was observed that incorporation of BA leads to the reinforcement of glass transition (Tg) and overall thermal stability indicating the attractive interactions between BA and CEOS network. In addition, an increase in epoxy conversion of CEOS was concluded for nanocomposites assuming that particles are involved in UV polymerisation processes.
The second epoxy/Boehmite nanocomposite is based on the bisphenol-A-diglycidyl ether (DGEBA) cured with methyl tetrahydrophtalic acid anhydride (MTHPA). Thermomechanical as well as nanomechanical properties of this material were investigated by DMTA and IR spectroscopy and the advanced Intermodulation AFM, respectively. In contrast to the first system, it was found that BA leads to a decrease of Tg and crosslink density of the polymer while the young’s modulus of the composite and local stiffness of polymer matrix increase significantly.
As a result, the versatile role of Boehmite was detected depending on the investigated systems. Based on the obtained results, the parameters indicating property-efficient epoxy/Boehmite system are suggested.
Different types of optical spectroscopies are introduced with special emphasis on method-inherent limitations and reliable instrument calibration and performance validation. In addition, procedures for the determination of spectroscopic key parameters like the photoluminescence quantum yield are presented including required instrument calibrations and material-specific effects related to certain emitters.
Surface functionalization of 2D- and 3D-supports and nanomaterials are nowadays at the core of many applications of functional materials in the life and material sciences. Examples range from membranes and microarrays over bead-based assays, immunoseparation, and next generation sequencing to nanometer-sized optical reporters, nanosensors, and magnetic and optical contrast agents. Typically performed functionalization procedures include silanization and grafting reactions with reactive monomers to introduce functional groups like amino or carboxylic acid groups and the attachment of ligands like polyethylene glycol (PEG) molecules and biomolecules such as peptides, proteins, and DNA.[1-3]
We present here a versatile concept to quantify the number of bioanalytically relevant functional groups like carboxyl, amino, and aldehyde moieties through the specific binding and subsequent release of small reporter molecules such as fluorescent dyes and non-fluorescent chromophores utilizing cleavable linkers or the formation of cleavable bonds as a reversible covalent labeling strategy. This is representatively demonstrated for different types of nano- and microparticles with different labeling densities of carboxyl, amino, and aldehyde groups. This strategy enables to separate the signal-generating molecule from the bead surface, thereby circumventing uncertainties associated with light scattering, binding-induced changes in reporter fluorescence, and fluorescence quenching dye-dye interactions on crowded material surfaces.[1-3] Moreover, the reporters are chosen to be detectable with different analytical methods as prerequisite for straightforward validation via method compari-sons and mass balances. Applications of these assays and multimodal cleavable probes range from a quantitative comparison of bead batches and process control to a qualitative prediction of the coupling efficiencies in bioconjugation reactions.
Solidification cracking of metals is a well-researched topic in the field of welding science. A material’s susceptibility to solidification cracking can be tested using numerous different specialized test procedures, one of which is the Modified Varestraint-/Transvarestraint test (MVT). It was developed at BAM in 1982 and is internationally standardised. Over the decades, this test has been extensively used to characterise the solidification cracking resistance of many different materials.
The present study was conducted to further investigate the influences of the standardised MVT testing parameters, as well as the characteristics of evaluation methods on the results. Several different high alloyed martensitic LTT (low transformation temperature) filler materials, CrNi and CrMn type, were used. In previous pilot studies, these alloys have shown a rather distinctive solidification cracking behaviour. During testing, energy input per unit length and bending speed were varied (especially the latter is usually kept at standard values), in addition to the most commonly altered factor - total deformation.
First, the effects of different process parameter sets on the solidification cracking response were measured using the standard approach - microscopic analysis of the specimen surface. It was found that not all parameter changes had the expected outcome. For the Cr8Ni6 and Cr11Mn5 filler materials, influences of energy input per unit length and welding speed were in direct opposition.
In order to investigate those apparent contradictions, μCT scans of MVT specimens were made. The results consistently show sub surface cracking, to significant, yet varying extents. Different primary solidification types were found using WDX-analysis, an aspect that is believed to be the main difference between the CrNi- and CrMn-type materials and their cracking characteristics.
Results show that when it comes to testing of modern high-performance alloys, one set of standard MVT testing parameters might not be equally suitable for all materials. Also, to properly accommodate different solidification types, sub-surface cracking has to be taken into account.
Over the past years economic and environmental considerations have led to a markedly increased demand for efficiency and flexibility in petrochemical plants. The operational temperatures and pressures required today can only be achieved by using new creep-resistant grades of steel. The modified 13CrMoV9-10 vanadium steel shows a good resistance against creep and compressed hydrogen and has been in use for the construction of petrochemical reactors since the mid-1990s. Nevertheless, processing of this type of steel requires extreme care during the welding procedure. This is due to its low toughness and high strength in the welded state when not post weld heat treated combined with increased susceptibility to cracking during stress relaxation. Previous research into crack formation in creep-resistant steels has largely focused on thermal and metallurgical factors; however, little knowledge has been gathered regarding the influence of the welding procedure on crack formation during post weld heat treatment considering real-life manufacturing conditions.
In this work, the influence of heat control on the mechanical properties has been investigated by simulating the real-life manufacturing conditions prevailing during the construction of petrochemical reactors using a special 3-D testing facility. The stresses resulting from preheating, welding, dehydrogenation heat treatment and the final post weld heat treatment were measured during experiments under varied heat control. In all experiments stress relief cracks formed during post weld heat treatment could be observed. The total crack lengths correlated with the stresses due to welding. The application of a special acoustic emission analysis indicated that the cracks formed during post weld heat treatment in a temperature range between 300 °C and 500 °C. In comparison to small scale samples welded without additional shrinkage restraint, the toughness of the restrained welds was significantly decreased. SEM and TEM analyses of all samples revealed accelerated aging due to early precipitation of special carbides during post weld heat treatment under component relevant restraint.
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.
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.
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.
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.