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Referierte Publikation
- ja (2037) (entfernen)
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- Additive manufacturing (79)
- Quantum yield (66)
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Paper des Monats
- ja (42)
The increasing demand for energy efficient separation processes fosters the development of new high performance polymers as selective separation layers for membranes. PIM-1 is the archetypal representative of the class of polymers of intrinsic microporosity (PIM) which are considered most promising in this sector, especially for gas separations. Since their introduction, PIMs stimulated a vast amount of research in this field and meanwhile evolved to the state of the art in membrane technology for gas separation. The major obstacle for extending the practical membrane application is their strong tendency to physical aging. For the first time, investigations by broadband dielectric spectroscopy (BDS) addressing molecular dynamics and conductivity in PIM 1 are presented. As chain packing during film formation from the casting solution and physical aging are key factors determining the separation performance of PIMs as membrane materials, characterization of the molecular mobility in such materials as revealed by BDS will provide valuable information for further development and optimization.
A process was developed for graphite particle exfoliation in water to stably dispersed multi-layer graphene. It uses electrohydraulic shockwaves and the functionalizing effect of solution plasma discharges in water. The discharges were excited by 100 ns high voltage pulsing of graphite particle chains that bridge an electrode gap. The underwater discharges allow simultaneous exfoliation and chemical functionalization of graphite particles to partially oxidized multi-layer graphene. Exfoliation is caused by shockwaves that result from rapid evaporation of carbon and water to plasma-excited gas species. Depending on discharge energy and locus of ignition, the shockwaves cause stirring, erosion, exfoliation and/or expansion of graphite flakes. The process was optimized to produce long-term stable aqueous dispersions of multi-layer graphene from graphite in a single process step without requiring addition of intercalants, surfactants, binders or special solvents. A setup was developed that allows continuous production of aqueous dispersions of flake size-selected multi-layer graphenes. Due to the well-preserved sp(2)-carbon structure, thin films made from the dispersed graphene exhibited high electrical conductivity. Underwater plasma discharge processing exhibits high innovation potential for morphological and chemical modifications of carbonaceous materials and surfaces, especially for the generation of stable dispersions of two-dimensional, layered materials.
To study the mechanical interface behavior of single-walled carbon nanotubes (CNTs) embedded in a noble metal, we performed CNT-metal pull-out tests with in situ scanning electron microscope experiments. Molecular dynamics (MD) simulations were conducted to predict force-displacement data during pull-out, providing critical forces for failure of the system. In MD simulations, we focused on the influence of carboxylic surface functional groups (SFGs) covalently linked to the CNT. Experimentally obtained maximum forces between 10 and 102 nN in palladium and gold matrices and simulated achievable pulling forces agree very well. The dominant failure mode in the experiment is CNT rupture, although several pull-out failures were also observed. We explain the huge scatter of experimental values with varying embedding length and SFG surface density. From simulation, we found that SFGs act as small anchors in the metal matrix and significantly enhance the maximum forces. This interface reinforcement can lead to tensile stresses sufficiently high to initiate CNT rupture. To qualify the existence of carboxylic SFGs on our CNT material, we performed analytical investigation by means of fluorescence labeling of surface species and discuss the results. With this contribution, we focus on a synergy between computational and experimental approaches involving MD simulations, nano scale testing, and analytics (1) to predict to a good degree of accuracy maximum pull-out forces of single-walled CNTs embedded in a noble metal matrix and (2) to provide valuable input to understand the underlying mechanisms of failure with focus on SFGs. This is of fundamental interest for the design of future mechanical sensors incorporating piezoresistive single-walled CNTs as the sensing element.
Introducing a single silicon nanowire with a known orientation and dimensions to a specific layout location constitutes a major challenge. The challenge becomes even more formidable, if one chooses to realize the task in a monolithic fashion with an extreme topography, a characteristic of microsystems. The need for such a monolithic integration is fueled by the recent surge in the use of silicon nanowires as functional building blocks in various electromechanical and optoelectronic applications. This challenge is addressed in this work by introducing a top-down, silicon-on-insulator technology. The technology provides a pathway for obtaining well-controlled silicon nanowires along with microstructures up to a three-order-of-magnitude scale difference. A two-step etching process is developed, where the first shallow etch defines a nanoscale protrusion on the wafer surface. After applying a conformal protection on the protrusion, a deep etch step is carried out forming the surrounding microscale features. A minimum nanowire cross-section of 35 nm by 168 nm is demonstrated in the presence of an etch depth of 10 m. All cross-sectional features are characterized via transmission electron microscopy and linked to specific process steps. The technology allows control on all dimensional aspects along with the exact location and orientation of the silicon nanowire.
Epoxy composites used for high-end structural applications are typically cured under the influence of temperature and pressure causing a number of complex chemical and physical transformations. On heating a mould, temperature gradients will occur through the component which will depend largely on the thermophysical properties of the specific composite. The crosslinking reaction is exothermic leading to additional heat release, thus complicating heat transportation models. If such effects are not accounted for, it can lead to variations in resin flow, poor fibre wetting causing voiding and inhomogeneous cure, leading to shrinkage and unfavourable variations in moulded part geometry. Limited information is available for thermal models used in the manufacture of reinforced thermosets. Autoclave [1, 2] and laser or infra-red curing processes [3, 4] typically use constant values determined on fully cured parts. In this work, the variation in thermal conductivity (K) (W/(m K)), thermal diffusivity (a) (m(2)/s) and specific heat capacity at constant pressure (c(p)) (J/(g K) is determined for a carbon fibre prepreg during cure. It is the intention to improve understanding of how these parameters are related to chemical or physical transformations occurring during cure, and where estimates or shortcuts may be used for heat transfer models
Seals used in containers for dangerous goods need to maintain leak tightness for several decades. For investigating the change in seal material properties during aging, a comprehensive aging program on both uncompressed and compressed EPDM and HNBR seals was started. In order to obtain results closely related to practical conditions, O-rings with a full-scale cord diameter of 10 mm were aged. However, this set-up can lead to heterogeneous aging caused by diffusion-limited oxidation (DLO) effects. These effects depend on material, dimensions, time and temperature. Heterogeneous aging results in distorted bulk properties such as compression stress relaxation and compression set (CS) suggesting that HNBR has better performance than EPDM at 150 °C but which is not the case at 100 °C. The presence of heterogeneous material properties was shown by hardness measurements across the seal cross-section. If DLO-affected data is excluded, extrapolations of CS data are possible using time-temperature shifts and Arrhenius graphs. Exemplary CS values of 50 % and 80 % would be reached after approx. 10 years and 29 years, respectively for HNBR and after approx. 400 years and 1100 years, respectively for EPDM.
In this work a novel iterative method for isothermal cure kinetic modelling of an epoxy resin system using differential scanning calorimetry (DSC) technique is presented. To reach the isothermal cure temperature, the sample has to be heated up from ambient temperature. This is commonly done with very high heat-up rates to minimise the time the sample reacts at temperatures other than the desired one. However, during heat up with high heating the amount of released energy rates cannot be measured directly because the shape of baseline is unknown. This means that the cure state at the beginning of the isothermal stage is unknown. For fast curing systems this unknown cure state causes significant inaccuracies in cure kinetics modelling.
The presented iterative approach attempts to estimate the released enthalpy during heat-up of an isothermal run through an iterative numerical modelling of the heat-up phase. In each iteration the algorithm starts by estimating the enthalpy released during heat-up based on the recorded temperature profile and the calibrated model of the previous iteration. At the same time, it estimates the degree of cure at the end of the heat-up phase. Once the initial cure state is known the total heat of enthalpy can be recalculated for the current iteration. Subsequently the degree of cure and curing rate are re-evaluated with the newly estimated total enthalpy and used for determining the kinetics parameters. This is done by simultaneous fitting of the selected model to all experimental heat flow curves using a non-linear nonrestricted multivariable fitting method. The model with these new parameters is used again to estimate the released enthalpy and cure degree during the heat-up phase. The described loop is repeated until a predefined convergence criterion is satisfied.
For modelling the reaction kinetics, the Kamal–Sourour equation accompanied with Rabinowitch approach to consider the diffusion effects is used. The diffusion reaction rate is modelled by the free volume model proposed by Huguenin and Klein. DiBenedetto model is applied to predict the Evolution of glass transition temperature against the degree of cure. In order to compensate the effect of the Initial values in the model’s calibration, the algorithm is implemented in a routine, which assesses the quality of the fitting and consequently selects the cure kinetics parameter. The described algorithm and the Routine are implemented in MATLAB. This paper demonstrates the application of this approach for using cure kinetics modelling to predict the degree of cure and the glass transition temperature. It supports the obtained results with validation tests using isothermal, dynamic and combined temperature profiles.
An electromagnetic weld pool support system for 20 mm thick duplex stainless steel AISI 2205 was investigated numerically and compared to experiments. In our former publications, it was shown how an alternating current (AC) magnetic field below the process zone directed perpendicular to the welding direction can induce vertically directed Lorentz forces. These can counteract the gravitational forces and allow for a suppression of material drop-out for austenitic stainless steels and aluminum alloys. In this investigation, we additionally adopted a steady-state complex magnetic permeability model for the consideration of the magnetic hysteresis behavior due to the ferritic characteristics of the material. The model was calibrated against the Jiles–Atherton model. The material model was also successfully tested against an experimental configuration before welding with a 30 mm diameter cylinder of austenitic stainless steel sur-rounded by duplex stainless steel. Thereby, the effects of the Curie temperature on the magnetic characteristics in the vicinity of the later welding zone were simulated. The welding process was modeled with a three-dimensional turbulent steady-state model including heat transfer and fluid dy-namics as well as the electromagnetic field equations. Main physical effects, the thermo-capillary (Marangoni) convection at the weld pool boundaries, the natural convection due to gravity as well as latent heat of solid–liquid phase transitions at the phase boundaries were accounted for in the model. The feedback of the electromagnetic forces on the weld pool was described in terms of the electromagnetic-induced pressure. The finite element software COMSOL Multiphysics 4.2 was used in this investigation. It is shown that the gravity drop-out associated with the welding of 20 mm thick duplex stainless steel plates due to the hydrostatic pressure can be prevented by the application of AC magnetic fields between around 70 and 90 mT. The corresponding oscillation frequencies were between 1 and 10 kHz and the electromagnetic AC powers were between 1 and 2.3 kW. In the experiments, values of the electromagnetic AC power between 1.6 and 2.4 kW at os-cillation frequencies between 1.2 and 2.5 kHz were found to be optimal to avoid melt sagging or drop-out of melt in single pass full-penetration laser beam welding of 15 and 20 mm thick AISI 2205.
The goal of reducing CO2 emissions in the automobile industry has led to the development of increasingly efficient lightweight material solutions that yield enhanced performance. In light of this goal, this current work involves the optimization of the pre-conditioning of novel, high toughness steel bearings without thermo-chemical treatment, with the aim of transferring the running-in phase into the final step of the mechanical finishing process. A case-hardened gear steel and two novel non-case-hardened steels were evaluated.
Full penetration high power bead-on-plate laser beam welding tests of up to 20 mm thick 2205 duplex steel plates were performed in PA position. A contactless inductive electromagnetic (EM) weld pool support system was used to prevent gravity drop-out of the melt. Welding experiments with 15 mm thick plates were carried out using IPG fiber laser YLR 20000 and Yb:YAG thin disk laser TruDisk 16002. The laser power needed to achieve a full penetration was found to be 10.9 and 8.56 kW for welding velocity of 1.0 and 0.5 m min−1, respectively. Reference welds without weld pool support demonstrate excessive root sag. The optimal value of the alternating current(AC) power needed to completely compensate the sagging on the root side was found to be ≈1.6 kW for both values of the welding velocity. The same EM weld pool support system was used in welding tests with 20 mm thick plates. The laser beam power (TRUMPF Yb:YAG thin disk laser TruDisk 16002) needed to reach a full penetration for 0.5 m min−1 was found to be 13.9 kW. Full penetration welding without EM weld pool support is not possible—the surface tension cannot stop the gravity drop-out of the melt. The AC power needed to completely compensate the gravity was found to be 2 kW.
The determination of material parameters from displacement field measurement is being examined for linear elastic solid. A frequently used approach to compute material constants can be found in many studies. Even though they presented the approach in many different variations, but in the end they are essentially based on the same algorithm: Parameters are iteratively tuned until the computed results are in accordance with the measurements. The main drawback of this approach is that mainly commercial software is used that hinders us to investigate its inner evaluation process. This leads to the question, how the results from this commercial software can be trusted. On the contrary to these debatable approaches, we present a method that inverts the procedure of finite element method by using the most general model for a least-squares adjustment – the GAUSS-HELMERT Model.
Theophylline has been used as an active pharmaceutical ingredient (API) in the treatment of pulmonary diseases, but due to its low water solubility reveals very poor bioavailability. Based on its different hydrogen-bond donor and acceptor groups, theophylline is an ideal candidate for the formation of cocrystals. The crystal structure of the 1:1 benzamide cocrystal of theophylline, C7H8N4O2·-C7H7NO, was determined from synchrotron X-ray powder diffraction data. The compound crystallizes in the tetragonal space group P41 with four Independent molecules in the asymmetric unit. The molecules form a hunter’s fence packing.
The crystal structure was confirmed by dispersion-corrected DFT calculations.
The possibility of salt formation was excluded by the results of Raman and 1H solid-state NMR spectroscopic analyses.
Fischer, Franziska ; Heidrich, Adrian ; Greiser, Sebastian ; Benemann, Sigrid ; Rademann, K. ; Emmerling, Franziska
The liquid-assisted grinding cocrystallisation of theophylline with benzamide leading to polymorphic compounds was investigated. A solvent screening with seventeen different solvents was performed. The dipole moment of the solvent used in the synthesis determines the structure of the polymorphic product. A detailed investigation leads to the determination of the kinetically and thermodynamically favored product. In situ observations of the formation pathway during the grinding process of both polymorphs show that the thermodynamically favored cocrystal is formed in a two-step mechanism with the kinetic cocrystal as intermediate.
Excellent tribological properties of an advanced polymer matrix composite were obtained by a combination of micro- and nano-sized fillers. Surface features and the nanostructure of tribofilms were characterized by advanced microscopic techniques, and correlated with the macroscopic behavior in terms of wear rate and friction evolution. A model based on movable cellular automata was applied for obtaining a better understanding of the sliding behavior of the nanostructured tribofilms. The failure of the conventional composite without silica nanoparticles could be attributed to severe oxidational wear after degradation of an initially formed polymer transfer film. The hybrid composite preserves its antiwear and antifriction properties because flash temperatures at micron-sized carbon fibers, lead to polymer degradation and subsequent release of nanoparticles. It has been shown that the released particles are mixed with other wear products and form stable films at the disc surface thus preventing further severe oxidational wear. Furthermore, the released wear product also is embedding carbon fibers at the composite surface thus preventing fiber fragmentation and subsequent third body abrasion. With nanoscale modelling we were able to show that low friction and wear can be expected if the nanostructured silica films contain at least 10 vol.% of a soft ingredient.
The method of movable cellular automata (MCA) was applied to simulate the stress-strain behavior of a nano composite consisting of an epoxy matrix and 6 vol. % silica nano particles. The size of the elements used for modelling was fixed at 10 nm, corresponding approximately to the diameter of the filler particles. Since not only the stress-strain response of the two constituents but also debonding of neighboring particles and granular flow was taken into account, plastic deformation as well as crack initiation and propagation could be simulated with the model. Modelling results were compared with tensile test results of both, pure epoxy as well as the epoxy-6 vol. % SiO2 composite. Since assuming bulk properties of the two constituents did not yield satisfactory results, slight modifications of the nanoparticle response functions and nanostructures were tested numerically. Finally, it was observed that only the assumption of slightly increased strength properties of the epoxy yielded good correlation between experimental and modelling results. This was attributed to an increased cross linking of the epoxy caused by the presence of silica nano particles.
Plastic products used in geotechnical engineering, so-called geosynthetics, are often made of polyolefins (polyethylene or polypropylene) and stabilized against oxidative degradation by antioxidants (AO). Three types of AO “packages” are used: (P1) phenols and phosphites/sulfides, (P2) hindered amines (HAS) with a marginal stabilization P1 of the basic resin, (P3) a combination of packages P1 and P2 with comparable amounts of phenol and HAS. We report about long-lasting oven aging and water immersion tests at 80 °C of 29 different polyolefin based products (geomembranes, geonets and geotextiles). Pronounced differences in the degradation behavior were found depending solely on the type of AO package. In case of P1, the oxidative degradation is prevented by the AO. Autocatalytic oxidation only begins after depletion of AO and may lead to catastrophic failure depending on the environmental conditions. In case of P2, degradation starts right from the beginning. However, it is decelerated and proceeds gradually. In case of P3, the degradation behavior seems to be a superposition of the characteristics obtained for P1 and P2. Plotting the fractional loss of the AO in P1 and P2 as function of the square root of aging time, we identified two regimes of AO depletion. We suggest to attribute this observation to the different mechanisms of AO depletion.
Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass – thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS.
The presented investigations have proved the principal suitability of the KorroPad method to assess the passive layer stability of stainless steels. The electrochemical mode of action could be described in detail and limitations of the applicability have been demonstrated. The influence of different surface finishes has been investigated and verified by known methods for describing corrosion resistances. As a result, the increased corrosion susceptibility of two ground surfaces has been detected, but also the corrosion resistance of further surface finishes could be confirmed.
An unusually fast and effective synthesis procedure for a host guest system consisting of a metal organic framework (MOF) and a polyoxometalate (POM) is described. The material was synthesised mechanochemically and the evolution of the structure was monitored ex and in situ using synchrotron X-ray diffraction (XRD).
We use a dynamic scanning electron microscope (DySEM) to map the spatial distribution of the vibration of a cantilever beam. The DySEM measurements are based on variations of the local secondary electron signal within the imaging electron beam diameter during an oscillation period of the cantilever. For this reason, the surface of a cantilever without topography or material variation does not allow any conclusions about the spatial distribution of vibration due to a lack of dynamic contrast. In order to overcome this limitation, artificial structures were added at defined positions on the cantilever surface using focused ion beam lithography patterning. The DySEM signal of such high-contrast structures is strongly improved, hence information about the surface vibration becomes accessible. Simulations of images of the vibrating cantilever have also been performed. The results of the simulation are in good agreement with the experimental images.