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We present an experimental approach to study the three-dimensional microstructure of gas diffusion layer (GDL) materials under realistic compression conditions. A dedicated compression device was designed that allows for synchrotron-tomographic investigation of circular samples under well-defined compression conditions. The tomographic data provide the experimental basis for stochastic modeling of nonwoven GDL materials. A plain compression tool is used to study the fiber courses in the material at different compression stages. Transport relevant geometrical parameters, such as porosity, pore size, and tortuosity distributions, are exemplarily evaluated for a GDL sample in the uncompressed state and for a compression of 30 vol.%. To mimic the geometry of the flow-field, we employed a compression punch with an integrated channel-rib-profile. It turned out that the GDL material is homogeneously compressed under the ribs, however, much less compressed underneath the channel. GDL fibers extend far into the channel volume where they might interfere with the convective gas transport and the removal of liquid water from the cell.
Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied with simple alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactands, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process
The Collaborative Research Center InPROMPT aims to establish a novel process concept for the hydroformylation of long-chained olefins, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro-emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the temperature and concentration sensitive multi-phase system demands a continuous observation of the reaction to achieve an operational and economically feasible plant operation. For that purpose, we tested the potential of both NMR and Raman spectroscopy for process control assistance. The lab-scale experiments were supported by sampling for off-line GC-analysis as reference analytics. The results of the NMR experiments will be part of another contribution.
As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magnitude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strategies. Therefore, the present project aims to advance the basic understanding of structural relaxation effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces.
Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hydration of glasses. These changes are highly related to the nature of network formers but are affected as well by the counter ions (network modifier). Results of the 1st project part suggest that structural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect.
In the 2nd project stage specific glasses compositions will be investigated to gain an improved understanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the related effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hydrous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temperature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry.
Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors controlling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived.
As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magni-tude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strat-egies. Therefore, the present project aims to advance the basic understanding of structural relaxa-tion effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces.
Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hy-dration of glasses. These changes are highly related to the nature of network formers but are affect-ed as well by the counter ions (network modifier). Results of the 1st project part suggest that struc-tural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect.
In the 2nd project stage specific glasses compositions will be investigated to gain an improved un-derstanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the relat-ed effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hy-drous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temper-ature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry.
Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors con-trolling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived.
In context with Japanese disposal and transport container safety assessment the German Federal Institute for Materials Research and Testing (Bundesanstalt für Materialforschung und -prüfung) per-formed extensive drop test series with prototypes of RAM packages in recent years.
The paper presents two cooperative projects focused on project management, testing performance and experimental results.
In the first project, a full-scale prototype of a package for transport and storage of spent fuel elements with a total mass of 127,000 kg and its reduced-scale model which was similar to the prototype in both geometry and design were drop tested in 9 m and 1 m puncture tests at various drop orientations under regulatory conditions. In context with a corresponding research project the test data was used in combination with numerical methods to investigate the phenomenon of internal cask- content collisions during drop tests. Here, technological gaps between basket or radioactive content and cask body or primary lid can be a reason for significant high dynamic loadings of cask components and its internals due to additional impact interactions in the cask cavity caused by inner relative movement between content and cask. Further investigations were carried out in the field of similarity mechanics comparing experimental drop test data of the full-scale prototype and reduced-scale model in regard to the transferability of package impact response from reduced-scale models to full-scale packages.
In the second project, drop tests with a waste container for intermediate depth disposal were per-formed being contracted by Kobe Steel, Ltd. and a consortium of Japanese electric power plant com-panies. The drop test program comprised three single 8-m drop tests in a specimen’s corner edge orientation. For drop tests according to legal regulations for interim storage or final disposal it is often necessary to use a target which represents the real ground of the storage facility. In such cases the container hits directly onto a well-defined concrete slab on top of the IAEA target. Here, the directly impact target for the drop tests were concrete slabs manufactured in Japan and connected by mortar to the impact pad of the unyielding IAEA target.
Currently at Deutsche Bahn (DB) ultrasonic inspections in maintenance procedures for wheelset axles with a bore hole are, to the greatest possible extent, carried out using automated ultrasonic inspection system. Although the acceptance levels are in accordance with DIN 27201 part 7, the testing results have shown in recent years that in the case of true indications, the effective defect sizes were far below the level of acceptance. Due to this experience it can be assumed that the automated ultrasonic inspection systems are testing substantially more sensitively than required. This increased sensitivity leads to an increase in false indications, generally resulting in the unnecessary demounting of wheelsets. In Research cooperation between Federal Institute for Materials Research and Testing (BAM) and DB the effective flaw detection sensitivity of existing automated ultrasonic inspection system will be determined and the true/false indication ratio optimised. Through systematic investigations with the Probability of Detection method on the existing automated ultrasonic inspection system the results could be directly applied to the optimisation of existing ultrasonic inspections of wheelset axles with a bore hole in maintenance procedures and the level of reliability can be considerably increased.
3-Aminovinylquinoxalines are readily accessible from (hetero)aryl glyoxylic acids or heterocyclic π-nucleophiles by consecutive four- and fivecomponent syntheses in the sense of an activation-alkynylation-cyclocondensation-addition sequence or glyoxylation-alkynylation-cyclocondensation-addition sequence in good yields. The title compounds are highly fluorescent with pronounced emission solvatochromicity and protochromic fluorescence quenching. Time-resolved fluorescence spectroscopy furnishes radiative and nonradiative fluorescence decay rates in various solvent polarities. The electronic structure is corroborated by DFT and TD-DFT calculations rationalizing the observed spectroscopic effects.
In the present study we have investigated whether the effect of water on properties of borate glasses resembles that of alkali oxide. Soda-lime-borate glasses with nominal compositions of x Na2O, 10 CaO, (90-x) B2O3 (x = 5, 15 and 25 mol%) were doped with up to 8 wt.% H2O by processing glass powder + distilled water in platinum capsules in an internally heated gas pressure vessel at 1523 K and 500 MPa. The water content of hydrous glasses was determined by Karl-Fischer titration and near-infrared spectroscopy. The glass transition temperature T-g. was derived from DTA and micropenetration experiments for which the effect of water loss at the surface of the hydrous glasses was studied. Heating glass samples at 10 K min(-1) in the DTA resulted in T-g values which are close to T-12 isokom temperatures confirming the equivalence of enthalpy relaxation and viscous relaxation for borate glasses. For all three glass series it is shown that T-g strongly decreases whereas the liquid fragility strongly increases upon the addition of water. These findings reveal that H2O primarily causes breaking of B-O-B bonds rather than supporting 4-fold coordinated boron as it is well-known for alkali oxides in this concentration range. (C) 2015 Elsevier B.V. All rights reserved.
Condensed-phase mechanisms play a major role in fire-retardant polymers. Generations of development have followed the concept of charring to improve fire properties. Whereas the principal reactions are believed to be known, the specific description for multicomponent systems is lacking, as is the picture across different systems. A two-step approach is proposed in general, and also presented in greater detail. The second step covers the specific reactions controlling charring, whereas the actual reactants are provided in the preceding step. This model consistently incorporates the variety of structureproperty relationships reported. A comprehensive case study is presented on seven phosphorus flame retardants in two epoxy resins to breathe life into the two-step approach.