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Eingeladener Vortrag
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Investigation of fuel cell materials and liquid water transport by means of synchrotron imaging
(2013)
Synchrotron imaging allows addressing various important issues in fuel cell research, for example water distribution and transport. The water distribution in polymer electrolyte membrane fuel cells (PEMFCs) was observed quasi in-situ directly after operation by means of synchrotron tomography. The 3D data set was compared with the tomogram of a dry cell in order to separate the water distribution from cell materials. Engineered transport pathways realized by perforating holes through the gas diffusion layer (GDL) are a recent approach to optimize water transport and cell performance. For some parameter sets a cell performance increase and an improvement of stabilization have already been proven. We present high resolution investigations of the water distribution in perforated GDLs of operating PEMFCs by means of in-situ synchrotron radiography. The surrounding areas of the holes exhibited a distinct hydrophilic character.
Merocyanine–triarylamine bichromophores are readily synthesized by sequentially Pd-catalyzed insertion alkynylation–Michael–Suzuki four-component reactions. White-light emissive systems form upon aggregation in 1 : 99 and 0.1 : 99.9 vol% CH2Cl2–cyclohexane mixtures, ascribed to aggregation-induced dual emission (AIDE) in combination with partial energy transfer between both chromophore units as supported by spectroscopic studies.
Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale
(2020)
Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation.
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Service life of geosynthetics made of polyolefin materials is mainly limited by oxidative degradation. Durability of polyolefin products depend on formulation, morphology resulting from manufacturing, design and particularly on the antioxidants used. Although the fundamental oxidative reactions are known, the complex effect of geosynthetic characteristics and external influences mean that durability assessments require practical tests.
The assessment of oxidative durability involves exposure to accelerating conditions as well as the material characterisation with respect to the state of stabilisation and/or degradation (e.g. by tensile testing and/or oxidation induction time).
The autoclave test developed by BAM for durability assessments of polyolefin geosynthetics is based on the simultaneous application of moderately elevated temperatures (up to 80 degrees Celsius) and elevated oxygen pressures (up to 5.0 MPa) in combination with a surrounding aqueous medium. Thus this test method provides several advantages in comparison to conventional oven testing, especially with respect to test duration, impact of surrounding environment and the potential to differentiate and rank oxidative resistance between products of very different dimensions (surface/volume) and stabilisation.
In view of the increasing demand for durability assessments of geosynthetic products with lifetimes significantly exceeding 25 years, the contribution is focused on practical aspects concerning implementation and optimisation of test procedures, conditions and evaluation of results. Furthermore, advanced approaches based on multiple exposure conditions will also be included and corresponding calculations of expected service life in typical applications will be evaluated with respect to significance and repeatability. Thereby involved standards and recommendations - such as EN ISO 13438, Part C or EAG-EDT - are considered.
Whenever geosynthetics are used to reinforce or stabilise infrastructural elements such as road- and railways, bridge abutments, run- and taxiways on airports or to protect coastlines of canals and other steep slopes they may be exposed to cyclic loads. Therefore, a reduction factor for dynamic effects on the geosynthetic tensile strength has been included into the calculation of the Long Term Design Strength (LTDS). An approach to assess the behaviour of geosynthetics is to adopt Woehler- or Smith graphs and Haigh-diagrams for polymers. This is because an endurance limit for polymers, which defines an infinite life under a defined cyclic load, has not been seen so far. A huge amount of mechanical testing is needed to predict the behaviour of geosynthetics against this particular background.
To reduce these efforts while getting an indication of the cyclic effect on geosynthetics, a combined method of mechanical and chemical analysis has been developed. The pure tensile strength tests to determine the residual strength after cyclic stress has been amended by IR-spectroscopy and Differential Scanning Calorimetry (DSC). In this context the chain change model of PET has been proven as valid for cyclic loads as well, which helps to define the endurance limit of materials made out of PET. For polyolefins such as PP and PE, a limit for the maximum alternating load has been identified at the point of the stress strain graph where the actual and the numerical stress of a material diverge from each other. Cyclic tensile strength tests have been carried out in a hydraulic test frame. The test parameters have been set to simulate the service life of a railway bed trafficked by high speed trains (ICE).
Microstructural aspects of composites such as reinforcement particle size, shape, and distribution play important roles in deformation behavior. In addition, Fe-rich inclusions and porosity also influence the behavior of these composites, particularly under fatigue loading. Three-dimensional (3-D) visualization of porosity and Fe-rich inclusions in three dimensions is critical to a thorough understanding of fatigue resistance of metal matrix composites (MMCs), because cracks often initiate at these defects. In this article, we have used X-ray synchrotron tomography to visualize and quantify the morphology and size distribution of pores and Fe-rich inclusions in a SiC particle-reinforced 2080 Al alloy composite. The 3-D data sets were also used to predict and understand the influence of defects on the deformation behavior by 3-D finite element modeling.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.