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Der Vortrag gibt einen Überblick über die vielfältigen Möglichkeiten der Oberflächenfunktionalisierung mittels Mikro- und Nanostrukturierung durch Ultrakurzpuls-Lasermaterialbeabeitung. Dies schließt eine Diskussion des Phänomens der Laser-induzierten periodischen Oberflächenstrukturen (LIPSS, engl.: Laser-induced Periodic Surface Structures, Ripples), sowie deren Klassifikation und Bildungsmechanismen mit ein. Ein Schwerpunkt der Präsentation liegt auf der Diskussion verschiedener Anwendungsmöglichkeiten der LIPSS in Bereichen der Optik, Fluidik, Tribologie und Medizin, sowie auf einem Ausblick auf die industrielle Skalierbarkeit der LIPSS-Technologie.
Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer showed a deviation for both poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone.
Nanoparticles (NPs) are tiny – around 1 to 100 billionths of a meter – and can have different chemistries and behaviours than the same material of larger size. This property has led to advances in a wide range of industries, but it can also confer toxicity. Size measurements are the main way NPs are identified but a lack of standardised methods for identifying ones with complex shapes has hindered evaluation of their potential harm.
Biofuels, particularly biodiesel, have gained significant attention as an alternative to traditional fossil fuels in recent years. Unlike diesel, which contains hundreds of compounds, biodiesel only contains a few compounds in the C16-C18 carbon chain. However, the use of biodiesel in automobile and transportation applications can result in problems of degradation or even damage in materials. Among the commonly used polymer materials, fluorocarbon (FKM) shows excellent performance and high stability and compatibility towards oil, diesel, ethanol, and other chemicals. FKM is a family of fluorocarbon-based fluoroelastomer materials, which provide excellent high-temperature and chemical stability compared to other elastomers. As a result, FKM is widely used in chemical processes such as petroleum refining, where it is used for sealings, pumps, and other components.
Mechanical stress often accelerates the failure of polymer materials. The aim of this research is to study the interaction between the sealing material FKM and biofuels B10 (heating oil with 10% biodiesel). The mechanical stress test was carried out in a special apparatus. Both mechanical and non-mechanical stress tests were conducted on specimens at 20, 40, and 70 °C for 28 days to document changes in mass, volume, and tensile properties. Both increasing temperature and mechanical stress have a significant effect on the tensile strength of the FKM polymer when exposed to B10. The combination of increasing temperature and mechanical stress induced rupture within 2 h. It was also established that FKM polymer with pre-exposure in B10 survived longer during mechanical stress compared to specimens exposed only to air. With the support of infrared (IR) spectroscopy, we were able to confirm the penetration of B10 into the FKM polymer.
Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy.
Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials.
The Na salt of chloroacetic acid is condensed in suspension. Furthermore,glycolic acid is condensed in bulk or in concentrated solution by means of SnCl2 or 4-toluene sulfonic acid (TSA) as catalysts. The temperatures are varied from 160 to 200°C and the time from 1 to 5 days. Low molar mass cyclic poly(glycolic acid) (PGA) is detected by means of matrix-assisted laser desorption ionization time-of-flight (MALDI TOF) mass spectrometry in most PGAs. A predominance of certain cycles having an even number of repeat units is observed suggesting a thermodynamically favored formation of extended-ring crystals. Extremely high melting temperatures (up to 237.5°C)and high melting enthalpies are found for polycondensations with TSA in 1,2-dichlorobenzene.
Kemnitz et al. developed a fluorolytic route to access metal fluorides 2 such as AlF3 3 and MgF2 4 which possess a high surface area. In aluminium-based systems, the synthetic approach led to amorphous xerogels that can be further converted into Lewis superacids.3 Still, despite zirconium oxide being described as a stronger Lewis acid than other metal oxides 4 zirconium fluoride-based materials have only recently been reported or investigated. 6 In this work we extend the class of amorphous Lewis acidic heterogeneous catalysts to an amorphous ZrF4 that is active in C-F bond activation.
Zirconium chloro fluoride as catalyst for C-F bond activation and HF transfer of fluoroalkanes
(2024)
In this work1, we have successfully synthesised amorphous zirconium chloro fluoride (ZCF), which exhibits medium lewis acidity. In addition to investigating the local coordination sphere around the Zr atoms and the material properties, we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present the first heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
By automatically recording as much information as possible in automated laboratory setups, reproducibility and traceability of experiments are vastly improved. This presentation shows what such an approach means for the quality of experiments in an X-ray scattering laboratory and an automated synthesis set-up.