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Der ultraschnelle Mechanismus der Alken-Hydrosylilierung lässt sich von den Flüssigsiliconen (LSRs) auf VNB-EPDM-Mischungen übertragen. In der Verarbeitung würde diese für VNB-EPDM die Wettbewerbsfähigkeit hinsichtlich realisierbarer kürzester Zykluszeiten und neue Marktsegmente alternativ zu den LSR-Materialien eröffnen, u.a. in speziellen Dichtungsanwendungen. Peroxidisch vernetzte EPDM-Mischungen können in wässrig-sauren und wässrig-alkalischen Medien eine bessere chemische Beständigkeit als LSR-Materialien bieten. Sie sind duch die radikalische Vernetzung in der Kinetik aber im Vergleich zu additionsvernetzbaren Elastomeren als deutlich träger einzustufen. Ein weiterer Aspekt ist die Permeationsbeständigkeit gegenüber Gasen und Lösemitteldämpfen, die in dieser Arbeit näher untersucht worden ist. In dieser Eigenschaft unterscheiden sich VNB-EPDM und LSR deutlich voneinander. Mit der Bestimmung von zeit- und temperaturabhängigen Permeationsraten von n-Hexan-Lösemitteldämpfen erfolgt ein Vergleich beider Elastomerklassen. Auf die Theorie der Gaspermeation und der sogenannten Pervaporation wird grundlegend eingegangen und zusätzlich der weitere Einfluss von Rezepturbestandteilen beleuchtet. Des Weiteren werden stationäre Permeationskoeffizienten für die Lösemittel-Dampf-Evaporation berechnet, indem die Ausprägung des Quelldrucks im Inneren der Elastomerwerkstoffe durch signifikante Volumenquellungen als eigentliche Triebkraft herangeszogen wird.
Palladium-doped silica materials with SiCH3 groups were fabricated by sol-gel method under various calcination atmospheres and membranes were made thereof by coating process. The results showed that air atmosphere can lead to the partial oxidation of metallic Pd0 to PdO while N2 and H2 atmospheres can effectively prevent metallic Pd0 from being oxidized. H2 atmosphere is proved to be a more prominent way to slow down the decomposition of organic SiCH3 group than N2 and air atmospheres. The surface area, micropore volume and porosity of palladium-doped silica membrane material calcined in H2 atmosphere are much higher than those calcined in N2 atmosphere. Compared with N2 atmosphere, the palladium-doped silica membranes calcined in H2 atmosphere showed higher H2 permeability and H2/CO2 selectivity before and after the steam exposure. The apparent activation energy of H2 permeation through the palladium-doped silica membrane calcined under H2 atmosphere (2.51 ± 0.05 kJ/mol) was slightly lower than that calcined under N2 atmosphere (2.84 ± 0.04 kJ/mol). Calcination atmosphere plays some role in membrane performance, which has greater influence on the permeance than on the gas permselectivity. Calcination under H2 atmosphere is well conducive to improve the gas permeance and H2 permselectivity of palladium-doped silica membrane.
Here, we report the continuous peroxide-initiated grafting of vinyltrimethoxysilane (VTMS) onto a standard polyolefin by means of reactive extrusion to produce a functionalized liquid ethylene propylene copolymer (EPM). The effects of the process parameters governing the grafting reaction and their synergistic interactions are identified, quantified and used in a mathematical model of the extrusion process. As process variables the VTMS and peroxide concentrations and the extruder temperature setting were systematically studied for their influence on the grafting and the relative grafting degree using a face-centered central composite design (FCD). The grafting degree was quantified by 1H NMR spectroscopy. Response surface methodology (RSM) was used to calculate the most efficient grafting process in terms of chemical usage and graft yield. With the defined processing window, it was possible to make precise predictions about the grafting degree with at the same time highest possible relative degree of grafting.
Hypothesis
The origin of negative surface charge at water/air interface is still not clear. The most probable origin is specific adsorption of OH− ions. From diffuse layer potential, we can evaluate the surface density of ions in the Stern layer which can be a measure for the specific adsorption of ions and determines whether the surface charge is solely due to the specific adsorption of OH− ions.
Experiments
Equilibrium thickness of foam films of pure water and aqueous solutions of NaCl, HCl, and NaOH was measured as a function of disjoining pressure for water and as a function of concentration for the aqueous solutions at 298.15 K. Quartz-glass cells thoroughly cleaned and immersed in pure water before use were used for the measurement.
Findings
Application of a modified Poisson-Boltzmann equation to the equilibrium film thickness gave the diffuse layer potential and the surface density of ions in the Stern layer. From the concentration dependence of the surface density, it was concluded that not only OH− ions but also Cl− ions and HCO3− and/or CO32− ions adsorb specifically at the water/air interface.
Indium tin oxide (ITO) particle coatings are known for high transparency in the visible, good conductive properties and near-infrared absorption. These properties depend on ITO particle's stiochiometric composition, defects and size. Here we present a method to gradually change ITO particle's optical properties by a simple and controlled laser irradiation process. The defined irradiation process and controlled energy dose input allows one to engineer the absorption and transsmission of coatings made from these particles. We investigate the role of the surrounding solvent, influence of laser fluence and the specific energy dose targeting modification of the ITO particle's morphology and chemistry by stepwise laser irradiation in a free liquid jet. TEM, SEM, EDX, XPS, XRD and Raman are used to elucidate the structural, morphological and chemical changes of the laser-induced ITO particles. On the basis of these results the observed modification of the optical properties is tentatively attributed to chemical changes, e.g. laser-induced defects or partial reduction.
High-performance liquid chromatography is one of the most important analytical tools for the identification and separation of substances. The efficiency of this method is largely determined by the stationary phase of the columns. Although monodisperse mesoporous silica microspheres (MPSM) represent a commonly used material as stationary phase their tailored preparation remains challenging. Here we report on the synthesis of four MPSMs via the hard template method. Silica nanoparticles (SNPs) which form the silica network of the final MPSMs were generated in situ from tetraethyl orthosilicate (TEOS) in the presence of (3-aminopropyl) triethoxysilane (APTES) functionalized p(GMA-co-EDMA) as hard template. Methanol, ethanol, 2-propanol, and 1-butanol were applied as solvents to control the size of the SNPs in the hybrid beads (HB). After calcination, MPSMs with different sizes, morphology and pore properties were obtained and characterized by scanning electron microscopy, nitrogen adsorption and desorption measurements, thermogravimetric analysis, solid state NMR and DRIFT IR spectroscopy. Interestingly, the 29Si NMR spectra of the HBs show T and Q group species which suggests that there is no covalent linkage between the SNPs and the template. The MPSMs were functionalized with trimethoxy (octadecyl) silane and used as stationary phases in reversed-phase chromatography to separate a mixture of eleven different amino acids. The separation characteristics of the MPSMs strongly depend on their morphology and pore properties which are controlled by the solvent during the preparation of the MPSMs. Overall, the separation behavior of the best phases is comparable with those of commercially available columns. The phases even achieve faster separation of the amino acids without loss of quality.
Unter der Zielsetzung der multimodalen, ortsaufgelösten optischen Spektroskopie für die markierungsfreie Charakterisierung biologischer Materialien nach Morphologie und Chemie werden vier Themenschwerpunkte behandelt.
1. Theorie der elastischen / inelastischen Lichtstreuung und laterale Auflösung in der Mikroskopie
2. Erweiterung eines Raman Mikroskops zu einem multimodalen spektralen Imaging System (MSIS) mit Photonenmigrations-Technologie
3. Erweiterung des MSIS zu Super-Resolution Raman Mikroskopie mit einer Festkörper-Immersionslinse
4. Anwendung des entwickelten MSIS auf biologische Materialien
One-pot synthesis of micron partly hollow anisotropic dumbbell shaped silica core-shell particles
(2016)
A facile method is described to prepare micron partly hollow dumbbell silica particles in a single step. The obtained particles consist of a large dense part and a small hollow lobe. The spherical dense core as well as the hollow lobe are covered by mesoporous channels. In the case of a smaller lobe these channels are responsible for the permeability of the shell which was demonstrated by confocal imaging and spectroscopy.
The properties of polyelectrolyte multilayers are ruled by the process parameters employed during self-assembly. This is the first study in which a design of experiment approach was used to validate and control the production of ultrathin polyelectrolyte multilayer coatings by identifying the ranges of critical process parameters (polyelectrolyte concentration, ionic strength and pH) within which coatings with reproducible properties (thickness, refractive index and hydrophilicity) are created. Mathematical models describing the combined impact of key process parameters on coatings properties were developed demonstrating that only ionic strength and pH affect the coatings thickness, but not polyelectrolyte concentration. While the electrolyte concentration had a linear effect, the pH contribution was described by a quadratic polynomial. A significant contribution of this study is the development of a new approach to estimate the thickness of polyelectrolyte multilayer nanofilms by quantitative rhodamine B staining, which might be useful in all cases when ellipsometry is not feasible due to the shape complexity or small size of the coated substrate. The novel approach proposed here overcomes the limitations of known methods as it offers a low spatial sampling size and the ability to analyse a wide area without restrictions on the chemical composition and shape of the substrate.
Herein the optimization of the physicochemical properties and surface biocompatibility of polyelectrolyte multilayers of the natural, biocompatible and biodegradable, linear polysaccharides hyaluronan and chitosan by Hofmeister anions was systematically investigated. We demonstrated that there is an interconnection between the bulk and surface properties of HA/Chi multilayers both varying in accordance with the arrangement of the anions in the Hofmeister series. Kosmotropic anions increased the hydration, thickness, micro- and macro-roughness, and hydrophilicity and improved the biocompatibility of the films by reduction (2 orders of magnitude) of the films stiffness and complete anti-thrombogenicity.