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- ItemViscoelastic and self-healing behavior of silica filled ionically modified poly(isobutylene-co-isoprene) rubber(London : RSC Publishing, 2018) Sallat, Aladdin; Das, Amit; Schaber, Jana; Scheler, Ulrich; Bhagavatheswaran, Eshwaran S.; Stöckelhuber, Klaus W.; Heinrich, Gert; Voit, Brigitte; Böhme, FrankRubber composites were prepared by mixing bromobutyl rubber (BIIR) with silica particles in the presence of 1-butylimidazole. In addition to pristine (precipitated) silica, silanized particles with aliphatic or imidazolium functional groups, respectively, were used as filler. The silanization was carried out either separately or in situ during compounding. The silanized particles were characterized by TGA, 1H-29Si cross polarization (CP)/MAS NMR, and Zeta potential measurements. During compounding, the bromine groups of BIIR were converted with 1-butylimidazole to ionic imidazolium groups which formed a dynamic network by ionic association. Based on DMA temperature and strain sweep measurements as well as cyclic tensile tests and stress-strain measurements it could be concluded that interactions between the ionic groups and interactions with the functional groups of the silica particles strongly influence the mechanical and viscoelastic behavior of the composites. A particularly pronounced reinforcing effect was observed for the composite with pristine silica, which was attributed to acid-base interactions between the silanol and imidazolium groups. In composites with alkyl or imidazolium functionalized silica particles, the interactions between the filler and the rubber matrix form dynamic networks with pronounced self-healing behavior and excellent tensile strength values of up to 19 MPa. This new approach in utilizing filler-matrix interactions in the formation of dynamic networks opens up new avenues in designing new kinds of particle-reinforced self-healing elastomeric materials with high technological relevance.
- ItemHigh performance stability of titania decorated carbon for desalination with capacitive deionization in oxygenated water(London : RSC Publishing, 2016) Srimuk, Pattarachai; Ries, Lucie; Zeiger, Marco; Fleischmann, Simon; Jäckel, Nicolas; Tolosa, Aura; Krüner, Benjamin; Aslan, Mesut; Presser, VolkerPerformance stability in capacitive deionization (CDI) is particularly challenging in systems with a high amount of dissolved oxygen due to rapid oxidation of the carbon anode and peroxide formation. For example, carbon electrodes show a fast performance decay, leading to just 15% of the initial performance after 50 CDI cycles in oxygenated saline solution (5 mM NaCl). We present a novel strategy to overcome this severe limitation by employing nanocarbon particles hybridized with sol–gel-derived titania. In our proof-of-concept study, we demonstrate very stable performance in low molar saline electrolyte (5 mM NaCl) with saturated oxygen for the carbon/metal oxide hybrid (90% of the initial salt adsorption capacity after 100 cycles). The electrochemical analysis using a rotating disk electrode (RDE) confirms the oxygen reduction reaction (ORR) catalytic effect of FW200/TiO2, preventing local peroxide formation by locally modifying the oxygen reduction reaction.
- ItemMechanistic insight of TiCl4catalyzed formal [3 + 3] cyclization of 1,3-bis(silyl enol ethers) with 1,3-dielectrophiles(London : RSC Publishing, 2015) Nisa, Riffat Un; Maria, Maria; Wasim, Fatima; Mahmood, Tariq; Ludwig, Ralf; Ayub, KhurshidThe mechanism of TiCl4 mediated formal [3 + 3] cyclization of 1,3-bis(silyl enol ethers) with 1,3-dielectrophiles is studied at the B3LYP level of density functional theory (DFT) to rationalize the experimental regioselectivity. Methyl and trifluoromethyl substituted 1,3 dielectrophiles are studied theoretically since they show different regioselectivities. Two different mechanisms involving 1,2 and 1,4 addition of 1,3-bis(silyl enol ethers) on 1,3-dielectrophiles are studied for each dienophile. The intramolecular transition metal catalyzed and non-catalyzed dynamic shift of the silyl moiety is also studied. The structure of the 1,3 dienophile and the associated Mulliken charges are the driving forces for different regioselectivities in methyl and trifluoromethyl dienophiles.
- ItemSPION@polydehydroalanine hybrid particles(London : RSC Publishing, 2015) von der Lühe, Moritz; Günther, Ulrike; Weidner, Andreas; Gräfe, Christine; Clement, Joachim H.; Dutz, Silvio; Schacher, Felix H.It is generally accepted that a protein corona is rapidly formed upon exposure of nanoparticles to biological fluids and that both the amount and the composition of adsorbed proteins affect the dispersion properties of the resulting particles. Hereby, the net charge and overall charge density of the pristine nanoparticles are supposed to play a crucial role. In an attempt to control both charge and charge distribution, we report on the coating of superparamagnetic iron oxide nanoparticles (SPIONs) with different polyelectrolytes. Starting from orthogonally protected polydehydroalanine, the material can be easily transformed into a polyanion (poly(tert-butoxycarbonyl acrylic acid), PtBAA), polycation (poly(aminomethylacrylate), PAMA), or even a polyzwitterion (polydehydroalanine, PDha). While coating of SPIONs with PtBAA and PDha was shown to be successful, approaches using PAMA have failed so far. The dispersion properties of the resulting hybrid particles have been investigated using dynamic light scattering (DLS), zeta-potential, and TEM measurements – the amount of adsorbed polymer was quantified using vibrating sample magnetometry (VSM) and thermogravimetric analysis (TGA).
- ItemPhotocatalytic degradation and toxicity evaluation of diclofenac by nanotubular titanium dioxide–PES membrane in a static and continuous setup(London : RSC Publishing, 2015) Fischer, K.; Kühnert, M.; Gläser, R.; Schulze, A.Diclofenac is a commonly used anti-inflammatory drug, which has been found in surface waters. Advanced oxidation processes (AOPs) seem to be the most suitable technique to prevent the entry of diclofenac and other pollutants into surface waters. TiO2 is especially reliable in mineralizing many organic molecules. The combination of TiO2 nanotubes with a polymer microfiltration membrane (polyethersulfone, PES) showed high photocatalytic activity by degrading diclofenac combined with an excellent membrane performance and long-term stability. By continuously degrading pollutants from water via a cross-flow setup, the molecules to be degraded are transported right to the membrane surface so that the overall reaction rate is increased. The toxicity of diclofenac was reduced by photocatalysis and photolysis; however, photocatalysis had greater impact. Moreover, the complete degradation of pollutants is very important to avoid highly toxic intermediate products.
- ItemPoly(ethylene oxide)-based block copolymers with very high molecular weights for biomimetic calcium phosphate mineralization(London : RSC Publishing, 2015) Mai, Tobias; Boye, Susanne; Yuan, Jiayin; Völkel, Antje; Gräwert, Marlies; Günter, Christina; Lederer, Albena; Taubert, AndreasThe present article is among the first reports on the effects of poly(ampholyte)s and poly(betaine)s on the biomimetic formation of calcium phosphate. We have synthesized a series of di- and triblock copolymers based on a non-ionic poly(ethylene oxide) block and several charged methacrylate monomers, 2-(trimethylammonium)ethyl methacrylate chloride, 2-((3-cyanopropyl)-dimethylammonium)ethyl methacrylate chloride, 3-sulfopropyl methacrylate potassium salt, and [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide. The resulting copolymers are either positively charged, ampholytic, or betaine block copolymers. All the polymers have very high molecular weights of over 106 g mol−1. All polymers are water-soluble and show a strong effect on the precipitation and dissolution of calcium phosphate. The strongest effects are observed with triblock copolymers based on a large poly(ethylene oxide) middle block (nominal Mn = 100 000 g mol−1). Surprisingly, the data show that there is a need for positive charges in the polymers to exert tight control over mineralization and dissolution, but that the exact position of the charge in the polymer is of minor importance for both calcium phosphate precipitation and dissolution.
- ItemThermally triggered optical tuning of π-conjugated graft copolymers based on reversible Diels–Alder reaction(London : RSC Publishing, 2016) Ahner, J.; Micheel, M.; Kötteritzsch, J.; Dietzek, B.; Hager, M.D.In order to design a π-conjugated polymer film with tunable optical properties by thermally triggered activation of energy transfer after processing, two monodisperse phenylene ethynylene based oligomers with different optical properties were synthesized and attached to aliphatic polymers as π-conjugated side chains. Subsequently, the exchange of the side chain chromophores between the prepared donor and acceptor graft polymers in the solid state based on a reversible Diels–Alder reaction was studied in detail. The resulting donor–acceptor graft copolymer exhibits intra polymer energy transfer upon excitation of the donor moiety. The photophysical properties of the original and exchanged graft copolymers were investigated by means of absorption and emission spectroscopy. This novel concept opens the possibility for optical tuning of π-conjugated polymer films after processing as well as applications as thermally triggered sensor systems.
- ItemB12X11(H2)−: exploring the limits of isotopologue selectivity of hydrogen adsorption(London : RSC Publishing, 2021) Wulf, Toshiki; Warneke, Jonas; Heine, ThomasWe study the isotopologue-selective binding of dihydrogen at the undercoordinated boron site of B12X11− (X = H, F, Cl, Br, I, CN) using ab initio quantum chemistry. With a Gibbs free energy of H2 attachment reaching up to 80 kJ mol−1 (ΔG at 300 K for X = CN), these sites are even more attractive than most undercoordinated metal centers studied so far. We thus believe that they can serve as an edge case close to the upper limit of isotopologue-selective H2 adsorption sites. Differences of the zero-point energy of attachment average 5.0 kJ mol−1 between D2 and H2 and 2.7 kJ mol−1 between HD and H2, resulting in hypothetical isotopologue selectivities as high as 2.0 and 1.5, respectively, even at 300 K. Interestingly, even though attachment energies vary substantially according to the chemical nature of X, isotopologue selectivities remain very similar. We find that the H–H activation is so strong that it likely results in the instantaneous heterolytic dissociation of H2 in all cases (except, possibly, for X = H), highlighting the extremely electrophilic nature of B12X11− despite its negative charge. Unfortunately, this high reactivity also makes B12X11− unsuitable for practical application in the field of dihydrogen isotopologue separation. Thus, this example stresses the two-edged nature of strong H2 affinity, yielding a higher isotopologue selectivity on the one hand but risking dissociation on the other, and helps define a window of adsorption energies into which a material for selective adsorption near room temperature should ideally fall.
- ItemPlant leaves as templates for soft lithography(London : RSC Publishing, 2016) Wu, Wenming; Guijt, Rosanne M.; Silina, Yuliya E.; Koch, Marcus; Manz, AndreasWe report a simple fast, practical and effective method for the replication of the complex venation patterns of natural leaves into PDMS with accuracy down to a lateral size of 500 nm. Optimising the amount of crosslinker enabled the replication and sealing of the microvascular structures to yield enclosed microfluidic networks. The use of plant leaves as templates for soft lithography was demonstrated across over ten species and included reticulate, arcuate, pinnate, parallel and palmate venation patterns. SEM imaging revealed replication of the plants microscopic and sub-microscopic topography into the PDMS structures, making this method especially attractive for mimicking biological structures for in vitro assays. Flow analysis revealed that the autonomous liquid transport velocity in 1st-order microchannel was 1.5–2.2 times faster than that in the 2nd-order microchannels across three leaf types, with the sorptivity rule surprisingly preserved during self-powered flow through leaf-inspired vascularity from Carpinus betulus.
- ItemComputer vision vs. spectrofluorometer-assisted detection of common nitro-explosive components with bola-type PAH-based chemosensors(London : RSC Publishing, 2021) Kovalev, Igor S.; Sadieva, Leila K.; Taniya, Olga S.; Yurk, Victoria M.; Minin, Artem S.; Santra, Sougata; Zyryanov, Grigory V.; Charushin, Valery N.; Chupakhin, Oleg N.; Tsurkan, Mikhail V.Computer vision (CV) algorithms are widely utilized in imaging processing for medical and personal electronics applications. In sensorics CV can provide a great potential to quantitate chemosensors' signals. Here we wish to describe a method for the CV-assisted spectrofluorometer-free detection of common nitro-explosive components, e.g. 2,4-dinitrotoluene (DNT) and 2,4,6-trinitrotoluene (TNT), by using polyaromatic hydrocarbon (PAH, PAH = 1-pyrenyl or 9-anthracenyl) – based bola-type chemosensors. The PAH components of these chemical bolas are able to form stable, bright emissive in a visual wavelength region excimers, which allows their use as extended matrices of the RGB colors after imaging and digital processing. In non-polar solvents, the excimers have poor chemosensing properties, while in aqueous solutions, due to the possible micellar formation, these excimers provide “turn-off” fluorescence detection of DNT and TNT in the sub-nanomolar concentrations. A combination of these PAH-based fluorescent chemosensors with the proposed CV-assisted algorithm offers a fast and convenient approach for on-site, real-time, multi-thread analyte detection without the use of fluorometers. Although we focus on the analysis of nitro-explosives, the presented method is a conceptual work describing a general use of CV for quantitative fluorescence detection of various analytes as a simpler alternative to spectrofluorometer-assisted methods.
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