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A process was developed for graphite particle exfoliation in water to stably dispersed multi-layer graphene. It uses electrohydraulic shockwaves and the functionalizing effect of solution plasma discharges in water. The discharges were excited by 100 ns high voltage pulsing of graphite particle chains that bridge an electrode gap. The underwater discharges allow simultaneous exfoliation and chemical functionalization of graphite particles to partially oxidized multi-layer graphene. Exfoliation is caused by shockwaves that result from rapid evaporation of carbon and water to plasma-excited gas species. Depending on discharge energy and locus of ignition, the shockwaves cause stirring, erosion, exfoliation and/or expansion of graphite flakes. The process was optimized to produce long-term stable aqueous dispersions of multi-layer graphene from graphite in a single process step without requiring addition of intercalants, surfactants, binders or special solvents. A setup was developed that allows continuous production of aqueous dispersions of flake size-selected multi-layer graphenes. Due to the well-preserved sp(2)-carbon structure, thin films made from the dispersed graphene exhibited high electrical conductivity. Underwater plasma discharge processing exhibits high innovation potential for morphological and chemical modifications of carbonaceous materials and surfaces, especially for the generation of stable dispersions of two-dimensional, layered materials.
Thin coatings of poly(acrylic acid) (PAA) and poly(hydroxyethylmethacrylate) (PHEMA) were deposited onto carbon fibers by means of the electrospray ionization (ESI) technique in ambient air. These high-molecular weight polymer layers were used as adhesion promoters in carbon fiberepoxy resin composites. Within the ESI process, the carbon fibers were completely enwrapped with polymer in the upper 10 plies of a carbon fiber roving. As identified with scanning electron microscopy also shadowed fibers in a bundle as well as backsides of fiber rovings were pinhole-free coated with polymers (electrophoretic effect'). Under the conditions used, the layers have a granular structure. Residual solvent was absent in the deposit. PAA and PHEMA films did not show any changes in composition and structure in comparison with the original polymers as analyzed by X-ray photo-electron spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Single-fiber pullout tests of coated fibers embedded in epoxy resin showed significantly increased interfacial shear strength. It is assumed that chemical bonds between carbon fiber poly(acrylic acid) and epoxy resin contribute significantly to the improved interactions.
In diesem Beitrag wird ein neuartiger Ansatz zur Erzeugung von Luftultraschall vorgestellt, der auf dem thermoakustischen Prinzip beruht. Mikro- und nanostrukturierte Kohlenstoffmaterialien werden dabei mit einem harmonischen Wechselstrom gespeist und erfahren durch ohmsche Verluste eine Temperaturänderung, die sich auf das umgebende Fluid überträgt. Daraus resultieren Druckmodulationen, und es wird eine ausbreitungsfähige Schallwelle erzeugt. Dabei tritt Frequenzverdopplung gegenüber der Anregungsfrequenz auf. Es konnte gezeigt werden, dass der entscheidende Parameter für die Effizienz der Methode, d.h. für ein möglichst großes Verhältnis von Schalldruck zu eingebrachter Leistung, die Wärmekapazität pro Flächeneinheit ist. Da dieser Quotient für Kohlenstoffmaterialien sehr klein sein kann, erlaubt das thermoakustische Prinzip hier die effiziente Erzeugung von Luftultraschall. Schalldruckmessungen an verschiedenen Materialproben wurden bis 100 kHz mit einem Mikrofon durchgeführt, oberhalb von 100 kHz wurde eine laservibrometrische Schnellemessung eingesetzt. In experimentellen Untersuchungen wurde die Schallerzeugung in Abhängigkeit der Materialeigenschaften analysiert und systematisiert. Die experimentellen Ergebnisse wurden mit numerischen und analytischen Berechnungsergebnissen verglichen.
Wet-chemically oxidized carbon nanotubes (CNTs) generally exhibit both covalently-bound acidic functional groups on the surface and surface-adsorbed acidic substances, i.e. carbonaceous CNT fragments from the oxidation procedure. Direct potentiometric titration of oxidizable high surface area materials with dynamically desorbing acidic fragments is slow and inaccurate. Adsorbed acidic fragments are deprotonated by sodium hydroxide and form anions in solution which is not the case for covalently bound acidic groups on the CNTs, so the following filtration after NaOH treatment separates desorbable acidic substances from non-desorbable or covalently bound groups. For a known concentration of NaOH, titration of the eluate with hydrochloric acid (HCl) allows determination of the concentrations of both types of acidities. However, contrary to reports in the literature, the NaOH consumed by non-desorbed acidic groups has to be accounted for and impedes distinction of desorbed acidic groups via their pKa values. Results are presented of a study on the information content and the reliability of indirect potentiometric Boehm titration for different oxidized multi-walled CNTs.