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    A successful approach to disperse MWCNTs in polyethylene by melt mixing using polyethylene glycol as additive
    (Oxford : Elsevier Science, 2012) Müller, Michael Thomas; Krause, Beate; Pötschke, Petra
    An additive-assisted one-step melt mixing approach was developed to produce nanocomposites based on linear low density polyethylene (LLDPE) with multiwalled carbon nanotube (MWCNT). The polymer granules, nanotube powder (2 wt% Nanocyl™ NC7000) and 1-10 wt% of the non-ionic additives poly(ethylene glycol) (PEG) or poly(ethylene oxide) (PEO) with molar masses between 100 g/mol and 100,000 g/mol were simply fed together in the hopper of a small-scale DSM Xplore 15 twin-screw microcompounder. The produced MWCNT/LLDPE composites showed excellent MWCNT dispersion and highly improved electrical properties as compared to samples without the additive, whereas the effects depend on the amount and molar mass of the additive. When 7 wt% PEG (2000 g/mol) were used, a reduction of the electrical percolation threshold from 2.5 wt% to 1.5 wt% was achieved. © 2012 Elsevier Ltd. All rights reserved.
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    Polypropylene-based melt mixed composites with singlewalled carbon nanotubes for thermoelectric applications: Switching from p-type to n-type by the addition of polyethylene glycol
    (Oxford : Elsevier Science, 2017) Luo, Jinji; Cerretti, Giacomo; Krause, Beate; Zhang, Long; Otto, Thomas; Jenschke, Wolfgang; Ullrich, Mathias; Tremel, Wolfgang; Voit, Brigitte; Pötschke, Petra
    The thermoelectric properties of melt processed conductive nanocomposites consisting of an insulating polypropylene (PP) matrix filled with singlewalled carbon nanotubes (CNTs) and copper oxide (CuO) were evaluated. An easy and cheap route to switch p-type composites into n-type was developed by adding polyethylene glycol (PEG) during melt mixing. At the investigated CNT concentrations of 0.8 wt% and 2 wt% (each above the electrical percolation threshold of ∼0.1 wt%), and a fixed CuO content of 5 wt%, the PEG addition converted p-type composites (positive Seebeck coefficient (S)) into n-type (negative S). PEG was also found to improve the filler dispersion inside the matrix. Two composites were prepared: P-type polymer/CNT composites with high S (up to 45 μV/K), and n-type composites (with S up to −56 μV/K) through the addition of PEG. Two prototypes with 4 and 49 thermocouples of these p- and n-type composites were fabricated, and delivered an output voltage of 21 mV and 110 mV, respectively, at a temperature gradient of 70 K.
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    Impact of synthesis temperature on morphology, rheology and electromagnetic interference shielding of CVD-grown carbon nanotube/polyvinylidene fluoride nanocomposites
    (Lausanne : Elsevier Sequoia, 2017) Mirkhani, Seyyed Alireza; Arjmand, Mohammad; Sadeghi, Soheil; Krause, Beate; Pötschke, Petra; Sundararaj, Uttandaraman
    Employing chemical vapor deposition technique, multi-walled carbon nanotubes (CNTs) were synthesized over Fe catalyst at a broad range of temperatures, i.e. 550° C to 950° C (at 100° C intervals). CNTs were melt-mixed into a polyvinylidene fluoride (PVDF) matrix at various loadings, and then compression molded. Surprisingly, despite the ascending trend of CNT powder conductivity with the synthesis temperature, the nanocomposites made with CNT synthesized at 650° C had significantly lower percolation threshold (around 0.4 wt%) and higher electromagnetic interference shielding effectiveness (EMI SE) (20.3 dB over the X-band for 3.5 wt% CNT and 1.1 mm thickness) than the other temperatures. Exhaustive characterization studies were conducted on both CNTs and composites to unveil their morphological and electrical characteristics. Superior EMI shielding of CNT650° C was attributed to a combination of high carbon purity, aspect ratio, crystallinity, and moderate powder conductivity along with decent state of dispersion within the PVDF matrix.
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    Comparison of the molecular properties and morphology of polypropylenes irradiated under different atmospheres and after annealing
    (Hoboken, NJ [u.a.] : Wiley InterScience, 2006) Krause, Beate; Häußler, Liane; Voigt, Dieter
    Electron-beam irradiation, a well-known way of generating long-chain branching, was used to modify polypropylene. Samples were investigated with differential scanning calorimetry, polarized light microscopy, and size exclusion chromatography. Independently of the atmosphere, postannealing led to the deactivation of residual radicals and to the reduction of the nucleus density. In comparison with the initial polypropylene, the crystallization temperatures increased for nonannealed samples but decreased for annealed samples. Stable products were obtained only by irradiation in nitrogen followed by annealing. A reaction including free radicals with oxygen in the ambient atmosphere led to increasing molar mass degradation and the formation of long-chain branching after Storage. © 2006 Wiley Periodicals, Inc.
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    Correlation of carbon nanotube dispersability in aqueous surfactant solutions and polymers
    (New York, NY [u.a.] : Pergamon Press, 2009) Krause, Beate; Petzold, Gudrun; Pegel, Sven; Pötschke, Petra
    In order to assess the dispersability of carbon nanotube materials, tubes produced under different synthesis conditions were dispersed in aqueous surfactant solutions and the sedimentation behaviour under centrifugation forces was investigated using a LUMiFuge stability analyzer. The electrical percolation threshold of the nanotubes after melt mixing in polyamide 6.6 was determined and the state of dispersion was studied. As a general tendency, the nanotubes having better aqueous dispersion stability showed lower electrical percolation threshold and better nanotube dispersion in the composites. This indicates that the investigation of the stability of aqueous dispersions is also able to give information about the nanotubes inherent dispersability in polymer melts, both strongly influenced by the entanglement and agglomerate structure of the tubes within the as-produced nanotube materials. The shape of the nanotubes in the aqueous dispersions was assessed using a SYSMEX flow particle image analyzer and found to correspond to the shape observed from cryofractured surfaces of the polymer composites. © 2008 Elsevier Ltd. All rights reserved.
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    Effect of synthesis catalyst on structure of nitrogen-doped carbon nanotubes and electrical conductivity and electromagnetic interference shielding of their polymeric nanocomposites
    (New York, NY [u.a.] : Pergamon Press, 2016) Arjmand, Mohammad; Chizari, Kambiz; Krause, Beate; Pötschke, Petra; Sundararaj, Uttandaraman
    Different catalysts including Co, Fe, and Ni were used to synthesize nitrogen-doped carbon nanotubes (N-CNTs) by chemical vapor deposition technique. Synthesized N-CNTs were melt mixed with a polyvinylidene fluoride (PVDF) matrix using a small scale mixer at different concentrations ranging from 0.3 to 3.5 wt%, and then compression molded. The characterization techniques revealed significant differences in the synthesis yield and the morphological and electrical properties of both N-CNTs and nanocomposites depending on the catalyst type. Whereas Co and Fe resulted in yields comparable to industrial multiwalled CNTs, Ni was much less effective. The N-CNT aspect ratio was the highest for Co catalyst, followed by Ni and Fe, whereas nitrogen content was the highest for Ni. Raman spectroscopy revealed lowest defect number and highest N-CNT crystallinity for Fe catalyst. Characterization of N-CNT/PVDF nanocomposites showed better dispersion for N-CNTs based on Co and Fe as compared to Ni, and the following order of electrical conductivity and electromagnetic interference shielding (from high to low): Co > Fe > Ni. The superior electrical properties of (N-CNT)Co nanocomposites were ascribed to a combination of high synthesis yield, high aspect ratio, low nitrogen content and high crystallinity of N-CNTs combined with a good state of N-CNT dispersion.
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    Characterization of electron beam irradiated polypropylene: Influence of irradiation temperature on molecular and rheological properties
    (Hoboken, NJ [u.a.] : Wiley InterScience, 2006) Krause, Beate; Voigt, Dieter; Häuβler, Liane; Auhl, Dietmar; Münstedt, Helmut
    The aim of the investigations was to analyze the influence of the temperature during the irradiation process of polypropylene on the molar mass, the formation of long chain branching and the final branching topology. A linear isotactic polypropylene homopolymer was modified by electron beam irradiation at different temperatures, with two irradiation doses to insert long chain branching. The Samples were analyzed by size exclusion chromatography coupled with a multiangle laser light scattering detector, by differential scanning calorimetry, and by shear and elongational rheology. The shear and elongational flow behavior isdiscussed in terms of the influence of molecular parameters and used to analyze the topology of the irradiated samples. With increasing temperature, a slight reduction of the molar mass, an increase of long chain branching and an increase of crystallization temperature were found. © 2006 Wiley Periodicals, Inc.
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    A method for determination of length distributions of multiwalled carbon nanotubes before and after melt processing
    (New York, NY [u.a.] : Pergamon Press, 2011) Krause, Beate; Boldt, Regine; Pötschke, Petra
    A relatively simple method to determine the length distribution of carbon nanotubes (CNTs) before and after melt processing was developed. This involves the selection of a suitable solvent for dispersing pristine CNTs as well as to dissolve the matrix of melt mixed composites and the choice of an appropriate nanotube concentration. The length of suitably individualized CNTs was visualized using transmission electron microscopy and length distributions were measured using image analysis. Examples are shown for Baytubes® C150HP and Nanocyl™ NC7000 and their melt mixed composites with polycarbonate where the same procedure was applied to both, measuring the initial length distribution and the distribution after recovering from the composites. These results indicated a significant shortening after melt processing up to 30% of the initial length. © 2010 Elsevier Ltd. All rights reserved.
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    Long-chain branching of polypropylene by electron-beam irradiation in the molten state
    (Hoboken, NJ [u.a.] : Wiley InterScience, 2006) Krause, Beate; Stephan, M.; Volkland, S.; Voigt, D.; Häußler, L.; Dorschner, H.
    The electron-beam irradiation of polymers generates modification effects in the macromolecular structure and material properties. Therefore, irradiation processing is mostly realized in the polymer solid state. In this way, the modification of linear polypropylene may result in long-chain branching of polypropylene macromolecules. The objective of this article is to investigate the effect of a polymer in the molten state during electron-beam irradiation on the macromolecular structure and material properties of polypropylene. For this procedure, a special irradiation vessel (BG3) has been developed in which a rapid transfer of polymer films from the solid state to the molten state and a defined temperature during electron-beam irradiation are realizable. The irradiated samples have been analyzed by high-temperature size exclusion chromatography coupled with a multi-angle laser light scattering detector and differential scanning calorimetry (DSC) measurements. With an increasing irradiation dose, a high reduction of the molar mass and an increasing amount of long-chain branching are found. Compared with irradiation in the solid state, the modification in the molten state leads to a higher degree of branching. The Theological experiments in elongation flow clearly exhibit the existence of long-chain branching. Furthermore, DSC measurements show that the glass-transition temperature and peak temperatures of melting and crystallization decrease. © 2005 Wiley Periodicals, Inc.
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    Dispersability of multiwalled carbon nanotubes in polycarbonate-chloroform solutions
    (Oxford : Elsevier Science, 2014) Staudinger, Ulrike; Krause, Beate; Steinbach, Christine; Pötschke, Petra; Voit, Brigitte
    The dispersion of commercial multiwalled carbon nanotubes (MWCNTs, Nanocyl™ NC7000) in chloroform and in polycarbonate (PC)-chloroform solutions was investigated by variation of the polymer concentration, MWCNT amount and sonication time and compared with PC/MWCNT composites, which were processed by melt mixing, subsequently dissolved in chloroform and dispersed via sonication under the same conditions. The sedimentation behaviour was characterised under centrifugal forces using a LUMiSizer® separation analyser. The space and time resolved extinction profiles as a measure of the stability of the dispersion and the particle size distribution were evaluated. Sonication up to 5 min gradually increases the amount of dispersed particles in the solutions. A significant improvement of the MWCNT dispersion in chloroform was achieved by the addition of PC indicating the mechanism of polymer chain wrapping around the MWCNTs. In dispersions of melt mixed PC/MWCNT composites the dispersion of MWCNTs is significantly enhanced already at a low sonication time of only 0.5 min due to very efficient polymer wrapping during the melt mixing process. However, the best dispersion quality does not lead to the highest electrical conductivity of thin composite films made of these PC/MWCNT dispersions.