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- ItemA 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, PetraA 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.
- ItemCharacterization of the state of dispersion of carbon nanotubes in polymer nanocomposites(Weinheim : Wiley-VCH Verl., 2011) Buschhorn, Samuel T.; Wichmann, Malte H. G.; Sumfleth, Jan; Schulte, Karl; Pegel, Sven; Kasaliwal, Gaurav R.; Villmow, Tobias; Krause, Beate; Göldel, Andreas; Pötschke, PetraA practical overview of possibilities and limits to characterize the state of dispersion of carbon nanotubes (CNT) in polymer based nanocomposites is given. The most important and widely available methods are discussed with practical employment in mind. One focus is the quantitative characterization of the state of dispersion in solid samples using microscopy techniques such as optical microscopy or transmission electron microscopy. For dispersions of CNTs in aqueous media, solvents or monomers a sedimentation analysis is presented. This way dispersability and dispersion state of CNTs can be assessed. Indirect methods such as electrical conductivity measurements and rheological tests, dynamic differential scanning calorimetry and mechanical test are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
- ItemElectrical, mechanical, and glass transition behavior of polycarbonate-based nanocomposites with different multi-walled carbon nanotubes(Oxford : Elsevier Science, 2011) Castillo, Frank Yepez; Socher, Robert; Krause, Beate; Headrick, Robert; Grady, Brian P.; Prada-Silvy, Ricardo; Pötschke, PetraFive commercially available multi-walled carbon nanotubes (MWNTs), with different characteristics, were melt mixed with polycarbonate (PC) in a twin-screw micro compounder to obtain nanocomposites containing 0.25-3.0 wt.% MWNT. The electrical properties of the composites were assessed using bulk electrical conductivity measurements, the mechanical properties of the composites were evaluated using tensile tests and dynamic mechanical analysis (DMA), and the thermal properties of the composites were investigated using differential scanning calorimetry (DSC). Electrical percolation thresholds (pcs) were observed between 0.28 wt.% and 0.60 wt.%, which are comparable with other well-dispersed melt mixed materials. Based on measurements of diameter and length distributions of unprocessed tubes it was found that nanotubes with high aspect ratios exhibited lower pcs, although one sample did show higher pc than expected (based on aspect ratio) which was attributed to poorer dispersion achieved during mixing. The stress-strain behavior of the composites is only slightly altered with CNT addition; however, the strain at break is decreased even at low loadings. DMA tests suggest the formation of a combined polymer-CNT continuous network evidenced by measurable storage moduli at temperatures above the glass transition temperature (T g), consistent with a mild reinforcement effect. The composites showed lower glass transition temperatures than that of pure PC. Lowering of the height of the tanδ peak from DMA and reductions in the heat capacity change at the glass transition from DSC indicate that MWNTs reduced the amount of polymer material that participates in the glass transition of the composites, consistent with immobilization of polymer at the nanotube interface. © 2011 Elsevier Ltd. All rights reserved.
- ItemElectrical and thermal properties of polyamide 12 composites with hybrid fillers systems of multiwalled carbon nanotubes and carbon black(Barking : Elsevier, 2011) Socher, Robert; Krause, Beate; Hermasch, Sylvia; Wursche, Roland; Pötschke, PetraHybrid filler systems of multiwalled carbon nanotubes (MWCNTs) and carbon black (CB) were incorporated into two types of polyamide 12 (PA12) using small-scale melt mixing in order to identify potential synergistic effects on the interaction of these two electrical conductive fillers. Although no synergistic effects were observed regarding the electrical percolation threshold, at loadings well above the percolation threshold higher volume conductivities were obtained for samples containing both, MWCNT and CB, as compared to single fillers. This effect was more pronounced when using a higher viscous PA12 matrix. The formation of a co-supporting network can be assumed. The combined use of CB and MWCNTs improved the macrodispersion of MWCNT agglomerates, which can be assigned as a synergistic effect. DSC measurements indicated an effect of the nanofiller on crystallisation temperatures of PA12; however this was independent of the kind or amount of the carbon nanofiller. © 2011 Elsevier Ltd.
- ItemInfluence of dry grinding in a ball mill on the length of multiwalled carbon nanotubes and their dispersion and percolation behaviour in melt mixed polycarbonate composites(Barking : Elsevier, 2011) Krause, Beate; Villmow, Tobias; Boldt, Regine; Mende, Mandy; Petzold, Gudrun; Pötschke, PetraBall milling of carbon nanotubes (CNTs) in the dry state is a common way to produce tailored CNT materials for composite applications, especially to adjust nanotube lengths. For NanocylTM NC7000 nanotube material before and after milling for 5 and 10h the length distributions were quantified using TEM analysis, showing decreases of the mean length to 54% and 35%, respectively. With increasing ball milling time in addition a decrease of agglomerate size and an increase of packing density took place resulting in a worse dispersability in aqueous surfactant solutions. In melt mixed CNT/polycarbonate composites produced using masterbatch dilution step, the electrical properties, the nanotube length distribution after processing, and the nano- and macrodispersion of the nanotubes were studied. The slight increase in the electrical percolation threshold in the melt mixed composites with ball milling time of CNTs can be assigned to lower nanotube lengths as well as the worse dispersability of the ball milled nanotubes. After melt compounding, the mean CNT lengths were shortened to 31%, 50%, and 66% of the initial lengths of NC7000, NC7000-5h, and NC7000-10h, respectively. © 2011 Elsevier Ltd.
- ItemPercolation behaviour of multiwalled carbon nanotubes of altered length and primary agglomerate morphology in melt mixed isotactic polypropylene-based composites(Barking : Elsevier, 2011) Menzer, Katharina; Krause, Beate; Boldt, Regine; Kretzschmar, Bernd; Weidisch, Roland; Pötschke, PetraThe effect of ball milling on the structural characteristics and further on the dispersion and percolation behaviour of multiwalled carbon nanotubes (MWCNTs) in melt mixed composites using a maleic anhydride modified isotactic polypropylene as matrix was investigated. TEM and SEM revealed that ball milled nanotubes were considerably shorter and showed a compact primary agglomerate morphology compared to the as-synthesised MWCNTs. At macro scale ball milled MWCNTs were found to be better dispersed, whereas at sub-micron scale the states of dispersion of both nanotube materials were comparable. The differences in the composite morphologies as well as in the composites electrical and rheological percolation behaviour were assigned to the altered MWCNT structure due to ball milling treatment. The dispersibility of ball milled MWCNTs was restricted due to their more compact agglomerate morphology. Furthermore, the ability to form percolated network structures was restrained by their shorter length and, again, their compact primary agglomerates. An effective agglomerate interaction radius depending on the nanotube structural characteristics, length and agglomerate morphology, is suggested in order to explain the experimental findings. © 2011 Elsevier Ltd.
- ItemMelt mixed nano composites of PA12 with MWNTs: Influence of MWNT and matrix properties on macrodispersion and electrical properties(Barking : Elsevier, 2011) Socher, Robert; Krause, Beate; Boldt, Regine; Hermasch, Sylvia; Wursche, Roland; Pötschke, PetraNanocomposites containing four different polyamide 12 (PA12) types and three grades of multiwalled carbon nanotubes (MWNTs) were prepared via small-scale melt processing to study the effect of different MWNTs and the influence of polymer properties on the dispersion of the fillers and the electrical properties of the composites. Under the selected mixing conditions the lowest electrical percolation threshold of 0.7. wt.% was found for Nanocyl™ NC7000 in low viscous PA12. Moreover, big influences of the end group functionality (acid or amine excess) and the melt viscosity of the matrix were found. Composites of PA12 with acid excess showed lower percolation thresholds than those based on amine terminated materials. At constant end group ratio low viscous matrices resulted in lower percolation thresholds than high viscous materials. The best MWNT dispersion was obtained in both high viscous PA12 composites. In these systems the mixing speed was varied indicating an optimum concerning electrical conductivity at 150 rpm as compared to 50 and 250 rpm. © 2010 Elsevier Ltd.
- ItemInfluence of feeding conditions in twin-screw extrusion of PP/MWCNT composites on electrical and mechanical properties(Barking : Elsevier, 2011) Müller, Michael Thomas; Krause, Beate; Kretzschmar, Bernd; Pötschke, PetraThe influence of feeding conditions of multiwalled carbon nanotube (MWCNT) materials, namely Baytubes® C150P and Nanocyl™ NC7000, into polypropylene (PP) was investigated with respect to achieving suitable nanotube dispersion, high electrical conductivity, and good mechanical properties. Both MWCNT materials were fed at selected concentrations either in the hopper of the twin-screw extruder or using a side feeder under otherwise identical extrusion conditions (rotation speed, throughput, temperature profile) using a Berstorff ZE 25 twin-screw extruder. Afterwards, injection molding was performed under identical conditions. The results indicate that the more compact Baytubes® C150P agglomerates should be added into the hopper, as the dispersion assessed by light microscopy is better, electrical resistivities measured on compression and injection molded samples are lower, and elastic modulus, yield strength and impact strength are higher as compared to side feeding. On the other hand, for the more loosely packed Nanocyl™ NC7000 agglomerates, addition using the side feeder leads to better dispersion, lower electrical resistivity, and higher mechanical properties. © 2011 Elsevier Ltd.
- ItemVerbundprojekt: Entwicklung polymerer Nanokomposite mit gleichzeitig verbesserten mechanischen und elektrischen Eigenschaften (COMPOMEL), Teilprojekt: Stofflich-verfahrenstechnische Zusammenhänge beim Schmelzemischen : Schlussbericht(Hannover : Technische Informationsbibliothek (TIB), 2011) Pötschke, Petra[no abstract available]