Search Results
Effects of high energy electrons on the properties of polyethylene / multiwalled carbon nanotubes composites: Comparison of as-grown and oxygen-functionalised MWCNT
2014, Krause, Beate, Pötschke, Petra, Gohs, U.
Polymer modification with high energy electrons (EB) is well established in different applications for many years. It is used for crosslinking, curing, degrading, grafting of polymeric materials and polymerisation of monomers. In contrast to this traditional method, electron induced reactive processing (EIReP) combines the polymer modification with high energy electrons and the melt mixing process. This novel reactive method was used to prepare polymer blends and composites. In this study, both methods were used for the preparation of polyethylene (PE)/ multiwalled carbon nanotubes (MWCNT) composites in the presence of a coupling agent. The influence of MWCNT and type of electron treatment on the gel content, the thermal conductivity, rheological, and electrical properties was investigated whereby as-grown and oxidised MWCNT were used. In the presence of a coupling agent and at an absorbed dose of 40 kGy, the gel content increased from 57 % for the pure PE to 74 % or 88 % by the addition of as-grown (Baytubes® C150P) or oxidised MWCNT, respectively. In comparison to the composites containing the as-grown MWCNTs, the use of the oxidised MWCNTs led to higher melt viscosity and higher storage modulus due to higher yield of filler polymer couplings. The melt viscosity increased due to the addition of MWCNT and crosslinking of PE. The thermal conductivity increased to about 150 % and showed no dependence on the kind of MWCNT and the type of electron treatment. In contrast, the lowest value of electrical volume resistivity was found for the non-irradiated samples and after state of the art electron treatment without any influence of the type of MWCNT. In the case of EIReP, the volume resistivity increased by 2 (as-grown MWCNT) or 3 decades (oxidised MWCNT) depending on the process parameters. © 2014 American Institute of Physics.
Methods to characterize the dispersability of carbon nanotubes and their length distribution
2012, Krause, Beate, Mende, Mandy, Petzold, Gudrun, Boldt, Regine, Pötschke, Petra
Two main properties of carbon nanotube (CNT) materials are discussed in this contribution. First, a method to characterize the dispersability of CNT materials in aqueous surfactant solutions in presented, which also allows conclusions towards the dispersability in other media, like polymer melts. On the other hand it is shown, how the length of CNTs before and after processing, e.g., after melt mixing with thermoplastics, can be quantified. Both methods are illustrated with examples and the practical relevance is shown. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Influence of talc with different particle sizes in melt-mixed LLDPE/MWCNT composites
2013, Müller, Michael Thomas, Dreyße, Janine, Häußler, Liane, Krause, Beate, Pötschke, Petra
Linear low-density polyethylene (LLDPE) was melt-mixed with multiwalled carbon nanotubes (MWCNTs) and varying amounts of three different kinds of talc (phyllo silicate), each with a different particle size distribution, to examine the effect of these filler combinations with regards to the electrical percolation behavior. The state of the filler dispersion was assessed using transmission light microscopy and electron microscopy. The use of talc as a second filler during the melt mixing of LLDPE/MWCNT composites resulted in an improvement in the dispersion of the MWCNTs and a decrease of the electrical percolation threshold. Talc with lower particle sizes showed a more pronounced effect than talc with larger particle sizes. However, the improvement in dispersion was not reflected in the mechanical properties. Modulus and stress values increase with both, MWCNT and talc addition, but not in a synergistic manner. The crystallization behavior of the composites was studied by differential scanning calorimetry to determine its potential influence on the electrical percolation threshold. It was found that the crystallinity of the matrix increased slightly with the addition of talc but no further increments were observed with the incorporation of the MWCNTs. © 2013 Wiley Periodicals, Inc.
Melt mixed PCL/MWCNT composites prepared at different rotation speeds: Characterization of rheological, thermal, and electrical properties, molecular weight, MWCNT macrodispersion, and MWCNT length distribution
2013, Pötschke, Petra, Villmow, Tobias, Krause, Beate
Composites of poly(caprolactone) (PCL) and 0.5 wt.% multiwalled carbon nanotubes (MWCNT) were prepared by melt-mixing in a conical twin-screw micro-compounder by varying the rotation speed between 25 and 400 rpm at constant mixing time and temperature. The state of dispersion analyzed by light microscopy was improved with increasing rotation speed but levels off starting at about 100 rpm. PCL molecular weight as well as crystallization and melting behavior did show only insignificant difference when varying the rotation speed. Concerning melt rheological properties, storage modulus G′ and complex viscosity η* at 0.1 rad/s increased up to a rotation speed of about 75 rpm illustrating improved dispersion. When further increasing the speed G′ and η* decreased which was attributed to more pronounced nanotube shortening as quantified by TEM measurements. Both effects - improved dispersion and nanotube shortening - are also reflected in the electrical resistivity values of compression molded samples which show a minimum of resistivity at the rotation speed of 75 rpm corresponding to a specific mechanical energy input of 0.47 kWh/kg. © 2013 Elsevier Ltd. All rights reserved.
A method for determination of length distributions of multiwalled carbon nanotubes before and after melt processing
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.
Achieving electrical conductive tracks by laser treatment of non-conductive polypropylene/polycarbonate blends filled with MWCNTs
2014, Liebscher, Marco, Krause, Beate, Pötschke, Petra, Barz, Andrea, Bliedtner, Jens, Möhwald, Michael, Letzsch, Alexander
Electrical non-conductive polymer blends consisting of a polypropylene (PP) matrix and dispersed particles of polycarbonate (PC) were melt compounded with 3 wt.% multiwalled carbon nanotubes (MWCNTs) loading and processed into plates by injection molding. The morphological analysis confirmed the selective localization of the MWCNTs in the PC component. By local irradiation with a CO2 laser beam, depending on the laser conditions, conductive tracks with dimensions of about 2 mm width, 80 to 370 μm depth and line resistances as low as 1.5 kΩ · cm-1 were created on the surface of the non-conductive plates. The factors affecting the line resistance are the PC content, the laser speed and laser power, as well as laser direction with respect to the melt flow direction. After the irradiation an enrichment of MWCNTs in the laser lines was detected indicating that conductive paths were generated by percolation of nanotubes selectively within these lines in otherwise non-conductive plates. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Interfacial chemistry using a bifunctional coupling agent for enhanced electrical properties of carbon nanotube based composites
2013, Socher, Robert, Jakisch, Lothar, Krause, Beate, Oertel, Ulrich, Voit, Brigitte, Pötschke, Petra
A bifunctional coupling agent (BCA) containing one oxazoline and one benzoxazinone group was applied to promote a reaction between polyamide 12 (PA12) and multiwalled carbon nanotubes (MWCNTs) during melt mixing. With this modification, the MWCNT content needed for the electrical percolation was significantly reduced by more than a factor of three. For amino functionalized MWCNT-PA12 composites adding 1 wt.% BCA electrical percolation was reached at only 0.37 wt.% MWCNTs compared to 1.0 wt.% without BCA. With the help of a model reaction, the covalent attachment of the BCA to the MWCNTs could be shown by thermogravimetric analysis (TGA) and via fluorescence spectroscopy. Model compounds were applied containing either only the oxazoline or the benzoxazinone group to show that the better electrical properties in the PA12-MWCNT composites were a result of a covalent bond between the polymer and the nanotube which only takes place when the BCA was used. In addition, significantly higher electrical conductivity values were obtained by the addition of BCA as well with amino functionalized as with nonmodified commercial MWCNTs. This surprising result was attributed to the significant hydroxy group content on the surface of those commercial MWCNTs. © 2013 Elsevier Ltd. All rights reserved.
Characterization of the state of dispersion of carbon nanotubes in polymer nanocomposites
2011, Buschhorn, Samuel T., Wichmann, Malte H. G., Sumfleth, Jan, Schulte, Karl, Pegel, Sven, Kasaliwal, Gaurav R., Villmow, Tobias, Krause, Beate, Göldel, Andreas, Pötschke, Petra
A 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.
Aspect ratio effects of multi-walled carbon nanotubes on electrical, mechanical, and thermal properties of polycarbonate/MWCNT composites
2014, Guo, Jiaxi, Liu, Yanjun, Prada-Silvy, Ricardo, Tan, Yongqiang, Azad, Samina, Krause, Beate, Pötschke, Petra, Grady, Brian P.
Two multi-walled carbon nanotubes (MWCNTs) having relatively high aspect ratios of 313 and 474 with approximately the same diameter were melt mixed with polycarbonate (PC) in a twin-screw conical micro compounder. The effects of aspect ratio on the electrical, mechanical, and thermal properties of the PC/MWCNT composites were investigated. Electrical conductivities and storage moduli of the filled samples are found to be independent of the starting aspect ratio for these high aspect ratio tubes; although the conductivities and storage moduli are still significantly higher than values of composites made with nanotubes having more commercially common aspect ratios of ∼100. Transmission electron microscopy results suggest that melt-mixing reduces these longer nanotubes to the same length, but still approximately two times longer than the length of commercially common aspect ratio tubes after melt-mixing. Molecular weight measurements show that during melt-mixing the longer nanotubes significantly degrade the molecular weight of the polymer as compared to very similar nanotubes with aspect ratio ∼100. Because of the molecular weight reduction glass transition temperatures predictably show a large decrease with increasing nanotube concentration. © 2013 Wiley Periodicals, Inc.
Dispersability of multiwalled carbon nanotubes in polycarbonate-chloroform solutions
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.
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