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    Does the Processing Method Resulting in Different States of an Interconnected Network of Multiwalled Carbon Nanotubes in Polymeric Blend Nanocomposites Affect EMI Shielding Properties?
    (Washington, DC : ACS Publications, 2018) Pawar, Shital Patangrao; Rzeczkowski, Piotr; Pötschke, Petra; Krause, Beate; Bose, Suryasarathi
    Electromagnetic interference (EMI), an unwanted phenomenon, often affects the reliability of precise electronic circuitry. To prevent this, an effective shielding is prerequisite to protect the electronic devices. In this study, an attempt was made to understand how processing of polymeric blend nanocomposites involving multiwalled carbon nanotubes (MWCNTs) affects the evolving interconnected network structure of MWCNTs and eventually their EMI shielding properties. Thereby, the overall blend morphology and especially the connectivity of the polycarbonate (PC) component, in which the MWCNTs tend to migrate, as well as the perfectness of their migration, and the state of nanotube dispersion are considered. For this purpose, blends of varying composition of PC and poly(methyl methacrylate) were chosen as a model system as they show a phase diagram with lower critical solution temperature type of characteristic. Such blends were processed in two different ways: solution mixing (from the homogeneous state) and melt mixing (in the biphasic state). In both the processes, MWCNTs (3 wt %) were mixed into the blends, and the evolved structures (after phase separation induced by annealing in solution-mixed blends) and the quenched structures (as the blends exit the extruder) were systematically studied using transmission electron microscopy (TEM). Both the set of blends were subjected to the same thermal history, however, under different conditions such as under quiescent conditions (in the case of solution mixing) and under shear (in the case of melt mixing). The electrical volume conductivity and the evolved morphologies of these blend nanocomposites were evaluated and correlated with the measured EMI shielding behavior. The results indicated that irrespective of the type of processing, the MWCNTs localized in the PC component; driven by thermodynamic factors and depending on the blend composition, sea-island, cocontinuous, and phase-inverted structures evolved. Interestingly, the better interconnected network structures of MWCNTs observed using TEM in the solution-mixed samples together with larger nanotube lengths resulted in higher EMI shielding properties (-27 dB at 18 GHz) even if slightly higher electrical volume conductivities were observed in melt-mixed samples. Moreover, the shielding was absorption-driven, facilitated by the dense network of MWCNTs in the PC component of the blends, at any given concentration of nanotubes. Taken together, this study highlights the effects of different blend nanocomposite preparation methods (solution and melt) and the developed morphology and nanotube network structure in MWCNT filled blend nanocomposites on the EMI shielding behavior.
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    Electrical and melt rheological characterization of PC and co-continuous PC/SAN blends filled with CNTs: Relationship between melt-mixing parameters, filler dispersion, and filler aspect ratio
    (Hoboken, NJ [u.a.] : Wiley, 2018) Liebscher, Marco; Domurath, Jan; Krause, Beate; Saphiannikova, Marina; Heinrich, Gert; Pötschke, Petra
    Electrical and melt rheological properties of melt-mixed polycarbonate (PC) and co-continuous PC/poly(styrene–acrylonitrile) (SAN) blends with carbon nanotubes (CNTs) are investigated. Using two sets of mixing parameters, different states of filler dispersion are obtained. With increasing CNT dispersion, an increase in electrical resistivity near the percolation threshold of PC–CNT composites and (PC + CNT)/SAN blends is observed. This suggests that the higher mixing energies required for better dispersion also result in a more severe reduction of the CNT aspect ratio; this effect was proven by CNT length measurements. Melt rheological studies show higher reinforcing effects for composites with worse dispersion. The Eilers equation, describing the melt viscosity as function of filler content, was used to fit the data and to obtain information about an apparent aspect ratio change, which was in accordance with measured CNT length reduction. Such fitting could be also transferred to the blends and serves for a qualitatively based discussion. © 2017 Wiley Periodicals
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    Methods to characterize the dispersability of carbon nanotubes and their length distribution
    (Weinheim : Wiley-VCH Verl., 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.
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    Improvement of carbon nanotube dispersion in thermoplastic composites using a three roll mill at elevated temperatures
    (Barking : Elsevier, 2013) Pötschke, Petra; Krause, Beate; Buschhorn, Samuel T.; Köpke, Ulf; Müller, Michael T.; Villmow, Tobias; Schulte, Karl
    The paper reports the effect of using of a three roll mill as additional dispersion step after twin-screw melt extrusion of nanocomposites containing thermoplastic polymers and multiwalled carbon nanotubes. The three roll milling technology was adapted to elevated temperatures of up to 180 °C and examples are shown for its use in processing of different pre-compounded thermoplastic polymer composites based on polypropylene, polycaprolactone and ethylene-vinyl acetate. The aim is to enhance the state of dispersion achieved by the previous melt extrusion step. In particular, depending on the state of dispersion before three roll milling and the adapted conditions, like number of runs and gap sizes, a reduction of number and size of remaining primary nanotube agglomerates was found. This was studied using light microscopy. The resulting improvements in mechanical properties were assessed and could be attributed to the improved dispersion. In some cases agglomerate free samples could be achieved after the three roll milling process. © 2012 Elsevier Ltd.
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    Tuneable Dielectric Properties Derived from Nitrogen-Doped Carbon Nanotubes in PVDF-Based Nanocomposites
    (Washington, DC : ACS Publications, 2018) Pawar, Shital Patangrao; Arjmand, Mohammad; Pötschke, Petra; Krause, Beate; Fischer, Dieter; Bose, Suryasarathi; Sundararaj, Uttandaraman
    Nitrogen-doped multiwall carbon nanotubes (N-MWNTs) with different structures were synthesized by employing chemical vapor deposition and changing the argon/ethane/nitrogen gas precursor ratio and synthesis time, and broadband dielectric properties of their poly(vinylidene fluoride) (PVDF)-based nanocomposites were investigated. The structure, morphology, and electrical conductivity of synthesized N-MWNTs were assessed via Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy, and powder conductivity techniques. The melt compounded PVDF nanocomposites manifested significantly high real part of the permittivity (ϵ′) along with low dissipation factor (tan δϵ) in 0.1 kHz to 1 MHz frequency range, suggesting use as efficient charge-storage materials. Longer synthesis time resulted in enhanced carbon purity as well as higher thermal stability, determined via TGA analysis. The inherent electrical conductivity of N-MWNTs scaled with the carbon purity. The charge-storage ability of the developed PVDF nanocomposites was commensurate with the amount of the nitrogen heteroatom (i.e., self-polarization), carbon purity, and inherent electrical conductivity of N-MWNTs and increased with better dispersion of N-MWNTs in PVDF.
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    Hybrid conductive filler/polycarbonate composites with enhanced electrical and thermal conductivities for bipolar plate applications
    (Manchester, NH : Wiley, 2019) Naji, Ahmed; Krause, Beate; Pötschke, Petra; Ameli, Amir
    Conductive polymer composites (CPCs) with high electrical and thermal conductivities are demanded for bipolar plates of fuel cells. In this work, CPCs of polycarbonate (PC) filled with carbon nanotube (CNT), carbon fiber (CF), graphite (G), and their double and triple hybrids were prepared using solution casting method followed by compression molding. The results showed that the electrical percolation thresholds for the PC-CNT and PC-CF were ~1 wt% and ~10 wt%, respectively, while no clear threshold was found for PC-G composites. Addition of 3–5 wt% CNT improved the electrical conductivity of PC-CF and PC-G systems up to 6 orders of magnitude and enhanced the thermal conductivity as much as 65%. The results of triple hybrid CPCs (with constant loading of 63 wt%) indicated that the combination of highest electrical and thermal conductivities is achieved when the CF and CNT loadings were near their percolation thresholds. Therefore, a triple filler system of 3 wt% CNT, 10 wt% CF, and 50 wt% G resulted in a composite with the through-plane and in-plane electrical conductivity, and thermal conductivity values of 12.8 S/cm, 8.3 S/cm, and 1.7 W/m•K, respectively. The results offer a combination of properties surpassing the existing values and suitable for high-conductivity applications such as bipolar plates. POLYM. COMPOS., 40:3189–3198, 2019. © 2018 Society of Plastics Engineers.
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    Influence of talc with different particle sizes in melt-mixed LLDPE/MWCNT composites
    (Hoboken, NJ [u.a.] : Wiley, 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.
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    Fe3O4 Nanoparticles Grown on Cellulose/GO Hydrogels as Advanced Catalytic Materials for the Heterogeneous Fenton-like Reaction
    (Washington, DC : ACS Publications, 2019) Chen, Yian; Pötschke, Petra; Pionteck, Jürgen; Voit, Brigitte; Qi, Haisong
    Cellulose/graphene oxide (GO)/iron oxide (Fe3O4) composites were prepared by coprecipitating iron salts onto cellulose/GO hydrogels in a basic solution. X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared, and X-ray diffraction characterization showed that Fe3O4 was successfully coated on GO sheets and cellulose. Cellulose/GO/Fe3O4 composites showed excellent catalytic activity by maintaining almost 98% of the removal of acid orange 7 (AO7) and showed stability over 20 consecutive cycles. This performance is attributable to the synergistic effect of Fe3O4 and GO during the heterogeneous Fenton-like reaction. Especially, the cellulose/GO/Fe3O4 composites preserve their activity by keeping the ratio of Fe3+/Fe2+ at 2 even after 20 catalysis cycles, which is supported by XPS analysis.
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    Influence 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, Petra
    The 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.
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    Comparison of nanotubes produced by fixed bed and aerosol-CVD methods and their electrical percolation behaviour in melt mixed polyamide 6.6 composites
    (Barking : Elsevier, 2010) Krause, Beate; Ritschel, M.; Täschner, C.; Oswald, S.; Gruner, W.; Leonhardt, A.; Pötschke, Petra
    The electrical percolation behaviour of five different kinds of carbon nanotubes (CNTs) synthesised by two CVD techniques was investigated on melt mixed composites based on an insulating polyamide 6.6 matrix. The electrical percolation behaviour was found to be strongly dependent on the properties of CNTs which varied with the synthesis conditions. The lowest electrical percolation threshold (0.04 wt.%) was determined for as grown multi-walled carbon nanotubes without any purification or chemical treatment. Such carbon nanotubes were synthesised by the aerosol method using acetonitrile as ferrocene containing solvent and show relatively low oxygen content near the surface, high aspect ratio, and good dispersability. Similar properties could be found for nanotubes produced by the aerosol method using cyclohexane, whereas CNTs produced by the fixed bed method using different iron contents in the catalyst material showed much higher electrical percolation thresholds between 0.35 and 1.02 wt.%. © 2009 Elsevier Ltd. All rights reserved.