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- ItemA 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, PetraAn 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.
- ItemElectrical 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, PetraElectrical 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
- ItemHybrid 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, AmirConductive 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.
- ItemAchieving electrical conductive tracks by laser treatment of non-conductive polypropylene/polycarbonate blends filled with MWCNTs(Weinheim : Wiley-VCH, 2014) Liebscher, Marco; Krause, Beate; Pötschke, Petra; Barz, Andrea; Bliedtner, Jens; Möhwald, Michael; Letzsch, AlexanderElectrical 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.
- ItemComparative study of singlewalled, multiwalled, and branched carbon nanotubes melt mixed in different thermoplastic matrices(Oxford : Elsevier Science, 2018) Krause, Beate; Barbier, Carine; Kunz, Karina; Pötschke, PetraIn this contribution, three different types of CNTs, namely single-walled (SWCNT), multi-walled (MWCNT) and branched MWCNTs were melt mixed in amounts of 0.1–10 wt.-% in polypropylene (PP), polycarbonate (PC) and poly(vinylidene fluoride) (PVDF) using a small-scale microcompounder. The filler dispersion of compression-moulded samples was characterized using light and electron microscopy, and the electrical and thermal properties were measured. The lowest electrical percolation thresholds were found for composites of PP/SWCNT, PP/branched MWCNT and PC/branched MWCNT, which percolated already at <0.1 wt.-% CNT loading. Low values of electrical volume resistivity of about 3 Ohm·cm (PVDF), 7 Ohm·cm (PP) and 2 Ohm·cm (PC) could be reached when loading with 2 wt.-% branched MWCNT. A homogeneous dispersion in the macro- and microlevel was observed especially for composites containing branched MWCNTs. For all CNT types, a matrix nucleation effect was found in PP and PVDF using differential scanning calorimetry.
- ItemInfluence 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, PetraLinear 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.
- ItemMelt mixed PCL/MWCNT composites prepared at different rotation speeds: Characterization of rheological, thermal, and electrical properties, molecular weight, MWCNT macrodispersion, and MWCNT length distribution(Oxford : Elsevier Science, 2013) Pötschke, Petra; Villmow, Tobias; Krause, BeateComposites 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.
- ItemPolypropylene-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, PetraThe 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.
- ItemThe influence of matrix viscosity on MWCNT dispersion and electrical properties in different thermoplastic nanocomposites(Oxford : Elsevier Science, 2012) Socher, Robert; Krause, Beate; Müller, Michael T.; Boldt, Regine; Pötschke, PetraComposites of MWCNTs having each three different levels of matrix viscosity with five different polymers (polyamide 12, polybutylene terephthalate, polycarbonate, polyetheretherketone and low density polyethylene) were melt mixed to identify the general influence of matrix viscosity on the electrical properties and the state of MWCNT dispersion. Huge differences in the electrical percolation thresholds were found using the same polymer matrix with different viscosity grades. The lowest percolation thresholds were always found in the composites based on the low viscosity matrix. The state of primary MWCNT agglomerate dispersion increased with increasing matrix viscosity due to the higher input of mixing energy. TEM investigations showed nanoagglomerated structures in the low viscosity samples which are obviously needed to achieve low resistivity values. The effect of nanotube shortening was quantified using two different viscosity grades of polycarbonate. Due to the higher mixing energy input the nanotube shortening was more pronounced in the high viscosity matrix which partially explains the higher percolation threshold. © 2011 Elsevier Ltd. All rights reserved.
- ItemEffects of high energy electrons on the properties of polyethylene / multiwalled carbon nanotubes composites: Comparison of as-grown and oxygen-functionalised MWCNT(Melville, NY : AIP, 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.