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Now showing 1 - 10 of 28
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    Melt-mixed PP/MWCNT composites: Influence of CNT incorporation strategy and matrix viscosity on filler dispersion and electrical resistivity
    (Basel : MDPI, 2019) Pötschke, Petra; Mothes, Fanny; Krause, Beate; Voit, Brigitte
    Small-scale melt mixing was performed for composites based on polypropylene (PP) and 0.5–7.5 wt % multiwalled carbon nanotubes (MWCNT) to determine if masterbatch (MB) dilution is a more effective form of nanofiller dispersion than direct nanotube incorporation. The methods were compared using composites of five different PP types, each filled with 2 wt % MWCNTs. After the determination of the specific mechanical energy (SME) input in the MB dilution process, the direct-incorporation mixing time was adjusted to achieve comparable SME values. Interestingly, the electrical resistivity of MB-prepared samples with 2 wt % MWCNTs was higher than that of those prepared using direct incorporation—despite their better dispersion—suggesting more pronounced MWCNT shortening in the two-step procedure. In summary, this study on PP suggests that the masterbatch approach is suitable for the dispersion of MWCNTs and holds advantages in nanotube dispersion, albeit at the cost of slightly increased electrical resistivity.
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    Characterization of highly filled PP/graphite composites for adhesive joining in fuel cell applications
    (Basel : MDPI, 2019) Rzeczkowski, Piotr; Krause, Beate; Pötschke, Petra
    In order to evaluate the suitability of graphite composite materials for use as bipolar plates in fuel cells, polypropylene (PP) was melt compounded with expanded graphite as conductive filler to form composites with different filler contents of 10–80 wt %. Electrical resistivity, thermal conductivity, and mechanical properties were measured and evaluated as a function of filler content. The electrical and thermal conductivities increased with filler content. Tensile and flexural strengths decreased with the incorporation of expanded graphite in PP. With higher graphite contents, however, both strength values remained more or less unchanged and were below the values of pure PP. Young’s-modulus and flexural modulus increased almost linearly with increasing filler content. The results of the thermogravimetric analysis confirmed the actual filler content in the composite materials. In order to evaluate the wettability and suitability for adhesive joining of graphite composites, contact angle measurements were conducted and surface tensions of composite surfaces were calculated. The results showed a significant increase in the surface tension of graphite composites with increasing filler content. Furthermore, graphite composites were adhesively joined and the strength of the joints was evaluated in the lap-shear test. Increasing filler content in the substrate material resulted in higher tensile lap-shear strength. Additionally, the influence of surface treatment (plasma and chemical) on surface tension and tensile lap-shear strength was investigated. The surface treatment led to a significant improvement of both properties.
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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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    The influence of the blend ratio in PA6/PA66/MWCNT blend composites on the electrical and thermal properties
    (Basel : MDPI, 2019) Krause, Beate; Kroschwald, Lisa; Pötschke, Petra
    It is known that the percolation threshold of polyamide 6 (PA6)/multiwalled carbon nanotube (MWCNT) composites is higher than that of PA66/MWCNT composites under the same mixing conditions and melt viscosity. A series of blends of PA6 and PA66 containing 1 wt % MWCNTs have been prepared to investigate this phenomenon. At contents up to 20 wt % PA66, the blends were not electrically conductive. The electrical resistivity dropped to 109 Ohm∙cm for PA66/PA6 30/70 blends. The resistivity was 105 Ohm∙cm at higher PA66 contents. Differential scanning calorimetry was used to investigate the thermal behavior of blends. The glass transition temperature was almost constant for all blend compositions, indicating that the amorphous phases are miscible. The MWCNT addition influenced the crystallization of PA66 much more than the PA6 crystallization. A heterogeneous crystallization of the polyamide in PA66/PA6 blends took place, and the MWCNTs were mainly localized in the earlier crystallizing PA66 phase. Thus, the formation of the nanotube network and thus the electrical volume resistivity of the PA6/PA66 blends with 1 wt % MWCNTs is significantly influenced by the crystallization behavior. In PA66/PA6 blends up to 60 wt %, the more expensive PA66 can be replaced by the cheaper PA6 while retaining its electrical properties
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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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    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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    Direction dependent electrical conductivity of polymer/carbon filler composites
    (Basel : MDPI, 2019) Kunz, Karina; Krause, Beate; Kretzschmar, Bernd; Juhasz, Levente; Kobsch, Oliver; Jenschke, Wolfgang; Ullrich, Mathias; Pötschke, Petra
    The method of measuring electrical volume resistivity in different directions was applied to characterize the filler orientation in melt mixed polymer composites containing different carbon fillers. For this purpose, various kinds of fillers with different geometries and aspect ratios were selected, namely carbon black (CB), graphite (G) and expanded graphite (EG), branched multiwalled carbon nanotubes (b-MWCNTs), non-branched multiwalled carbon nanotubes (MWCNTs), and single-walled carbon nanotubes (SWCNTs). As it is well known that the shaping process also plays an important role in the achieved electrical properties, this study compares results for compression molded plates with random filler orientations in the plane as well as extruded films, which have, moreover, conductivity differences between extrusion direction and perpendicular to the plane. Additionally, the polymer matrix type (poly (vinylidene fluoride) (PVDF), acrylonitrile butadiene styrene (ABS), polyamide 6 (PA6)) and filler concentration were varied. For the electrical measurements, a device able to measure the electrical conductivity in two directions was developed and constructed. The filler orientation was analyzed using the ratio σin/th calculated as in-plane conductivity σin-plane (σin) divided by through-plane conductivity σthrough-plane (σth). The ratio σin/th is expected to increase with more pronounced filler orientation in the processing direction. In the extruded films, alignment within the plane was assigned by dividing the in-plane conductivity in the extrusion direction (x) by the in-plane conductivity perpendicular to the extrusion direction (y). The conductivity ratios depend on filler type and concentration and are higher the higher the filler aspect ratio and the closer the filler content is to the percolation concentration.
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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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    Electrical, 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, Petra
    Five 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.