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- ItemDevelopment of joining methods for highly filled Graphite/PP composite based bipolar plates for fuel cells: Adhesive joining and welding(Melville, NY : AIP, 2019) Rzeczkowski, P.; Lucia, M.; Müller, A.; Facklam, M.; Cohnen, A.; Schäfer, P.; Hopmann, C.; Hickmann, T.; Pötschke, Petra; Krause, BeateNovel material solutions for bipolar plates in fuel cells require adapted ways of joining and sealing technologies. Safe and life time enduring leak-tight contacts must be achieved by automatic processes using reasonable joint forces. A proper sealing should manage such challenges as good ageing properties, excellent leaktightness, high thermal conductivity and low gas permeability. Hence in this work, adhesive bonding and welding are considered as suitable methods, which can fulfill the requirements mentioned above. Adhesive systems seem to be more easy to apply than conventional sealing (hand layed-up rubber gaskets), e.g. with automatic dispensers. Additionally, the properties of an adhesive joint can be enhanced by a process-specific surface pre-treatment. This work focuses on the characterization of adhesive systems and their joints with highly filled graphite composites. Mechanical properties of the joints were characterized through lap-shear tests. The influence of ageing caused by humidity or acidic solvent at increased temperature on the bond line properties as well as neat adhesive was examined. The thermal conductivities of neat adhesives and through the entire joint were examined. In order to improve above conductivities, roughening, substrate pre-heating, post-curing and various contact pressure weights were applied. Plasma treatment was chosen as surface pre-treatment method for improving substrate's surface energy. An alternative to bonding is plastic welding, which does not require the use of sealants and adhesives. Based on former study of influences of filler content on the welding process using ultrasonic, hot plate or infrared welding, a welding method for joining the graphite compounds was derived.
- ItemElectrical and thermal conductivity of polypropylene filled with combinations of carbon fillers(Melville, NY : AIP, 2016) Krause, Beate; Pötschke, PetraThe thermal and electrical conductivity of polymer composites filled with a low content up to 7.5 vol% of different carbon fillers (carbon nanotubes, carbon fibers, graphite nanoplates) were investigated. It was found that the combination of two or three carbon fillers leads to an increase of thermal conductivity up to 193% which is higher than the sum of the effects of both fillers.
- ItemDoes 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, SuryasarathiElectromagnetic 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.
- 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
- ItemPolymer - Carbon nanotube composites for thermoelectric applications(Melville, NY : AIP, 2017) Luo, J.; Krause, Beate; Pötschke, PetraThe thermoelectric (TE) performance of electrically conductive thermoplastic composites prepared by melt mixing was investigated. A cost effective widely used in industry polymer, namely polypropylene (PP), was chosen as the matrix to fabricate the composites. Singlewalled carbon nanotubes (SWCNTs), the amount (2 wt%) of which was selected to be above the electrical percolation threshold (< 0.2 wt%), were used to form an electrical conducting network. Besides as-produced SWCNTs plasma modified tubes were employed to study the influence of the functionalization on the morphology, dispersion and TE properties of the PP composites. In addition, melt processing conditions, e.g. temperature, rotation speed, and time during mixing in a small-scale compounder were varied. Furthermore, an ionic liquid (IL, 1-methyl-3-octylimidazolium tetrafluoroborate) was used as a processing additive during melt mixing, which was confirmed to improve the electrical conductivity of the composites. Simultaneous increase in the Seebeck coefficient up to a value of 64 μV/K was recorded, leading to a much better power factor of 0.26 μW/(m·K2) compared to composites without IL. This melt mixing strategy opens new avenues for solvent-free, large scale fabrication of polymer based TE materials.
- ItemMethods 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, PetraTwo 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.
- ItemEffect of additives on MWCNT dispersion and electrical percolation in polyamide 12 composites(Melville, NY : AIP, 2017) Socher, Robert; Krause, Beate; Pötschke, PetraThe aim of this study was to decrease the electrical percolation threshold of multiwalled carbon nanotubes (MWCNTs) in a polyamide 12 matrix by the use of additives. Different kinds of additives were selected which either interact with the π-system of the MWCNTs (imidazolium based ionic liquid (IL) and perylene-3,4,9,10-tetracarboxylic dianhydride (PTCDA)) or improve the MWCNT wettability (cyclic butylene terephthalate, CBT). The composites were melt mixed using a DACA microcompounder. The electrical percolation threshold for PA12/MWCNT without additives, measured on compression molded plates, was found between 2.0 and 2.25 wt%. With all used additives, a significant reduction of the electrical percolation threshold could be achieved. Whereas the addition of IL and CBT resulted in MWCNT percolation at around 1.0 wt%, a slightly higher percolation threshold between 1.0 and 1.5 wt% was found for PTCDA as an additive. Interestingly, the electrical resistivity at higher loadings was decreased by nearly two decades when using CBT and one decade after application of PTCDA, whereas IL did not contribute to lower values in this range. In all cases macrodispersion as assessed by light microscopy was not improved and even worse as compared to non-modified composites. In summary, the results illustrate that these kinds of additives are able to improve the performance of PA12 based MWCNT nanocomposites.
- ItemMelt-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, BrigitteSmall-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.
- ItemImprovement 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, KarlThe 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.