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- 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.
- ItemCharacterization of highly filled PP/graphite composites for adhesive joining in fuel cell applications(Basel : MDPI, 2019) Rzeczkowski, Piotr; Krause, Beate; Pötschke, PetraIn 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.
- 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.
- 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 force of MOFs: The potential of switchable metal-organic frameworks as solvent stimulated actuators(Cambridge : RSC, 2020) Freund, Pascal; Senkovska, Irena; Zheng, Bin; Bon, Volodymyr; Krause, Beate; Maurin, Guillaume; Kaskel, StefanWe evaluate experimentally the force exerted by flexible metal-organic frameworks through expansion for a representative model system, namely MIL-53(Al). The results obtained are compared with data collected from intrusion experiments while molecular simulations are performed to shed light on the re-opening of the guest-loaded structure. The critical impact of the transition stimulating medium on the magnitude of the expansion force is demonstrated.
- ItemThe 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, PetraIt 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
- ItemImpact 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, UttandaramanEmploying 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.
- ItemEffect of filler synergy and cast film extrusion parameters on extrudability and direction-dependent conductivity of PVDF/carbon nanotube/carbon black composites(Basel : MDPI, 2020) Krause, Beate; Kunz, Karina; Kretzschmar, Bernd; Kühnert, Ines; Pötschke, PetraIn the present study, melt-mixed composites based of poly (vinylidene fluoride) (PVDF) and fillers with different aspect ratios (carbon nanotubes (CNTs), carbon black (CB)) and their mixtures in composites were investigated whereby compression-molded plates were compared with melt-extruded films. The processing-related orientation of CNTs with a high aspect ratio leads to direction-dependent electrical and mechanical properties, which can be reduced by using mixed filler systems with the low aspect ratio CB. An upscaling of melt mixing from small scale to laboratory scale was carried out. From extruded materials, films were prepared down to a thickness of 50 µm by cast film extrusion under variation of the processing parameters. By combining CB and CNTs in PVDF, especially the electrical conductivity through the film could be increased compared to PVDF/CNT composites due to additional contact points in the sample thickness. The alignment of the fillers in the two directions within the films was deduced from the differences in electrical and mechanical film properties, which showed higher values in the extrusion direction than perpendicular to it.
- ItemCuxCo1-xFe2O4 (x = 0.33, 0.67, 1) Spinel Ferrite Nanoparticles Based Thermoplastic Polyurethane Nanocomposites with Reduced Graphene Oxide for Highly Efficient Electromagnetic Interference Shielding(Basel : Molecular Diversity Preservation International (MDPI), 2022-2-26) Anju; Yadav, Raghvendra Singh; Pötschke, Petra; Pionteck, Jürgen; Krause, Beate; Kuřitka, Ivo; Vilčáková, Jarmila; Škoda, David; Urbánek, Pavel; Machovský, Michal; Masař, Milan; Urbánek, MichalCuxCo1-x Fe2O4 (x = 0.33,0.67,1)-reduced graphene oxide (rGO)-thermoplastic polyurethane (TPU) nanocomposites exhibiting highly efficient electromagnetic interference (EMI) shielding were prepared by a melt-mixing approach using a microcompounder. Spinel ferrite Cu0.33Co0.67Fe2O4 (Cu-CoF1), Cu0.67Co0.33Fe2O4 (CuCoF2) and CuFe2O4 (CuF3) nanoparticles were synthesized using the sonochemical method. The CuCoF1 and CuCoF2 exhibited typical ferromagnetic features, whereas CuF3 displayed superparamagnetic characteristics. The maximum value of EMI total shielding effectiveness (SEt) was noticed to be 42.9 dB, 46.2 dB, and 58.8 dB for CuCoF1-rGO-TPU, CuCoF2-rGO-TPU, and CuF3-rGO-TPU nanocomposites, respectively, at a thickness of 1 mm. The highly efficient EMI shielding performance was attributed to the good impedance matching, conductive, dielectric, and magnetic loss. The demonstrated nanocomposites are promising candidates for a lightweight, flexible, and highly efficient EMI shielding material.
- 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.