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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.
- ItemLightweight polymer-carbon composite current collector for lithium-ion batteries(Basel : MDPI, 2020) Fritsch, Marco; Coeler, Matthias; Kunz, Karina; Krause, Beate; Marcinkowski, Peter; Pötschke, Petra; Wolter, Mareike; Michaelis, AlexanderA hermetic dense polymer-carbon composite-based current collector foil (PCCF) for lithium-ion battery applications was developed and evaluated in comparison to state-of-the-art aluminum (Al) foil collector. Water-processed LiNi0.5Mn1.5O4 (LMNO) cathode and Li4Ti5O12 (LTO) anode coatings with the integration of a thin carbon primer at the interface to the collector were prepared. Despite the fact that the laboratory manufactured PCCF shows a much higher film thickness of 55 µm compared to Al foil of 19 µm, the electrode resistance was measured to be by a factor of 5 lower compared to the Al collector, which was attributed to the low contact resistance between PCCF, carbon primer and electrode microstructure. The PCCF-C-primer collector shows a sufficient voltage stability up to 5 V vs. Li/Li+ and a negligible Li-intercalation loss into the carbon primer. Electrochemical cell tests demonstrate the applicability of the developed PCCF for LMNO and LTO electrodes, with no disadvantage compared to state-of-the-art Al collector. Due to a 50% lower material density, the lightweight and hermetic dense PCCF polymer collector offers the possibility to significantly decrease the mass loading of the collector in battery cells, which can be of special interest for bipolar battery architectures. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.
- ItemExperimental and computational analysis of thermoelectric modules based on melt-mixed polypropylene composites(Amsterdam : Elsevier, 2023) Doraghi, Qusay; Żabnieńska-Góra, Alina; Norman, Les; Krause, Beate; Pötschke, Petra; Jouhara, HussamResearchers are constantly looking for new materials that exploit the Seebeck phenomenon to convert heat into electrical energy using thermoelectric generators (TEGs). New lead-free thermoelectric materials are being investigated as part of the EU project InComEss, with one of the anticipated uses being converting wasted heat into electric energy. Such research aims to reduce the production costs as well as the environmental impact of current TEG modules which mostly employ bismuth for their construction. The use of polymers that, despite lower efficiency, achieve increasingly higher values of electrical conductivity and Seebeck coefficients at a low heat transfer coefficient is increasingly discussed in the literature. This article presents two thermoelectric generator (TEG) models based on data previously described in the literature. Two types of designs are presented: consisting of 4- and 49-leg pairs of p- and n-type composites based on polypropylene melt-mixed with single-walled carbon nanotubes. The models being developed using COMSOL Multiphysics software and validated based on measurements carried out in the laboratory. Based on the results of the analysis, conductive polymer composites employing insulating matrices can be considered as a promising material of the future for TEG modules.
- ItemNitrogen-Doped Carbon Nanotube/Polypropylene Composites with Negative Seebeck Coefficient(Basel : MDPI, 2020) Krause, Beate; Konidakis, Ioannis; Arjmand, Mohammad; Sundararaj, Uttandaraman; Fuge, Robert; Liebscher, Marco; Hampel, Silke; Klaus, Maxim; Serpetzoglou, Efthymis; Stratakis, Emmanuel; Pötschke, PetraThis study describes the application of multi-walled carbon nanotubes that were nitrogen-doped during their synthesis (N-MWCNTs) in melt-mixed polypropylene (PP) composites. Different types of N-MWCNTs, synthesized using different methods, were used and compared. Four of the five MWCNT grades showed negative Seebeck coefficients (S), indicating n-type charge carrier behavior. All prepared composites (with a concentration between 2 and 7.5 wt% N-MWCNTs) also showed negative S values, which in most cases had a higher negative value than the corresponding nanotubes. The S values achieved were between 1.0 µV/K and −13.8 µV/K for the N-MWCNT buckypapers or powders and between −4.7 µV/K and −22.8 µV/K for the corresponding composites. With a higher content of N-MWCNTs, the increase in electrical conductivity led to increasing values of the power factor (PF) despite the unstable behavior of the Seebeck coefficient. The highest power factor was achieved with 4 wt% N-MWCNT, where a suitable combination of high electrical conductivity and acceptable Seebeck coefficient led to a PF value of 6.1 × 10−3 µW/(m·K2). First experiments have shown that transient absorption spectroscopy (TAS) is a useful tool to study the carrier transfer process in CNTs in composites and to correlate it with the Seebeck coefficient.
- 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
- 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.
- 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.
- ItemInfluence of Polyvinylpyrrolidone on Thermoelectric Properties of Melt-Mixed Polymer/Carbon Nanotube Composites(Basel : MDPI, 2023) Krause, Beate; Imhoff, Sarah; Voit, Brigitte; Pötschke, PetraFor thermoelectric applications, both p- and n-type semi-conductive materials are combined. In melt-mixed composites based on thermoplastic polymers and carbon nanotubes, usually the p-type with a positive Seebeck coefficient (S) is present. One way to produce composites with a negative Seebeck coefficient is to add further additives. In the present study, for the first time, the combination of single-walled carbon nanotubes (SWCNTs) with polyvinylpyrrolidone (PVP) in melt-mixed composites is investigated. Polycarbonate (PC), poly(butylene terephthalate) (PBT), and poly(ether ether ketone) (PEEK) filled with SWCNTs and PVP were melt-mixed in small scales and thermoelectric properties of compression moulded plates were studied. It could be shown that a switch in the S-value from positive to negative values was only possible for PC composites. The addition of 5 wt% PVP shifted the S-value from 37.8 µV/K to −31.5 µV/K (2 wt% SWCNT). For PBT as a matrix, a decrease in the Seebeck coefficient from 59.4 µV/K to 8.0 µV/K (8 wt% PVP, 2 wt% SWCNT) could be found. In PEEK-based composites, the S-value increased slightly with the PVP content from 48.0 µV/K up to 54.3 µV/K (3 wt% PVP, 1 wt% SWCNT). In addition, the long-term stability of the composites was studied. Unfortunately, the achieved properties were not stable over a storage time of 6 or 18 months. Thus, in summary, PVP is not suitable for producing long-term stable, melt-mixed n-type SWCNT composites.
- ItemThermoelectric Properties of N-Type Poly (Ether Ether Ketone)/Carbon Nanofiber Melt-Processed Composites(Basel : MDPI, 2022) Paleo, Antonio Jose; Krause, Beate; Soares, Delfim; Melle-Franco, Manuel; Muñoz, Enrique; Pötschke, Petra; Rocha, Ana MariaThe thermoelectric properties, at temperatures from 30 °C to 100 °C, of melt-processed poly(ether ether ketone) (PEEK) composites prepared with 10 wt.% of carbon nanofibers (CNFs) are discussed in this work. At 30 °C, the PEEK/CNF composites show an electrical conductivity (σ) of ~27 S m−1 and a Seebeck coefficient (S) of −3.4 μV K−1, which means that their majority charge carriers are electrons. The origin of this negative Seebeck is deduced because of the impurities present in the as-received CNFs, which may cause sharply varying and localized states at approximately 0.086 eV above the Fermi energy level (EF) of CNFs. Moreover, the lower S, in absolute value, found in PEEK/CNF composites, when compared with the S of as-received CNFs (−5.3 μV K−1), is attributed to a slight electron withdrawing from the external layers of CNFs by the PEEK matrix. At temperatures from 30 °C to 100 °C, the σ (T) of PEEK/CNF composites, in contrast to the σ (T) of as-received CNFs, shows a negative temperature effect, understood through the 3D variable-range hopping (VRH) model, as a thermally activated hopping mechanism across a random network of potential wells. Moreover, their nonlinear S (T) follows the same behavior reported before for polypropylene composites melt-processed with similar CNFs at the same interval of temperatures.