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- 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.
- 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.
- 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.
- ItemThermal conductivity and electrical resistivity of melt-mixed polypropylene composites containing mixtures of carbon-based fillers(Basel : MDPI, 2019) Krause, Beate; Rzeczkowski, Piotr; Pötschke, PetraMelt-mixed composites based on polypropylene (PP) with various carbon-based fillers were investigated with regard to their thermal conductivity and electrical resistivity. The composites were filled with up to three fillers by selecting combinations of graphite nanoplatelets (GNP), carbon fibers (CF), carbon nanotubes (CNT), carbon black (CB), and graphite (G) at a constant filler content of 7.5 vol%. The thermal conductivity of PP (0.26 W/(m·K)) improved most using graphite nanoplatelets, whereas electrical resistivity was the lowest when using multiwalled CNT. Synergistic effects could be observed for different filler combinations. The PP composite, which contains a mixture of GNP, CNT, and highly structured CB, simultaneously had high thermal conductivity (0.5 W/(m·K)) and the lowest electrical volume resistivity (4 Ohm·cm).
- 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.
- ItemMixed Carbon Nanomaterial/Epoxy Resin for Electrically Conductive Adhesives(Basel : MDPI, 2020) Lopes, Paulo E.; Moura, Duarte; Hilliou, Loic; Krause, Beate; Pötschke, Petra; Figueiredo, Hugo; Alves, Ricardo; Lepleux, Emmanuel; Pacheco, Louis; Paiva, Maria C.The increasing complexity of printed circuit boards (PCBs) due to miniaturization, increased the density of electronic components, and demanding thermal management during the assembly triggered the research of innovative solder pastes and electrically conductive adhesives (ECAs). Current commercial ECAs are typically based on epoxy matrices with a high load (>60%) of silver particles, generally in the form of microflakes. The present work reports the production of ECAs based on epoxy/carbon nanomaterials using carbon nanotubes (single and multi-walled) and exfoliated graphite, as well as hybrid compositions, within a range of concentrations. The composites were tested for morphology (dispersion of the conductive nanomaterials), electrical and thermal conductivity, rheological characteristics and deposition on a test PCB. Finally, the ECA’s shelf life was assessed by mixing all the components and conductive nanomaterials, and evaluating the cure of the resin before and after freezing for a time range up to nine months. The ECAs produced could be stored at −18 °C without affecting the cure reaction.
- ItemThermoelectric Performance of Polypropylene/Carbon Nanotube/Ionic Liquid Composites and Its Dependence on Electron Beam Irradiation(Basel : MDPI, 2022-1-11) Voigt, Oliver; Krause, Beate; Pötschke, Petra; Müller, Michael T.; Wießner, SvenThe thermoelectric behavior of polypropylene (PP) based nanocomposites containing single walled carbon nanotubes (SWCNTs) and five kinds of ionic liquids (Ils) dependent on composite composition and electron beam irradiation (EB) was studied. Therefore, several samples were melt-mixed in a micro compounder, while five Ils with sufficiently different anions and/or cations were incorporated into the PP/SWCNT composites followed by an EB treatment for selected composites. Extensive investigations were carried out considering the electrical, thermal, mechanical, rheological, morphological and, most significantly, thermoelectric properties. It was found that it is possible to prepare n-type melt-mixed polymer composites from p-type commercial SWCNTs with relatively high Seebeck coefficients when adding four of the selected Ils. The highest Seebeck coefficients achieved in this study were +49.3 µV/K (PP/2 wt.% SWCNT) for p-type composites and −27.6 µV/K (PP/2 wt.% SWCNT/4 wt.% IL type AMIM Cl) for n-type composites. Generally, the type of IL is decisive whether p-or n-type thermoelectric behavior is achieved. After IL addition higher volume conductivity could be reached. Electron beam treatment of PP/SWCNT leads to increased values of the Seebeck coefficient, whereas the EB treated sample with IL (AMIM Cl) shows a less negative Seebeck coefficient value.
- ItemDoes the Type of Polymer and Carbon Nanotube Structure Control the Electromagnetic Shielding in Melt-Mixed Polymer Nanocomposites?(Basel : MDPI, 2020-1-15) Biswas, Sourav; Muzata, Tanyaradzwa S.; Krause, Beate; Rzeczkowski, Piotr; Pötschke, Petra; Bose, SuryasarathiA suitable polymer matrix and well dispersed conducting fillers forming an electrically conducting network are the prime requisites for modern age electromagnetic shield designing. An effective polymer-based shield material is designed that can attenuate 99.9% of incident electromagnetic (EM) radiation at a minimum thickness of <0.5 mm. This is accomplished by the choice of a suitable partially crystalline polymer matrix while comparing non-polar polypropylene (PP) with polar polyvinylidene fluoride (PVDF) and a best suited filler nanomaterial by comparing different types of carbon nanotubes such as; branched, single-walled and multi-walled carbon nanotubes, which were added in only 2 wt %. Different types of interactions (polar-polar and CH-π and donor-acceptor) make b-MWCNT more dispersible in the PVDF matrix, which together with high crystallinity resulted in the best electrical conductivity and electromagnetic shielding ability of this composite. This investigation additionally conceals the issues related to the thickness of the shield material just by stacking individual thin nanocomposite layers containing different carbon nanotube (CNT) types with 0.3 mm thickness in a simple manner and finally achieves 99.999% shielding efficiency at just 0.9 mm thickness when using a suitable order of the different PVDF based nanocomposites.
- 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.
- 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