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- ItemTuneable Dielectric Properties Derived from Nitrogen-Doped Carbon Nanotubes in PVDF-Based Nanocomposites(Washington, DC : ACS Publications, 2018) Pawar, Shital Patangrao; Arjmand, Mohammad; Pötschke, Petra; Krause, Beate; Fischer, Dieter; Bose, Suryasarathi; Sundararaj, UttandaramanNitrogen-doped multiwall carbon nanotubes (N-MWNTs) with different structures were synthesized by employing chemical vapor deposition and changing the argon/ethane/nitrogen gas precursor ratio and synthesis time, and broadband dielectric properties of their poly(vinylidene fluoride) (PVDF)-based nanocomposites were investigated. The structure, morphology, and electrical conductivity of synthesized N-MWNTs were assessed via Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy, and powder conductivity techniques. The melt compounded PVDF nanocomposites manifested significantly high real part of the permittivity (ϵ′) along with low dissipation factor (tan δϵ) in 0.1 kHz to 1 MHz frequency range, suggesting use as efficient charge-storage materials. Longer synthesis time resulted in enhanced carbon purity as well as higher thermal stability, determined via TGA analysis. The inherent electrical conductivity of N-MWNTs scaled with the carbon purity. The charge-storage ability of the developed PVDF nanocomposites was commensurate with the amount of the nitrogen heteroatom (i.e., self-polarization), carbon purity, and inherent electrical conductivity of N-MWNTs and increased with better dispersion of N-MWNTs in PVDF.
- ItemGraphene Derivatives Doped with Nickel Ferrite Nanoparticles as Excellent Microwave Absorbers in Soft Nanocomposites(Weinheim : Wiley-VCH, 2017) Pawar, Shital Patangrao; Gandi, Mounika; Arief, Injamamul; Krause, Beate; Pötschke, Petra; Bose, SuryasarathiHerein, we report the development of soft polymeric composites containing multiwall carbon nanotubes (MWNTs, 1–3 wt%) and graphene derivatives doped with nickel ferrite nanoparticles (rGO@NF, 10 wt%) as lightweight microwave absorbers. The soft nanocomposites were designed using melt-mixed blends of varying compositions of PC (polycarbonate) and SAN (poly styrene acrylonitrile) by compartmentalized functional nanoparticles in one of the components of the blend (here PC). Maximum attenuation of the incoming electromagnetic (EM) radiation mainly through absorption was achieved. The hetero-dielectric media at microscopic length scale in the PC component provided large interfaces which facilitated multiple scattering thereby attenuating the incoming EM radiation. This strategy of positioning the functional nanoparticles in one of the components in the blends resulted in significantly enhanced shielding effectiveness (SE), at any given concentration of MWNTs, in contrast to PC based composites. This enhancement in SE was realized in the special morphology of the bicomponent PC/SAN=60/40 wt% blends where both the components are continuous. The enhanced SE in co-continuous blends is due to combined effect of enhanced electrical conductivity (more precisely due to interconnected network of the nanoparticles) and the presence of a hetero-dielectric media generating large scattering interfaces. For instance, the PC/SAN (60/40 wt%) co-continuous blend containing 3 wt% MWNTs and 10 wt% rGO@NF manifested in a total shielding effectiveness (SET) of −32.3 dB (i. e. more than 99.9 % attenuation of incoming EM radiation) mainly through absorption.
- 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
- ItemScreening of Different Carbon Nanotubes in Melt-Mixed Polymer Composites with Different Polymer Matrices for Their Thermoelectrical Properties(Basel : MDPI, 2019-12-7) Krause, Beate; Barbier, Carine; Levente, Juhasz; Klaus, Maxim; Pötschke, PetraThe aim of this study is to reveal the influences of carbon nanotube (CNT) and polymer type as well as CNT content on electrical conductivity, Seebeck coefficient (S), and the resulting power factor (PF) and figure of merit (ZT). Different commercially available and laboratory made CNTs were used to prepare melt-mixed composites on a small scale. CNTs typically lead to p-type composites with positive S-values. This was found for the two types of multi-walled CNTs (MWCNT) whereby higher Seebeck coefficient in the corresponding buckypapers resulted in higher values also in the composites. Nitrogen doped MWCNTs resulted in negative S-values in the buckypapers as well as in the polymer composites. When using single-walled CNTs (SWCNTs) with a positive S-value in the buckypapers, positive (polypropylene (PP), polycarbonate (PC), poly (vinylidene fluoride) (PVDF), and poly(butylene terephthalate) (PBT)) or negative (polyamide 66 (PA66), polyamide 6 (PA6), partially aromatic polyamide (PARA), acrylonitrile butadiene styrene (ABS)) S-values were obtained depending on the matrix polymer and SWCNT type. The study shows that the direct production of n-type melt-mixed polymer composites from p-type commercial SWCNTs with relatively high Seebeck coefficients is possible. The highest Seebeck coefficients obtained in this study were 66.4 µV/K (PBT/7 wt % SWCNT Tuball) and −57.1 µV/K (ABS/0.5 wt % SWCNT Tuball) for p-and n-type composites, respectively. The highest power factor and ZT of 0.28 µW/m·K2 and 3.1 × 10−4, respectively, were achieved in PBT with 4 wt % SWCNT Tuball.
- 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.
- 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).
- ItemComparative study of singlewalled, multiwalled, and branched carbon nanotubes melt mixed in different thermoplastic matrices(Oxford : Elsevier Science, 2018) Krause, Beate; Barbier, Carine; Kunz, Karina; Pötschke, PetraIn this contribution, three different types of CNTs, namely single-walled (SWCNT), multi-walled (MWCNT) and branched MWCNTs were melt mixed in amounts of 0.1–10 wt.-% in polypropylene (PP), polycarbonate (PC) and poly(vinylidene fluoride) (PVDF) using a small-scale microcompounder. The filler dispersion of compression-moulded samples was characterized using light and electron microscopy, and the electrical and thermal properties were measured. The lowest electrical percolation thresholds were found for composites of PP/SWCNT, PP/branched MWCNT and PC/branched MWCNT, which percolated already at <0.1 wt.-% CNT loading. Low values of electrical volume resistivity of about 3 Ohm·cm (PVDF), 7 Ohm·cm (PP) and 2 Ohm·cm (PC) could be reached when loading with 2 wt.-% branched MWCNT. A homogeneous dispersion in the macro- and microlevel was observed especially for composites containing branched MWCNTs. For all CNT types, a matrix nucleation effect was found in PP and PVDF using differential scanning calorimetry.
- ItemHybrid conductive filler/polycarbonate composites with enhanced electrical and thermal conductivities for bipolar plate applications(Manchester, NH : Wiley, 2019) Naji, Ahmed; Krause, Beate; Pötschke, Petra; Ameli, AmirConductive polymer composites (CPCs) with high electrical and thermal conductivities are demanded for bipolar plates of fuel cells. In this work, CPCs of polycarbonate (PC) filled with carbon nanotube (CNT), carbon fiber (CF), graphite (G), and their double and triple hybrids were prepared using solution casting method followed by compression molding. The results showed that the electrical percolation thresholds for the PC-CNT and PC-CF were ~1 wt% and ~10 wt%, respectively, while no clear threshold was found for PC-G composites. Addition of 3–5 wt% CNT improved the electrical conductivity of PC-CF and PC-G systems up to 6 orders of magnitude and enhanced the thermal conductivity as much as 65%. The results of triple hybrid CPCs (with constant loading of 63 wt%) indicated that the combination of highest electrical and thermal conductivities is achieved when the CF and CNT loadings were near their percolation thresholds. Therefore, a triple filler system of 3 wt% CNT, 10 wt% CF, and 50 wt% G resulted in a composite with the through-plane and in-plane electrical conductivity, and thermal conductivity values of 12.8 S/cm, 8.3 S/cm, and 1.7 W/m•K, respectively. The results offer a combination of properties surpassing the existing values and suitable for high-conductivity applications such as bipolar plates. POLYM. COMPOS., 40:3189–3198, 2019. © 2018 Society of Plastics Engineers.
- ItemElectrically Conductive Polyetheretherketone Nanocomposite Filaments: From Production to Fused Deposition Modeling(Basel : MDPI, 2018-8-18) Gonçalves, Jordana; Lima, Patrícia; Krause, Beate; Pötschke, Petra; Lafont, Ugo; Gomes, José R.; Abreu, Cristiano S.; Paiva, Maria C.; Covas, José A.The present work reports the production and characterization of polyetheretherketone (PEEK) nanocomposite filaments incorporating carbon nanotubes (CNT) and graphite nanoplates (GnP), electrically conductive and suitable for fused deposition modeling (FDM) processing. The nanocomposites were manufactured by melt mixing and those presenting electrical conductivity near 10 S/m were selected for the production of filaments for FDM. The extruded filaments were characterized for mechanical and thermal conductivity, polymer crystallinity, thermal relaxation, nanoparticle dispersion, thermoelectric effect, and coefficient of friction. They presented electrical conductivity in the range of 1.5 to 13.1 S/m, as well as good mechanical performance and higher thermal conductivity compared to PEEK. The addition of GnP improved the composites' melt processability, maintained the electrical conductivity at target level, and reduced the coefficient of friction by up to 60%. Finally, three-dimensional (3D) printed test specimens were produced, showing a Young's modulus and ultimate tensile strength comparable to those of the filaments, but a lower strain at break and electrical conductivity. This was attributed to the presence of large voids in the part, revealing the need for 3D printing parameter optimization. Finally, filament production was up-scaled to kilogram scale maintaining the properties of the research-scale filaments.
- ItemAn updated micromechanical model based on morphological characterization of carbon nanotube nanocomposites(Oxford [u.a.] : Elsevier, 2017) Talò, Michela; Krause, Beate; Pionteck, Jürgen; Lanzara, Giulia; Lacarbonara, WalterBy leveraging on extensive morphological analysis of carbon nanotube nanocomposites, an update of the Eshelby-Mori-Tanaka method is proposed for a more accurate estimation of the nanocomposites effective elastic response. The experimental results are employed to overcome the main modeling limitations inherent in most common micromechanical theories, such as the perfect dispersion of the nanofiller and the uniformity of the nanofiller's aspect ratio within the nanocomposite. The actual variability of the CNTs aspect ratio and the CNTs degree of dispersion are experimentally measured and introduced in the proposed model by averaging the Eshelby tensor over the actual CNT lengths distribution and by accounting for the effective CNT volume fraction. The effects of the nanofiller morphology on the mechanical response of three different thermoplastic nanocomposites with low- and high-aspect ratio CNTs are explored, and monotonic tensile tests are performed to validate the predictions of the proposed model. A good agreement is found between the predicted nanocomposites elastic moduli and the experimental data.