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    Graphene 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, Suryasarathi
    Herein, 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.
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    Effects of synthesis catalyst and temperature on broadband dielectric properties of nitrogen-doped carbon nanotube/polyvinylidene fluoride nanocomposites
    (New York, NY [u.a.] : Pergamon Press, 2016) Ameli, A.; Arjmand, M.; Pötschke, Petra; Krause, Beate; Sundararaj, U.
    This study reports on nitrogen-doped carbon nanotube (N-CNT)/polymer nanocomposites exhibiting relatively high and frequency independent real permittivity (ϵ′) together with low dielectric loss (tan δ). N-CNTs were synthesized by chemical vapor deposition, and their nanocomposites were prepared by melt-mixing with polyvinylidene fluoride (PVDF). In the synthesis of N-CNTs, three catalysts of Co, Fe and Ni, and three temperatures of 650, 750 and 950 °C were employed. The morphology, aspect ratio, synthesis yield, remaining residue, nitrogen content, nitrogen bonding type, and powder conductivity of N-CNTs, and the morphology, polar crystalline phase, and broadband dielectric properties of N-CNT/PVDF nanocomposites were investigated. The results revealed that by proper selection of synthesis catalyst (Fe) and temperature (650 °C and 950 °C), nitrogen doping generated polarizable nanotubes via providing local polarization sites, and resulted in nanocomposites with favorable dielectric properties for charge storage applications at N-CNT loadings as low as 1.0 wt%. As a result, 3.5 wt% (N-CNT)Fe/950°C/PVDF nanocomposites exhibited an insulative behavior with ϵ' = 23.12 and tan δ = 0.05 at 1 kHz, a combination superior to that of PVDF, i.e., ϵ' = 8.4 and tan δ = 0.03 and to those of percolative nanocomposites, e.g., ϵ' = 71.20 and tan δ = 63.20 for 3.5 wt% (N-CNT)Fe/750°C/PVDF. Also, the relationships between the dielectric properties, N-CNT structure, and nanocomposite morphology were identified.
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    Effect of synthesis catalyst on structure of nitrogen-doped carbon nanotubes and electrical conductivity and electromagnetic interference shielding of their polymeric nanocomposites
    (New York, NY [u.a.] : Pergamon Press, 2016) Arjmand, Mohammad; Chizari, Kambiz; Krause, Beate; Pötschke, Petra; Sundararaj, Uttandaraman
    Different catalysts including Co, Fe, and Ni were used to synthesize nitrogen-doped carbon nanotubes (N-CNTs) by chemical vapor deposition technique. Synthesized N-CNTs were melt mixed with a polyvinylidene fluoride (PVDF) matrix using a small scale mixer at different concentrations ranging from 0.3 to 3.5 wt%, and then compression molded. The characterization techniques revealed significant differences in the synthesis yield and the morphological and electrical properties of both N-CNTs and nanocomposites depending on the catalyst type. Whereas Co and Fe resulted in yields comparable to industrial multiwalled CNTs, Ni was much less effective. The N-CNT aspect ratio was the highest for Co catalyst, followed by Ni and Fe, whereas nitrogen content was the highest for Ni. Raman spectroscopy revealed lowest defect number and highest N-CNT crystallinity for Fe catalyst. Characterization of N-CNT/PVDF nanocomposites showed better dispersion for N-CNTs based on Co and Fe as compared to Ni, and the following order of electrical conductivity and electromagnetic interference shielding (from high to low): Co > Fe > Ni. The superior electrical properties of (N-CNT)Co nanocomposites were ascribed to a combination of high synthesis yield, high aspect ratio, low nitrogen content and high crystallinity of N-CNTs combined with a good state of N-CNT dispersion.
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    A method for determination of length distributions of multiwalled carbon nanotubes before and after melt processing
    (New York, NY [u.a.] : Pergamon Press, 2011) Krause, Beate; Boldt, Regine; Pötschke, Petra
    A relatively simple method to determine the length distribution of carbon nanotubes (CNTs) before and after melt processing was developed. This involves the selection of a suitable solvent for dispersing pristine CNTs as well as to dissolve the matrix of melt mixed composites and the choice of an appropriate nanotube concentration. The length of suitably individualized CNTs was visualized using transmission electron microscopy and length distributions were measured using image analysis. Examples are shown for Baytubes® C150HP and Nanocyl™ NC7000 and their melt mixed composites with polycarbonate where the same procedure was applied to both, measuring the initial length distribution and the distribution after recovering from the composites. These results indicated a significant shortening after melt processing up to 30% of the initial length. © 2010 Elsevier Ltd. All rights reserved.
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    Characterization of the state of dispersion of carbon nanotubes in polymer nanocomposites
    (Weinheim : Wiley-VCH Verl., 2011) Buschhorn, Samuel T.; Wichmann, Malte H. G.; Sumfleth, Jan; Schulte, Karl; Pegel, Sven; Kasaliwal, Gaurav R.; Villmow, Tobias; Krause, Beate; Göldel, Andreas; Pötschke, Petra
    A practical overview of possibilities and limits to characterize the state of dispersion of carbon nanotubes (CNT) in polymer based nanocomposites is given. The most important and widely available methods are discussed with practical employment in mind. One focus is the quantitative characterization of the state of dispersion in solid samples using microscopy techniques such as optical microscopy or transmission electron microscopy. For dispersions of CNTs in aqueous media, solvents or monomers a sedimentation analysis is presented. This way dispersability and dispersion state of CNTs can be assessed. Indirect methods such as electrical conductivity measurements and rheological tests, dynamic differential scanning calorimetry and mechanical test are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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    A promising approach to low electrical percolation threshold in PMMA nanocomposites by using MWCNT-PEO predispersions
    (Oxford : Elsevier Science, 2016) Mir, Seyed Mohammad; Jafari, Seyed Hassan; Khonakdar, Hossein Ali; Krause, Beate; Pötschke, Petra; Taheri Qazvini, Nader
    Electrical conductive poly(methyl methacrylate) (PMMA) nanocomposites with low percolation threshold are very challenging to be prepared. Here, we show that the miscibility between poly(ethylene oxide) (PEO) as matrix for predispersions of multi-walled carbon nanotubes (MWCNTs) and PMMA represents an efficient approach to achieve very low electrical percolation threshold. PMMA/PEO-MWCNTs nanocomposites were prepared by a two-step solution casting method involving pre-mixing of MWCNTs with PEO and then mixing of PEO-MWCNTs with PMMA, resulting in a PMMA/PEO ratio of 80/20 wt%. The electrical percolation threshold (EPT) value was determined to be ~ 0.07 wt% which is significantly lower than most of the reported EPT values in the literature for PMMA/CNT composites. The very low electrical percolation threshold was attributed to the effectual role of PEO in self-assembly of secondary structures of nanotubes into an electrically conductive network. This was further confirmed by transmission electron microscopy and by comparing the obtained EPT value with the prediction of the excluded volume model in which statistical percolation threshold is defined based on uniform distribution of high-aspect ratio sticks in a matrix. Moreover, based on UV–Vis measurements and linear viscoelastic rheological measurements, optical and rheological percolation thresholds were obtained at nearly 0.01 wt% and 0.5 wt%, respectively.
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    Achieving electrical conductive tracks by laser treatment of non-conductive polypropylene/polycarbonate blends filled with MWCNTs
    (Weinheim : Wiley-VCH, 2014) Liebscher, Marco; Krause, Beate; Pötschke, Petra; Barz, Andrea; Bliedtner, Jens; Möhwald, Michael; Letzsch, Alexander
    Electrical non-conductive polymer blends consisting of a polypropylene (PP) matrix and dispersed particles of polycarbonate (PC) were melt compounded with 3 wt.% multiwalled carbon nanotubes (MWCNTs) loading and processed into plates by injection molding. The morphological analysis confirmed the selective localization of the MWCNTs in the PC component. By local irradiation with a CO2 laser beam, depending on the laser conditions, conductive tracks with dimensions of about 2 mm width, 80 to 370 μm depth and line resistances as low as 1.5 kΩ · cm-1 were created on the surface of the non-conductive plates. The factors affecting the line resistance are the PC content, the laser speed and laser power, as well as laser direction with respect to the melt flow direction. After the irradiation an enrichment of MWCNTs in the laser lines was detected indicating that conductive paths were generated by percolation of nanotubes selectively within these lines in otherwise non-conductive plates. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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    Aspect ratio effects of multi-walled carbon nanotubes on electrical, mechanical, and thermal properties of polycarbonate/MWCNT composites
    (Hoboken, NJ [u.a.] : Wiley, 2014) Guo, Jiaxi; Liu, Yanjun; Prada-Silvy, Ricardo; Tan, Yongqiang; Azad, Samina; Krause, Beate; Pötschke, Petra; Grady, Brian P.
    Two multi-walled carbon nanotubes (MWCNTs) having relatively high aspect ratios of 313 and 474 with approximately the same diameter were melt mixed with polycarbonate (PC) in a twin-screw conical micro compounder. The effects of aspect ratio on the electrical, mechanical, and thermal properties of the PC/MWCNT composites were investigated. Electrical conductivities and storage moduli of the filled samples are found to be independent of the starting aspect ratio for these high aspect ratio tubes; although the conductivities and storage moduli are still significantly higher than values of composites made with nanotubes having more commercially common aspect ratios of ∼100. Transmission electron microscopy results suggest that melt-mixing reduces these longer nanotubes to the same length, but still approximately two times longer than the length of commercially common aspect ratio tubes after melt-mixing. Molecular weight measurements show that during melt-mixing the longer nanotubes significantly degrade the molecular weight of the polymer as compared to very similar nanotubes with aspect ratio ∼100. Because of the molecular weight reduction glass transition temperatures predictably show a large decrease with increasing nanotube concentration. © 2013 Wiley Periodicals, Inc.
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    Electrical 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, Petra
    Electrical 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
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    Influence of talc with different particle sizes in melt-mixed LLDPE/MWCNT composites
    (Hoboken, NJ [u.a.] : Wiley, 2013) Müller, Michael Thomas; Dreyße, Janine; Häußler, Liane; Krause, Beate; Pötschke, Petra
    Linear low-density polyethylene (LLDPE) was melt-mixed with multiwalled carbon nanotubes (MWCNTs) and varying amounts of three different kinds of talc (phyllo silicate), each with a different particle size distribution, to examine the effect of these filler combinations with regards to the electrical percolation behavior. The state of the filler dispersion was assessed using transmission light microscopy and electron microscopy. The use of talc as a second filler during the melt mixing of LLDPE/MWCNT composites resulted in an improvement in the dispersion of the MWCNTs and a decrease of the electrical percolation threshold. Talc with lower particle sizes showed a more pronounced effect than talc with larger particle sizes. However, the improvement in dispersion was not reflected in the mechanical properties. Modulus and stress values increase with both, MWCNT and talc addition, but not in a synergistic manner. The crystallization behavior of the composites was studied by differential scanning calorimetry to determine its potential influence on the electrical percolation threshold. It was found that the crystallinity of the matrix increased slightly with the addition of talc but no further increments were observed with the incorporation of the MWCNTs. © 2013 Wiley Periodicals, Inc.