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    High-Performance, Lightweight, and Flexible Thermoplastic Polyurethane Nanocomposites with Zn2+-Substituted CoFe2O4 Nanoparticles and Reduced Graphene Oxide as Shielding Materials against Electromagnetic Pollution
    (Washington, DC : ACS Publications, 2021-10-11) Anju; Yadav, Raghvendra Singh; Pötschke, Petra; Pionteck, Jürgen; Krause, Beate; Kuřitka, Ivo; Vilcakova, Jarmila; Skoda, David; Urbánek, Pavel; Machovsky, Michal; Masař, Milan; Urbánek, Michal; Jurca, Marek; Kalina, Lukas; Havlica, Jaromir
    The development of flexible, lightweight, and thin high-performance electromagnetic interference shielding materials is urgently needed for the protection of humans, the environment, and electronic devices against electromagnetic radiation. To achieve this, the spinel ferrite nanoparticles CoFe2O4 (CZ1), Co0.67Zn0.33Fe2O4 (CZ2), and Co0.33Zn0.67Fe2O4 (CZ3) were prepared by the sonochemical synthesis method. Further, these prepared spinel ferrite nanoparticles and reduced graphene oxide (rGO) were embedded in a thermoplastic polyurethane (TPU) matrix. The maximum electromagnetic interference (EMI) total shielding effectiveness (SET) values in the frequency range 8.2-12.4 GHz of these nanocomposites with a thickness of only 0.8 mm were 48.3, 61.8, and 67.8 dB for CZ1-rGO-TPU, CZ2-rGO-TPU, and CZ3-rGO-TPU, respectively. The high-performance electromagnetic interference shielding characteristics of the CZ3-rGO-TPU nanocomposite stem from dipole and interfacial polarization, conduction loss, multiple scattering, eddy current effect, natural resonance, high attenuation constant, and impedance matching. The optimized CZ3-rGO-TPU nanocomposite can be a potential candidate as a lightweight, flexible, thin, and high-performance electromagnetic interference shielding material.
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    The Localization Behavior of Different CNTs in PC/SAN Blends Containing a Reactive Component
    (Basel : MDPI, 2021-3-1) Gültner, Marén; Boldt, Regine; Formanek, Petr; Fischer, Dieter; Simon, Frank; Pötschke, Petra
    Co-continuous blend systems of polycarbonate (PC), poly(styrene-co-acrylonitrile) (SAN), commercial non-functionalized multi-walled carbon nanotubes (MWCNTs) or various types of commercial and laboratory functionalized single-walled carbon nanotubes (SWCNTs), and a reactive component (RC, N-phenylmaleimide styrene maleic anhydride copolymer) were melt compounded in one step in a microcompounder. The blend system is immiscible, while the RC is miscible with SAN and contains maleic anhydride groups that have the potential to reactively couple with functional groups on the surface of the nanotubes. The influence of the RC on the localization of MWCNTs and SWCNTs (0.5 wt.%) was investigated by transmission electron microscopy (TEM) and energy-filtered TEM. In PC/SAN blends without RC, MWCNTs are localized in the PC component. In contrast, in PC/SAN-RC, the MWCNTs localize in the SAN-RC component, depending on the RC concentration. By adjusting the MWCNT/RC ratio, the localization of the MWCNTs can be tuned. The SWCNTs behave differently compared to the MWCNTs in PC/SAN-RC blends and their localization occurs either only in the PC or in both blend components, depending on the type of the SWCNTs. CNT defect concentration and surface functionalities seem to be responsible for the localization differences.
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    Bio-inspired deposition of electrochemically exfoliated graphene layers for electrical resistance heating applications
    (Bristol : IOP Publishing, 2020-12-4) Utech, Toni; Pötschke, Petra; Simon, Frank; Janke, Andreas; Kettner, Hannes; Paiva, Maria; Zimmerer, Cordelia
    Electrochemically exfoliated graphene (eeG) layers possess a variety of potential applications, e.g. as susceptor material for contactless induction heating in dynamic electro-magnetic fields, and as flexible and transparent electrode or resistivity heating elements. Spray coating of eeG dispersions was investigated in detail as a simple and fast method to deposit both, thin conducting layers and ring structures on polycarbonate substrates. The spray coating process was examined by systematic variation of dispersion concentration and volume applied to heated substrates. Properties of the obtained layers were characterized by UV-VIS spectroscopy, SEM and Confocal Scanning Microscopy. Electrical conductivity of eeG ring structures was measured using micro-four-point measurements. Modification of eeG with poly(dopamine) and post-thermal treatment yields in the reduction of the oxidized graphene proportion, an increase in electrical conductivity, and mechanical stabilization of the deposited thin layers. The chemical composition of modified eeG layer was analyzed via x-ray photoelectron spectroscopy pointing to the reductive behavior of poly(dopamine). Application oriented experiments demonstrate the direct electric current heating (Joule-Heating) effect of spray-coated eeG layers.
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    Blend Structure and n-Type Thermoelectric Performance of PA6/SAN and PA6/PMMA Blends Filled with Singlewalled Carbon Nanotubes
    (Basel : MDPI, 2021-4-28) Krause, Beate; Liguoro, Alice; Pötschke, Petra
    The present study investigates how the formation of melt-mixed immiscible blends based on PA6/SAN and PA6/PMMA filled with single walled nanotubes (SWCNTs) affects the thermoelectric (TE) properties. In addition to the detailed investigation of the blend morphology with compositions between 100/0 wt.% and 50/50 wt.%, the thermoelectric properties are investigated on blends with different SWCNT concentrations (0.25–3.0 wt.%). Both PA6 and the blend composites with the used type of SWCNTs showed negative Seebeck coefficients. It was shown that the PA6 matrix polymer, in which the SWCNTs are localized, mainly influenced the thermoelectric properties of blends with high SWCNT contents. By varying the blend composition, an increase in the absolute Seebeck coefficient, power factor (PF), and figure of merit (ZT) was achieved compared to the PA6 composite which is mainly related to the selective localization and enrichment of SWCNTs in the PA6 matrix at constant SWCNT loading. The maximum PFs achieved were 0.22 µW/m·K2 for PA6/SAN/SWCNT 70/30/3 wt.% and 0.13 µW/m·K2 for PA6/PMMA/SWCNT 60/40/3 wt.% compared to 0.09 µW/m·K2 for PA6/3 wt.% SWCNT which represent increases to 244% and 144%, respectively. At higher PMMA or SAN concentration, the change from matrix-droplet to a co-continuous morphology started, which, despite higher SWCNT enrichment in the PA6 matrix, disturbed the electrical conductivity, resulting in reduced PFs with still increasing Seebeck coefficients. At SWCNT contents between 0.5 and 3 wt.% the increase in the absolute Seebeck coefficient was compensated by lower electrical conductivity resulting in lower PF and ZT as compared to the PA6 composites.
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    Surface modification of MWCNT and its influence on properties of paraffin/MWCNT nanocomposites as phase change material
    (Hoboken, NJ [u.a.] : Wiley InterScience, 2020) Avid, Arezoo; Jafari, Seyed Hassan; Khonakdar, Hossein Ali; Ghaffari, Mehdi; Krause, Beate; Pötschke, Petra
    Multiwalled carbon nanotubes (MWCNTs) were modified by an organo-silane in order to improve their dispersion state and stability in paraffin wax. A family of paraffin-based phase change material (PCM) composites filled with MWCNTs was prepared with different loadings (0, 0.1, 0.5, and 1 wt%) of pristine MWCNTs and organo-silane modified MWCNTs (Si-MWCNT). Structural analyses were performed by means of Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and rheological studies using temperature sweeps. Moreover, phase change transition temperatures and heat of fusion as well as thermal and electrical conductivities of the developed PCM nanocomposites were determined. The SEM micrographs and FTIR absorption bands appearing at approximately 1038 and 1112 cm−1 confirmed the silane modification. Differential scanning calorimetery (DSC) results indicate that the presence of Si-MWCNTs leads to slightly favorable enhancement in the energy storage capacity at the maximum loading. It was also shown that the thermal conductivity of the PCM nanocomposites, in both solid and liquid phases, increased with increasing the MWCNT content independent of the kind of MWCNTs by up to about 30% at the maximum loading of MWCNTs. In addition, the modification of MWCNTs made the samples completely electrically nonconductive, and the electrical surface resistivity of the PCMs containing pristine MWCNTs decreased with increasing MWCNTs loading. Furthermore, the rheological assessment under consecutive cyclic phase change demonstrated that the samples containing modified MWCNTs are more stable compared to the PCM containing pristine MWCNTs. © 2019 Wiley
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    CuxCo1-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, Michal
    CuxCo1-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.
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    Nonlinear Thermopower Behaviour of N-Type Carbon Nanofibres and Their Melt Mixed Polypropylene Composites
    (Basel : MDPI, 2022-1-10) Paleo, Antonio J.; Krause, Beate; Cerqueira, Maria F.; Muñoz, Enrique; Pötschke, Petra; Rocha, Ana M.
    The temperature dependent electrical conductivity σ (T) and thermopower (Seebeck coeffi-cient) S (T) from 303.15 K (30◦ C) to 373.15 K (100◦ C) of an as-received commercial n-type vapour grown carbon nanofibre (CNF) powder and its melt-mixed polypropylene (PP) composite with 5 wt.% of CNFs have been analysed. At 30◦ C, the σ and S of the CNF powder are ~136 S m−1 and −5.1 µV K−1, respectively, whereas its PP/CNF composite showed lower conductivities and less negative S-values of ~15 S m−1 and −3.4 µV K−1, respectively. The σ (T) of both samples presents a dσ/dT < 0 character described by the 3D variable range hopping (VRH) model. In contrast, their S (T) shows a dS/dT > 0 character, also observed in some doped multiwall carbon nanotube (MWCNT) mats with nonlinear thermopower behaviour, and explained here from the contribution of impurities in the CNF structure such as oxygen and sulphur, which cause sharply varying and localized states at approximately 0.09 eV above their Fermi energy level (EF).
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    Aerogels based on reduced graphene oxide/cellulose composites: Preparation and vapour sensing abilities
    (Basel : MDPI, 2020) Chen, Yian; Pötschke, Petra; Pionteck, Jürgen; Voit, Brigitte; Qi, Haisong
    This paper reports on the preparation of cellulose/reduced graphene oxide (rGO) aerogels for use as chemical vapour sensors. Cellulose/rGO composite aerogels were prepared by dissolving cellulose and dispersing graphene oxide (GO) in aqueous NaOH/urea solution, followed by an in-situ reduction of GO to reduced GO (rGO) and lyophilisation. The vapour sensing properties of cellulose/rGO composite aerogels were investigated by measuring the change in electrical resistance during cyclic exposure to vapours with varying solubility parameters, namely water, methanol, ethanol, acetone, toluene, tetrahydrofuran (THF), and chloroform. The increase in resistance of aerogels on exposure to vapours is in the range of 7 to 40% with methanol giving the highest response. The sensing signal increases almost linearly with the vapour concentration, as tested for methanol. The resistance changes are caused by the destruction of the conductive filler network due to a combination of swelling of the cellulose matrix and adsorption of vapour molecules on the filler surfaces. This combined mechanism leads to an increased sensing response with increasing conductive filler content. Overall, fast reaction, good reproducibility, high sensitivity, and good differentiation ability between different vapours characterize the detection behaviour of the aerogels. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.
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    Nanocomposites with p-and n-type conductivity controlled by type and content of nanotubes in thermosets for thermoelectric applications
    (Basel : MDPI, 2020) Kröning, Katharina; Krause, Beate; Pötschke, Petra; Fiedler, Bodo
    In this work, composites based on epoxy resin and various carbon nanotubes (CNTs) were studied regarding their thermoelectric properties. The epoxy composites were prepared by infiltration of preformed CNT buckypapers. The influence of different types of CNTs on the Seebeck coefficient was investigated, namely lab-made and commercially available multi walled carbon nanotubes (MWCNTs), lab-made nitrogen doped MWCNTs (N-MWCNT) and commercially available single walled carbon nanotubes (SWCNTs). It was found that only by varying the lab-made MWCNT content could both n-and p-type composites be produced with Seebeck coefficients between -9.5 and 3.1 µV/K. The incorporation of N-MWCNTs resulted in negative Seebeck coefficients of -11.4 to -17.4 µV/K. Thus, the Seebeck coefficient of pure SWCNT changed from 37.4 to -25.5 µV/K in the epoxy/1 wt. % SWCNT composite. A possible explanation for the shift in the Seebeck coefficient is the change of the CNTs Fermi level depending on the number of epoxy molecules on the CNT surface. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.
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    Ultrathin structures derived from interfacially modified polymeric nanocomposites to curb electromagnetic pollution
    (Cambridge : Royal Society of Chemistry, 2021) Sushmita, Kumari; Formanek, Petr; Fischer, Dieter; Pötschke, Petra; Madras, Giridhar; Bose, Suryasarathi
    The use of electronic devices and wireless networks is increasing rapidly, and electromagnetic (EM) pollution remediation remains a challenge. We employed a unique approach to fabricate two ultrathin (approx. 53 μm) multilayered assemblies to address this. By sequentially stacking thin films of polyvinylidene difluoride (PVDF) and polycarbonate (PC) nanocomposites and interfacially locking them with a mutually miscible polymer (PMMA, polymethyl methacrylate), materials with enhanced structural properties and electromagnetic interference (EMI) shielding performance can be designed. Utilizing reduced graphene oxide (rGO) and molybdenum disulfide (MoS2) as a template, ferrite was grown on the surface to design two different nanohybrid structures (rGO–Fe3O4 and MoS2–Fe3O4). PVDF was composited with either rGO–Fe3O4 or MoS2–Fe3O4, and multiwall carbon nanotubes (CNTs) were dispersed in the PC component. As PC and PVDF are immiscible, their poor interface would result in inferior structural properties, which can be challenging in designing EMI shielding materials due to cyclic thermal fatigue. Hence, PMMA is sandwiched to interfacially stitch the components (PC and PVDF) and improve interfacial adhesion. This was confirmed using SEM/EDS and Raman mapping/imaging. The mechanical stability of the multilayered assemblies was characterized using a dynamic mechanical analyzer (DMA), and the storage modulus was found to be as high as 2767 MPa at 40 °C (@constant frequency and strain amplitude), for the multilayered film with rGO–Fe3O4 in PVDF, PMMA as a sandwich layer and CNTs in PC. A typical assembly of 9 multilayers (∼480 μm) with rGO–Fe3O4 in PVDF, and CNTs in PC, and interfacially stitched with PMMA gave rise to a high EMI shield effectiveness (SET) of −26.3 dB @ 26.5 GHz. This unique arrangement of a multilayered assembly suppressed EMI primarily by absorption.