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    Optical, electrical and chemical properties of PEO:I2 complex composite films
    (Heidelberg [u.a.] : Springer, 2022) Telfah, Ahmad; Al-Bataineh, Qais M.; Tolstik, Elen; Ahmad, Ahmad A.; Alsaad, Ahmad M.; Ababneh, Riad; Tavares, Carlos J.; Hergenröder, Roland
    Synthesized PEO:I2 complex composite films with different I2 concentrations were deposited onto fused silica substrates using a dip-coating method. Incorporation of PEO films with I2 increases the electrical conductivity of the composite, reaching a maximum of 46 mS/cm for 7 wt% I2. The optical and optoelectronic properties of the complex composite films were studied using the transmittance and reflectance spectra in the UV-Vis region. The transmittance of PEO decreases with increasing I2 content. From this study, the optical bandgap energy decreases from 4.42 to 3.28 eV as I2 content increases from 0 to 7 wt%. In addition, the refractive index for PEO films are in the range of 1.66 and 2.00.1H NMR spectra of pure PEO film shows two major peaks at 3.224 ppm and 1.038 ppm, with different widths assigned to the mobile polymer chains in the amorphous phase, whereas the broad component is assigned to the more rigid molecules in the crystalline phase, respectively. By adding I2 to the PEO, both peaks (amorphous and crystal) are shifted to lower NMR frequencies indicating that I2 is acting as a Lewis acid, and PEO is acting as Lewis base. Hence, molecular iodine reacts favorably with PEO molecules through a charge transfer mechanism, and the formation of triiodide (I3-), the iodite (IO2-) anion, I 2· · · PEO and I2+···PEO complexes. PEO:I2 complex composite films are expected to be suitable for optical, electrical, and optoelectronic applications.
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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.
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    Synthesis and characterization of poly(1,2,3-triazole)s with inherent high sulfur content for optical applications
    (Hoboken, NJ : Wiley, 2023) Mazumder, Kajari; Komber, Hartmut; Bittrich, Eva; Voit, Brigitte; Banerjee, Susanta
    The synthesis of solution-processable sulfur-containing polytriazoles for optoelectronic applications is a relatively less explored domain in polymer research. The synthesis of novel bifunctional (DA) and trifunctional (TA) azido-monomers with inherent high sulfur content and of organo-soluble high refractive index poly(1,2,3-triazole)s using the azido-monomers via Cu(I) assisted click polymerization reactions are reported in this work. The azido-monomers were synthesized by the conversion of previously reported amine-functionalized compounds to azides using azidotrimethylsilane in a polar aprotic solvent. Dialkyne monomers were also synthesized and reacted with the azides to prepare a series of five linear and two hyperbranched poly(1,2,3-triazole)s. Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, differential scanning calorimetry and thermogravimetric analysis were used to characterize the synthesized polymers. It was also demonstrated that the use of the trifunctional azide in optimized conditions resulted in increased solubility of an otherwise insoluble linear poly(1,2,3-triazole). The optical characterization of the polymers was carried out on thin polymer films with thickness in the nanometer range, which were successfully prepared by spin-coating on silicon wafers. It was found that the increase in the sulfur and aromatic content in the polymer backbone successfully increased the refractive index of the polymers up to 1.743 at 589 nm.
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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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    Revealing all states of dewetting of a thin gold layer on a silicon surface by nanosecond laser conditioning
    (Amsterdam : Elsevier, 2021) Ernst, Owen C.; Uebel, David; Kayser, Stefan; Lange, Felix; Teubner, Thomas; Boeck, Torsten
    Dewetting is a ubiquitous phenomenon which can be applied to the laser synthesis of nanoparticles. A classical spinodal dewetting process takes place in four successive states, which differ from each other in their morphology. In this study all states are revealed by interaction of pulsed nanosecond UV laser light with thin gold layers with thicknesses between 1 nm and 10 nm on (100) silicon wafers. The specific morphologies of the dewetting states are discussed with particular emphasis on the state boundaries. The main parameter determining which state is formed is not the duration for which the gold remains liquid, but rather the input energy provided by the laser. This shows that each state transition has a separate measurable activation energy. The temperature during the nanosecond pulses and the duration during which the gold remains liquid was determined by simulation using the COMSOL Multiphysics® software package. Using these calculations, an accurate local temperature profile and its development over time was simulated. An analytical study of the morphologies and formed structures was performed using Minkowski measures. With aid of this tool, the laser induced structures were compared with thermally annealed samples, with perfectly ordered structures and with perfectly random structures. The results show that both, structures of the laser induced and the annealed samples, strongly resemble the perfectly ordered structures. This reveals a close relationship between these structures and suggests that the phenomenon under investigation is indeed a spinodal dewetting generated by an internal material wave function. The purposeful generation of these structures and the elucidation of the underlying mechanism of dewetting by short pulse lasers may assist the realisation of various technical elements such as nanowires in science and industry. © 2020
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    Stable 15N isotopes in fine and coarse urban particulate matter
    (Philadelphia, Pa : Taylor & Francis, 2021) Wiedenhaus, Hanna; Ehrnsperger, Laura; Klemm, Otto; Strauss, Harald
    Particulate nitrogen has far-reaching negative effects on human health and the environment, and effective strategies for reducing it require understanding its sources and formation processes. To learn about these factors, we recorded size-resolved nitrogen isotope ratios (δ15N) of total particulate N at an urban site in northwest Germany during a four-week measuring campaign. We observed a steady decrease in δ15N when going from fine to coarse particles, with values between +18 ‰ and −2 ‰. This difference based on particle size is caused by different isotope fractionation processes during particle formation: The fine particles contain ammonium nitrate, which is formed in an equilibrium process, leading to an enrichment of 15N. Moreover, fine particles are more reactive due to their larger surface areas and relatively long residence times in the atmosphere, which leads to an additional enrichment of 15N; a key step of this process likely occurs when the ammonium particles interact with ammonia from agricultural sources. In contrast to fine particles, coarse particles are formed by direct absorption of HNO3 on preexisting particles; the HNO3 stems from traffic emissions of NOx and subsequent oxidation in the atmospheric gas phase. Because only a small amount of isotope fractionation is associated with non-equilibrium processes during phase transitions, there is less 15N enrichment in the coarse particles. Overall, nitrogen isotopes clearly reflect the different formation processes of fine and coarse aerosol particles. © 2021 The Author(s). Published with license by Taylor & Francis Group, LLC.
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    Mobility particle size spectrometers: Calibration procedures and measurement uncertainties
    (Philadelphia, Pa : Taylor & Francis, 2017) Wiedensohler, A.; Wiesner, A.; Weinhold, K.; Birmili, W.; Hermann, M.; Merkel, M.; Müller, T.; Pfeifer, S.; Schmidt, A.; Tuch, T.; Velarde, F.; Quincey, P.; Seeger, S.; Nowak, A.
    Mobility particle size spectrometers (MPSS) belong to the essential instruments in aerosol science that determine the particle number size distribution (PNSD) in the submicrometer size range. Following calibration procedures and target uncertainties against standards and reference instruments are suggested for a complete MPSS quality assurance program: (a) calibration of the CPC counting efficiency curve (within 5% for the plateau counting efficiency; within 1 nm for the 50% detection efficiency diameter), (b) sizing calibration of the MPSS, using a certified polystyrene latex (PSL) particle size standard at 203 nm (within 3%), (c) intercomparison of the PNSD of the MPSS (within 10% and 20% of the dN/dlogDP concentration for the particle size range 20–200 and 200–800 nm, respectively), and (d) intercomparison of the integral PNC of the MPSS (within 10%). Furthermore, following measurement uncertainties have been investigated: (a) PSL particle size standards in the range from 100 to 500 nm match within 1% after sizing calibration at 203 nm. (b) Bipolar diffusion chargers based on the radioactive nuclides Kr85, Am241, and Ni63 and a new ionizer based on corona discharge follow the recommended bipolar charge distribution, while soft X-ray-based charges may alter faster than expected. (c) The use of a positive high voltage supply show a 10% better performance than a negative one. (d) The intercomparison of the integral PNC of an MPSS against the total number concentration is still within the target uncertainty at an ambient pressure of approximately 500 hPa. Copyright © 2018 Published with license by American Association for Aerosol Research.
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    The second ACTRIS inter-comparison (2016) for Aerosol Chemical Speciation Monitors (ACSM): Calibration protocols and instrument performance evaluations
    (Philadelphia, Pa.: Taylor & Francis, 2019) Freney, Evelyn; Zhang, Yunjiang; Croteau, Philip; Amodeo, Tanguy; Williams, Leah; Truong, François; Petit, Jean-Eudes; Sciare, Jean; Sarda-Esteve, Roland; Bonnaire, Nicolas; Arumae, Tarvo; Aurela, Minna; Bougiatioti, Aikaterini; Mihalopoulos, Nikolaos; Coz, Esther; Artinano, Begoña; Crenn, Vincent; Elste, Thomas; Heikkinen, Liine; Poulain, Laurent; Wiedensohler, Alfred; Herrmann, Hartmut; Priestman, Max; Alastuey, Andres; Stavroulas, Iasonas; Tobler, Anna; Vasilescu, Jeni; Zanca, Nicola; Canagaratna, Manjula; Carbone, Claudio; Flentje, Harald; Green, David; Maasikmets, Marek; Marmureanu, Luminita; Cruz Minguillon, Maria; Prevot, Andre S.H.; Gros, Valerie; Jayne, John; Favez, Olivier
    This work describes results obtained from the 2016 Aerosol Chemical Speciation Monitor (ACSM) intercomparison exercise performed at the Aerosol Chemical Monitor Calibration Center (ACMCC, France). Fifteen quadrupole ACSMs (Q_ACSM) from the European Research Infrastructure for the observation of Aerosols, Clouds and Trace gases (ACTRIS) network were calibrated using a new procedure that acquires calibration data under the same operating conditions as those used during sampling and hence gets information representative of instrument performance. The new calibration procedure notably resulted in a decrease in the spread of the measured sulfate mass concentrations, improving the reproducibility of inorganic species measurements between ACSMs as well as the consistency with co-located independent instruments. Tested calibration procedures also allowed for the investigation of artifacts in individual instruments, such as the overestimation of m/z 44 from organic aerosol. This effect was quantified by the m/z (mass-to-charge) 44 to nitrate ratio measured during ammonium nitrate calibrations, with values ranging from 0.03 to 0.26, showing that it can be significant for some instruments. The fragmentation table correction previously proposed to account for this artifact was applied to the measurements acquired during this study. For some instruments (those with high artifacts), this fragmentation table adjustment led to an “overcorrection” of the f44 (m/z 44/Org) signal. This correction based on measurements made with pure NH4NO3, assumes that the magnitude of the artifact is independent of chemical composition. Using data acquired at different NH4NO3 mixing ratios (from solutions of NH4NO3 and (NH4)2SO4) we observe that the magnitude of the artifact varies as a function of composition. Here we applied an updated correction, dependent on the ambient NO3 mass fraction, which resulted in an improved agreement in organic signal among instruments. This work illustrates the benefits of integrating new calibration procedures and artifact corrections, but also highlights the benefits of these intercomparison exercises to continue to improve our knowledge of how these instruments operate, and assist us in interpreting atmospheric chemistry. © 2019, © 2019 Author(s). Published with license by Taylor & Francis Group, LLC.
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    Heat accumulation during femtosecond laser treatment at high repetition rate – A morphological, chemical and crystallographic characterization of self-organized structures on Ti6Al4V
    (Amsterdam : Elsevier, 2021) Schnell, Georg; Lund, Henrik; Bartling, Stephan; Polley, Christian; Riaz, Abdullah; Senz, Volkmar; Springer, Armin; Seitz, Hermann
    This study presents a detailed characterization of self-organized nano- and microstructures on Ti6Al4V evoked by different scanning strategies and fluences with a 300 fs laser operating at a laser wavelength of 1030 nm. The resulting surface morphology was visualized via field emission scanning electron microscopy (FEG-SEM) images of the surface and cross-sections. X-ray diffraction (XRD)-analysis was performed to analyse changes in crystal structures. The chemical surface composition of the near-surface layer was determined by X-ray photoelectron spectroscopy (XPS). Results show a significant influence of heat accumulation while processing with high laser repetition rates on the formation, crystallinity and chemical composition of self-organized structures depending on the scanning strategy. The ablation with different laser scanning strategies led to varying dynamics of growth-mechanisms of self-organized structures, formation of intermetallic phases (Ti3Al), sub-oxides and oxides (Ti6O, TiO) as well as ions (Ti3+, Ti4+) in surface layer reliant on applied fluence. Furthermore, investigations revealed a heat-affected zone up to several micrometers in non-ablated material. © 2021 The Authors