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    Crystal structure of (2S,4S,7S)-7,7-dichloro-4-(1-chloro-1-methylethyl)-1- (2,2,2-trichloroethyl)bicyclo[4.1.0]heptane, C12H16Cl 6
    (Berlin : de Gruyter, 2009) Boualy, B.; el Firdoussi, L.; Ali, M.A.; Karim, A.; Spannenberg, A.
    C12H16Cl6, orthorhombic, P2 12121 (no. 19), a = 6.0742(3) Å, b = 9.7189(6) Å, c = 26.700(1) Å, V = 1576.2 Å3, Z = 4, Rgt(F) = 0.019, wRref(F2) = 0.045, T= 200 K. © by Oldenbourg Wissenschaftsverlag.
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    Mechanisms of bonding effected by nanoparticles in zirconia coatings applied by spraying of suspensions
    (Saarbrücke : Leibniz-Institut für Neue Materialien, 2008) Adam, Jens; Aslan, Mesut; Drumm, Robert; Veith, Michael
    Zirconia coatings consisting of a mixture of coarse and fine grained zirconia powders prepared by spraying of suspensions and subsequent thermal treatment at limited temperatures (up to 500°C) are poor in adherence and in intrinsic mechanical strength. We have shown elsewhere that mechanical properties of these coatings can be improved clearly by adding a small amount of nanoscaled zirconia. Here, the structural and the chemical development of this coating material and of the nanoparticles is examined to gain information about the underlying bonding mechanisms. The applied temperature is relatively low in comparison to the usual onset temperature of accelerated sintering. Nevertheless, the results show that diffusion controlled material transport mechanisms play their role in bonding. The condensation of surface OH groups may participate in bonding, too. These first results confirm the potential of nanoparticles to act as inorganic binder. Additional research effort to clarify the underlying mechanisms in detail is of interest. For the practical side, it can be concluded that the resulting effect of mechanical consolidation of ceramic structures at relatively low temperatures enables new ceramic applications, for example a new type of ceramic coatings on metallic substrates.
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    Thermoelectric 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 Maria
    The 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.
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    Li+/H+ exchange of Li7La3Zr2O12 single and polycrystals investigated by quantitative LIBS depth profiling
    (Cambridge : Royal Society of Chemistry, 2022) Smetaczek, Stefan; Limbeck, Andreas; Zeller, Veronika; Ring, Joseph; Ganschow, Steffen; Rettenwander, Daniel; Fleig, Jürgen
    Li7La3Zr2O12 (LLZO) garnets are highly attractive to be used as solid electrolyte in solid-state Li batteries. However, LLZO suffers from chemical interaction with air and humidity, causing Li+/H+ exchange with detrimental implication on its performance, processing and scalability. To better understand the kinetics of the detrimental Li+/H+ exchange and its dependence on microstructural features, accelerated Li+/H+ exchange experiments were performed on single crystalline and polycrystalline LLZO, exposed for 80 minutes to 80 °C hot water. The resulting chemical changes were quantified by analytical methods, i.e. inductively coupled plasma optical emission spectroscopy (ICP-OES) and laser induced breakdown spectroscopy (LIBS). From the time dependence of the Li+ enrichment in the water, measured by ICP-OES, a bulk interdiffusion coefficient of Li+/H+ could be determined (7 × 10−17 m2 s−1 at 80 °C). Depth dependent concentrations were obtained from the LIBS data for both ions after establishing a calibration method enabling not only Li+ but also H+ quantification in the solid electrolyte. Short interdiffusion lengths in the 1 μm range are found for the single crystalline Ga:LLZO, in accordance with the measured bulk diffusion coefficient. In polycrystalline Ta:LLZO, however, very long diffusion tails in the 20 μm range and ion exchange fractions up to about 70% are observed. Those are attributed to fast ion interdiffusion along grain boundaries. The severe compositional changes also strongly affect the electrical properties measured by impedance spectroscopy. This study highlights that microstructural effects may be decisive for the Li+/H+ ion exchange kinetics of LLZO.
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    Different Radial Modification Profiles Observed on APPJ-Treated Polypropylene Surfaces according to the Distance between Plasma Outlet and Target
    (Basel : MDPI, 2022) do Nascimento, Fellype; Silva Leal, Bruno; Quade, Antje; Kostov, Konstantin Georgiev
    The plasma jet transfer technique relies on a conductive wire at floating potential, which, upon entering in contact with a primary discharge, is capable of igniting a small plasma plume at the distal end of a long flexible plastic tube. In this work, two different long tube configurations were employed for the surface modification of polypropylene (PP) samples using argon as the working gas. One of the jet configurations has a thin copper (Cu) wire, which was installed inside the long tube. In the other configuration, the floating electrode is a metallic mesh placed between two plastic tubes in a coaxial arrangement. In the first case, the tip of the Cu wire is in direct contact with the working gas at the plasma outlet, whereas, in the second, the inner plastic tube provides an additional dielectric barrier that prevents the conductor from being in contact with the gas. Water contact angle (WCA) measurements on treated PP samples revealed that different surface modification radial profiles are formed when the distance (d) between the plasma outlet and target is changed. Moreover, it was found that the highest WCA reduction does not always occur at the point where the plasma impinges the surface of the material, especially when the d value is small. Through X-ray photoelectron spectroscopy (XPS) analysis, it was confirmed that the WCA values are directly linked to the oxygen-functional groups formed on the PP surfaces after the plasma treatment. An analysis of the WCA measurements along the surface, as well as their temporal evolution, together with the XPS data, suggest that, when the treatment is performed at small d values, the plasma jet removes some functional groups at the point where the plasma hits the surface, thus leading to peculiar WCA profiles.
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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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    Polymers Best Paper Award 2014
    (Basel : MDPI, 2014) Böker, Alexander
    [No abstract available]
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    Fusion of MALDI Spectrometric Imaging and Raman Spectroscopic Data for the Analysis of Biological Samples
    (Lausanne : Frontiers Media, 2018) Ryabchykov, Oleg; Popp, Jürgen; Bocklitz, Thomas W.
    Despite of a large number of imaging techniques for the characterization of biological samples, no universal one has been reported yet. In this work, a data fusion approach was investigated for combining Raman spectroscopic data with matrix-assisted laser desorption/ionization (MALDI) mass spectrometric data. It betters the image analysis of biological samples because Raman and MALDI information can be complementary to each other. While MALDI spectrometry yields detailed information regarding the lipid content, Raman spectroscopy provides valuable information about the overall chemical composition of the sample. The combination of Raman spectroscopic and MALDI spectrometric imaging data helps distinguishing different regions within the sample with a higher precision than would be possible by using either technique. We demonstrate that a data weighting step within the data fusion is necessary to reveal additional spectral features. The selected weighting approach was evaluated by examining the proportions of variance within the data explained by the first principal components of a principal component analysis (PCA) and visualizing the PCA results for each data type and combined data. In summary, the presented data fusion approach provides a concrete guideline on how to combine Raman spectroscopic and MALDI spectrometric imaging data for biological analysis.
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    TiO2 as Photosensitizer and Photoinitiator for Synthesis of Photoactive TiO2-PEGDA Hydrogel Without Organic Photoinitiator
    (Lausanne : Frontiers Media, 2018-8-7) Glass, Sarah; Trinklein, Betsy; Abel, Bernd; Schulze, Agnes
    The replacement of potentially toxic photoinitiators is of increasing interest regarding the synthesis of biomaterials by photopolymerization. Therefore, we present a new method for the preparation of UV polymerized hydrogels with TiO2 as a photoinitiator. Titania is known to be an excellent photoactive compound which is non-toxic, inert, and cheap. The so-formed hydrogels possess excellent mechanical properties, a high swelling ratio, and high thermal stability. Furthermore, no TiO2 is released from the hydrogels. Thus, the material is highly suitable for medical applications. Additionally, the present TiO2 in the hydrogels remains photoactive as demonstrated by degradation of methylene blue. This enables the application of TiO2-hydrogels in photodynamic therapy.
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    Inactivation of airborne bacteria by plasma treatment and ionic wind for indoor air cleaning
    (Hoboken, NJ : Wiley Interscience, 2020) Prehn, Franziska; Timmermann, Eric; Kettlitz, Manfred; Schaufler, Katharina; Günther, Sebastian; Hahn, Veronika
    Airborne bacteria are a general problem in medical or health care facilities with a high risk for nosocomial infections. Rooms with a continuous airflow, such as operation theaters, are of particular importance due to a possible dissemination and circulation of pathogens including multidrug-resistant microorganisms. In this regard, a cold atmospheric-pressure plasma (CAP) may be a possibility to support usual disinfection procedures due to its decontaminating properties. The aim of this study was to determine the antimicrobial efficacy of a plasma decontamination module that included a dielectric barrier discharge for plasma generation. Experimental parameters such as an airflow velocity of 4.5 m/s and microbial contaminations of approximately 6,000 colony-forming units (cfu)/m3 were used to simulate practical conditions of a ventilation system in an operating theater. The apathogenic microorganism Escherichia coli K12 DSM 11250/NCTC 10538 and the multidrug-resistant strains E. coli 21181 and 21182 (isolated from patients) were tested to determine the antimicrobial efficacy. In summary, the number of cfu was reduced by 31–89% for the tested E. coli strains, whereby E. coli K12 was the most susceptible strain toward inactivation by the designed plasma module. A possible correlation between the number or kind of resistances and susceptibility against plasma was discussed. The inactivation of microorganisms was affected by plasma intensity and size of the plasma treatment area. In addition, the differences of the antimicrobial efficacies caused through the nebulization of microorganisms in front (upstream) or behind (downstream) the plasma source were compared. The presence of ionic wind had no influence on the reduction of the number of cfu for E. coli K12, as the airflow velocity was too high for a successful precipitation, which would be a prerequisite for an increased antimicrobial efficacy. The inactivation of the tested microorganisms confirms the potential of CAP for the improvement of air quality. The scale-up of this model system may provide a novel tool for an effective air cleaning process.