Browsing by Subject "Surface analysis"

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    The formation and characterization of cyclodextrin functionalized polystyrene nanofibers produced by electrospinning
    (2009) Uyar, Tamer; Havelund, R.; Hacaloglu J.; Zhou X.; Besenbacher F.; Kingshott P.
    Polystyrene (PS) nanofibers containing the inclusion complex forming beta-cyclodextrin (β-CD) were successfully produced by electrospinning aimed at developing functional fibrous nanowebs. By optimization of the electrospinning parameters, which included varying the relative concentration of PS and β-CD in the solutions, bead-free fibers were produced. Homogeneous solutions of β-CD and PS in dimethylformamide (DMF) were used with concentrations of PS varying from 10% to 25% (w/v, with respect to DMF), and β-CD concentrations of 1% to 50% (w/w, with respect to PS). The presence of β-CD facilitated the production of bead-free PS fibers even from lower polymer concentrations as a result of the higher conductivity of the PS/CD solutions. The morphology and the production of bead-free PS/CD fibers were highly dependent on the β-CD contents. Transmission electron microscope (TEM) and atomic force microscope (AFM) images showed that incorporation of β-CD yielded PS fibers with rougher surfaces. Thermogravimetric analysis (TGA) and direct insertion probe pyrolysis mass spectroscopy (DP-MS) results confirmed the presence of β-CD in the PS fibers. X-ray diffraction (XRD) spectra of the fibers indicated that the β-CD molecules are distributed within the PS matrix without any phase separated crystalline aggregates up to 40% (w/w) β-CD loading. Furthermore, chemical analyses by Fourier transform infrared (FTIR) spectroscopy studies confirm that β-CD molecules are located within the PS fiber matrix. Finally, preliminary investigations using x-ray photoelectron spectroscopy (XPS) and time-of-flight static secondary ion mass spectrometry (ToF-static-SIMS) show the presence of the cyclodextrin molecules in the outer molecular layers of the fiber surfaces. The XPS and ToF-SIMS findings indicate that cyclodextrin functionalized PS webs would have the potential to be used as molecular filters and/or nanofilters for the purposes of filtration/purification/separation owing to surface associated β-CD molecules which have inclusion complexation capability. © 2009 IOP Publishing Ltd.
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    ItemOpen Access
    Nature of the Ti-Ba interactions on the BaO/TiO2/Al 2O3 NOx storage system
    (2009) Andonova, S. M.; Şentürk, G. S.; Kayhan, E.; Ozensoy, E.
    A ternary oxide-based NO* storage material in the form of BaOZTiO2Zy-Al2O3 was synthesized and characterized. Thermally induced structural changes occurring on the surfaces of the TiO2Zy-Al2O3 and BaOZ TiO 2Zy-Al2O3 systems were studied in a comparative manner within 300-1273 K via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, and BET surface area analysis. The surface acidity of the studied oxide systems was also investigated via pyridine adsorption monitored by in-situ Fourier transform infrared (FTIR) spectroscopy. BaO/TiO2γ-Al 2O3 ternary oxide was synthesized by incorporating different loadings of (8-20 wt %) BaO onto the TiO2/γ Al 2O3 support material, which was originally prepared using the sol-gel method. In the TiO2Zy-Al2O3 binary oxide support material, anatase phase exhibited a relatively high thermal stability at T < 1073 K. The presence of TiO2 domains on the surface of the alumina particles was found to alter the surface acidity of alumina by providing new medium-strength Lewis acid sites. SEMZEDX results indicate that in the BaO/TiO2γ-Al2O3 system, TiO2 domains present a significant affinity toward BaO and/or Ba(NO3) 2 resulting in a strong Ti-Ba interaction and the formation of overlapping domains on the surface. The presence of TiO2 also leads to a decrease in the decomposition temperature of the Ba(N03) 2 phase with respect to the Ti-free Ba(N03) 2ZyAl2O3 system. Such a destabilization is likely to occur due to a weaker interaction between Ba(N03) 2 and y-Al203 domains in the ternary oxide as well as due to the change in the surface acidity in the presence of TiO 2. At relatively high temperatures (e.g., 873-1273 K) formation of complex structures in the form of BaTiO3, Ba1.23Al 2.46Ti5.54O16, BaTiO5, andor Ba x:AlyTizOn., were also observed. © 2009 American Chemical Society.