Supporting Information Microspheres with an Au@SiO2 Core and Mesoporous Aluminosilica Shell as Superior Heterogeneous Catalyst for the Aerobic Epoxidation of cis-Cyclooctene
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چکیده
copper specimen grids (300 meshes) with formvar/carbon (Beijing XXBR Technology Co.) were employed as received without further purifications. Deionized (DI) water (resistance >18.2 MΩ • cm-1) was used in all of our experiments. Characterization: Nitrogen physisorption isotherms were measured at 77 K with a static volumetric instrument Autosorb-6b (Quanta Chrome). Prior to each measurement, the sample was outgassed at 373 K to a residual pressure below 10 −4 Torr. A Baratron pressure transducer (0.001–10 Torr) was used for low-pressure measurements. The specific surface area was estimated by the Brunauer–Emmett–Teller (BET) method. 1 The pore size distribution (PSD) was calculated from the adsorption branch using the Barrett–Joyner–Halenda (BJH) method. 2 Powder XRD measurements were conducted on a Bruker AXS D8 X-ray diffraction meter (Cu Kα, λ=1.5406 Ǻ, 40 kV, 30 mA) under ambient conditions. Diffraction data were collected with a solution of 0.02º (2θ) in the angle range 20-90 º. Prior to test, samples were dried at 373 K overnight. TEM was performed on a JEOL JEM-1400, operated at 100 kV. The samples were suspended in DI water and dried on holey carbon-coated Cu grids. The mean particle diameter was calculated from the mean frequency distribution by counting ca. 200 particles according to: where Ʃ is the sum of i over the entire sample, n i is the i i i n d n d number of particles with particle diameter d i in a certain range. The XPS measurements were performed on a VG Escalab 250 spectrometer equipped with an Al anode (Al Ka = 1486.6 eV). The background pressure in the analysis chamber was lower than 1×10 −7 Pa.
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تاریخ انتشار 2015