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Facile Preparation of Macroporous Structures Assembled from Branched Cu<sub>2</sub>O Crystals
Facile Preparation of Macroporous Structures Assembled from Branched Cu2O Crystals
Bulletin of the Korean Chemical Society. 2014. Aug, 35(8): 2533-2536
Copyright © 2014, Korea Chemical Society
  • Received : March 17, 2014
  • Accepted : April 03, 2014
  • Published : August 20, 2014
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Young-Sik Cho
Young-Duk Huh

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Experimental
CuCl 2 · 2H 2 O (99%, Aldrich), polyethylene glycol (PEG, Mw 20,000, Aldrich), D-(+)-glucose (ACS reagent, Aldrich), and N,N,N′,N′- tetramethyl ethylenediamine (TMEDA, 98%, TCI) were used as received. The microwave-assisted method used here for the preparation of the Cu 2 O products is similar to that of our previous study.18 In a typical preparation of a Cu 2 O product, 10 mL of a 4.16 mM aqueous D-(+)-glucose solution and 0.2 g PEG were added to 139.9 mL of a 1.19 mM CuCl 2 ·2H 2 O aqueous solution with stirring at room temperature for 30 min. Then, 0.0622 mL TMEDA was added to the solution. The total volume of the aqueous solution was fixed at 150 mL. In this case, the final reactant concentrations of CuCl 2 ·2H 2 O, D-(+)-glucose, TMEDA, and PEG were 1.11 mM, 0.277 mM, 2.77 mM, and 66.0 mM, respectively. To investigate the variation in the branched shapes of the Cu 2 O products, four different concentrations of CuCl 2 ·2H 2 O (1.11 mM, 2.22 mM, 4.44 mM, and 13.3 mM) were used while keeping the relative reactant concentrations constant. The final mixed solution was placed into a commercial microwave oven (Magic MWO-230KD, 2.45 GHz, 800 W). When we examined the effects of varying the CuCl 2 ·2H 2 O concentration on the shapes of the Cu 2 O products, the microwave irradiation time was set at 240 s. Powder forms of the Cu 2 O products were obtained by using a centrifuge at 4000 rpm for 10 min. The Cu 2 O products were then washed several times with ethanol and water, and then dried at 60 °C for 12 h in a drying oven.
The crystal structures of the Cu 2 O products were characterized by using powder X-ray diffraction (XRD, PANalytical, X’Pert-proMPD). The morphologies of the Cu 2 O products were examined by performing scanning electron microscopy (SEM, Hitachi S-4300) and high-resolution transmission electron microscopy (HRTEM, JEOL JEM-3010).
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