Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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Solvothermal Synthesis of Supercrystals of Hematite via the Self-assembly of Nanocubes

  • Received : 2013.12.30
  • Accepted : 2014.02.05
  • Published : 2014.06.20
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Abstract

Keywords

Experimental Section

FeCl3⋅6H2O (Aldrich), K4Fe(CN)6 (Aldrich), sodium oleate (TCI), oleic acid (Aldrich), and tetraoctylammonium bro-mide (TOABr, Aldrich) were used as received. In a typical synthesis of α-Fe2O3 supercrystals, 0.10 M FeCl3⋅6H2O was dissolved in 20 mL water. 1.83 g sodium oleate, 5.0 mL oleic acid, and 40 mL toluene were then added to the solution. The water-toluene bilayer mixture was vigorously stirring for 1 h at room temperature to allow the transfer of Fe3+ ions from the aqueous solution to the toluene phase through coordination with the oleate anions to form iron-oleate complexes. 3.28 g TOABr in 40 mL toluene was then added to 20 mL aqueous solution of Fe(CN)64− ions to obtain the TOA-[Fe(CN)6] complexes into the toluene phase. The two toluene solutions containing the Fe-OA and TOA-[Fe(CN)6] complexes were mixed under stirring. After mix-ing the two optically transparent solutions, the resulting solution was transferred to a 100 mL Teflon-lined autoclave. To prepare the α-Fe2O3 supercrystals, solvothermal reactions were conducted at 180 °C for 72 h. The product was collect-ed by centrifuging the solution at 4000 rpm for 10 min. The precipitated products were washed several times with water and ethanol, and dried at 60 °C for 12 h.

The α-Fe2O3 product was examined with a Raman micro-scope (Kaiser, RamanRxn Microprobe). The capping organic compound in the supercrystals of α-Fe2O3 was examined by using an FT-IR spectrometer (Perkin Elmer 100 FT-IR). The α-Fe2O3 product was also analyzed by powder X-ray diffr-action (XRD, PANanlytical, X’pert-pro MPD) using Cu Kα radiation. The morphologies of the supercrystals and the superlattice patterns of the nanocubes of α-Fe2O3 were ex-amined by using scanning electron microscopy (SEM, Hitachi S-4300) and high resolution transmission electron micro-scopy (HRTEM, JEOL JEM-3010), respectively.

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