Preparation of Barium (II) Copper (II) Binuclear Complex Particles and their Conversion into Composite Oxides
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概要
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Moderatesy uniform binuclear complex particles, N, N'-bis (3-carboxysalicylidene) -1, 2-ethanediaminobarium (II) copper (II) monohydrate, C<SUB>18</SUB>H<SUB>12</SUB>N<SUB>2</SUB>O<SUB>6</SUB>BaCu · H<SUB>2</SUB>O ; BaCu (fsaen) · H<SUB>2</SUB>O, were prepared by mixing a N, N'-bis (3-carboxysalicylidene) -1, 2-ethanediaminocopper (II) hemihydrate, Cu (H<SUB>2</SUB>fsaen) · 0.5H<SUB>2</SUB>O, solution and a barium (II) nitrate solution under the conditions of [Cu (H<SUB>2</SUB>fsaen)] <SUB>t</SUB> = 3.0×10<SUP>-3</SUP> mol [13a<SUP>2+</SUP>] <SUB>t</SUB>/ [Cu (H<SUB>2</SUB>fsaen)] <SUB>t</SUB>= 1.0, and a methanol content of 75% by volume at 1°C. The latter starting mononuclear copper (II) complex was prepared through direct reaction of 3-formylsalicylic acid (H<SUB>2</SUB>fsa), 1, 2-ethanediamine (en), and copper (II) nitrate in a sodium carbonate solution. An average size of the binuclear complex particles was 4.8, μm with a relative standard deviation of 0.2. A molar ratio, n (Ba) /n (Cu), of the particles was estimated to be 0.974, which corresponded to an equimolar hetero metal complex. A yield of the resulting products was estimated to be 89%. Morphology and size of these complex particles depended on the concentrations of the mononuclear copper (II) complex and methanol in the mixed solution.. The binuclear complex particles were converted into composite barium (II) copper (II) oxide, BaCuO<SUB>2</SUB>, via γ-barium (II) carbonate and copper (II) oxide through calcination at 850°C for 3 h. Correlation between radii of the metal ions and bond length in the hetero metal complex was explained on the basis of the ligand molecule structure. Additionally, segregation of barium (II) ions at outermost layers of the composite oxide surface was discussed according to results of X-ray photoelectron spectrometry.
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