Kosińska-Klähn Magdalena, John Łukasz, Drąg-Jarząbek Anna, Utko Józef, Petrus Rafał, Jerzykiewicz Lucjan B, Sobota Piotr
Faculty of Chemistry, University of Wrocław , 14 F. Joliot-Curie, 50-383 Wrocław, Poland.
Inorg Chem. 2014 Feb 3;53(3):1630-6. doi: 10.1021/ic402987n. Epub 2014 Jan 10.
In this Article, we present how the molecular precursor of binary oxide material having an excess of alkali earth metal can be transformed to the highly phase pure BaTiO3 perovskite. Here, we synthesized and compared two barium-titanium complexes with and without chloride ligands to determine the influences of different ligands on the phase purity of binary oxide nanoparticles. We prepared two barium-titanium complexes, i.e., [Ba4Ti2(μ6-O)(OCH2CH2OCH3)10(HOCH2CH2OCH3)2(HOOCCPh3)4] (1) and [Ba4Ti2(μ6-O)(μ3,η2-OCH2CH2OCH3)8(μ-OCH2CH2OCH3)2(μ-HOCH2CH2OCH3)4Cl4] (2). The barium-titanium precursors were characterized using elemental analysis, infrared and nuclear magnetic resonance spectroscopies, and single-crystal X-ray structural analysis, and their thermal decomposition products were compared. The complex 1 decomposed at 800 °C to give a mixture of BaTiO3 and Ba2TiO4, whereas 2 gave a BaCl2/BaTiO3 mixture. Particles of submicrometer size (30-50 nm) were obtained after leaching of BaCl2 from the raw powder using deionized water. Preliminary studies of barium titanate doped with Eu(3+) sintered at 900 °C showed that the dominant luminescence band arose from the strong electric dipole transition, (5)D0-(7)F2.
在本文中，我们展示了具有过量碱土金属的二元氧化物材料的分子前驱体如何转化为高相纯的钛酸钡钙钛矿。在此，我们合成并比较了两种含和不含氯配体的钡钛配合物，以确定不同配体对二元氧化物纳米颗粒相纯度的影响。我们制备了两种钡钛配合物，即[Ba4Ti2(μ6-O)(OCH2CH2OCH3)10(HOCH2CH2OCH3)2(HOOCCPh3)4]（1）和[Ba4Ti2(μ6-O)(μ3,η2-OCH2CH2OCH3)8(μ-OCH2CH2OCH3)2(μ-HOCH2CH2OCH3)4Cl4]（2）。使用元素分析、红外和核磁共振光谱以及单晶X射线结构分析对钡钛前驱体进行了表征，并比较了它们的热分解产物。配合物1在800℃分解，得到BaTiO3和Ba2TiO4的混合物，而配合物2得到BaCl2/BaTiO3混合物。使用去离子水从原始粉末中浸出BaCl2后，获得了亚微米尺寸（30 - 50 nm）的颗粒。对在900℃烧结的Eu(3+)掺杂钛酸钡的初步研究表明，主要发光带源于强电偶极跃迁(5)D0-(7)F2。
