高濃度塩酸水溶液中四塩化チタンの低温加水分解反応により生成する酸化チタン超微粒子のキャラクタリゼーション(アナリティカルレポート)

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Ultrafine particles of TiO_2 were prepared by the hydrolysis of titanium tetrachloride (TiCl_4) in a highly concentrated hydrochloric acid aqueous solution at a low temperature, in which the surfacing modifier did not coexist. The absorption spectrum of the prepared TiO_2 ultrafine particle showed a blue shift, which was more remarkable than that of a bulk sample. The fluorescence of the prepared TiO_2 fine particles confirmed being within the ultraviolet wavelength range with a peak at 370nm by changing the excitation wavelength from 220nm to 300nm. The bulk TiO_2 of Rutile and Anatase type showed light absorption in proportion to the transition of inter-bands at 413nm (3.0 eV) and 388nm (3.2 eV), respectively. Because the excitation wavelength of 230nm corresponds to 5.4 eV, it is converted into the band energy. The size of TiO_2 identified from a laser scatter measurement was 3.5±1.0nm, which was confirmed to be the size at which a quantum size effect appears. From the XRD measurement, secondary fine particles (aggregate) of TiO_2 after separation by a membrane filter was identified to be of the Rutile type. The size of the (110), (101) and (211) crystal planes were estimated to be 5.3, 8.0 and 5.1nm by an evaluation using the Scherrer equation for the half-value width of the diffraction peak of each crystal plane. The shape of the aggregate observed from the SEM image was tabular, of μm size. It was concluded that TiO_2 fine particles with a hierarchy of sizes from nm to μm were possible by the low-temperature hydrolysis of TiCl_4 in a high concentration of hydrochloric acid aqueous solution. Application to an ultraviolet ray protective agent for UVC, UVB and UVA is expected in the future.
社団法人日本分析化学会の論文
2007-01-05

高濃度塩酸水溶液中四塩化チタンの低温加水分解反応により生成する酸化チタン超微粒子のキャラクタリゼーション(アナリティカルレポート)

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