Preparation of Oxide Fibers from Metal Alcoholates

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  • KAMIYA Kanichi
    Department of Industrial Chemistry, Faculty of Engineering, Mie University
  • SAKKA Sumio
    Department of Industrial Chemistry, Faculty of Engineering, Mie University
  • ITO Satoshi
    Department of Industrial Chemistry, Faculty of Engineering, Mie University

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Other Title
  • 金属アルコレートを原料とする酸化物繊維の製造　　水及び酸の添加による紡糸可能なＴｉＯ?S２?T‐ＳｉＯ?S２?T系アルコレート溶液の調製
  • キンゾク アルコレート オ ゲンリョウ ト スル サンカブツ センイ ノ セイ
  • 水及び酸の添加による紡糸可能なTiO<sub>2</sub>-SiO<sub>2</sub>系アルコレート溶液の調製

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The viscous and spinnable alcoholate mixtures of Ti (O-isoC3H7)4 and Si(O-C2H5)4 corresponding to the oxide composition of 10TiO2⋅90SiO2, 30TiO2⋅70SiO2 and 50TiO2⋅50SiO2 by weight were prepared by hydrolysis by adding hydrochloric acid and water at ambient temperature (ca. 20°C) after bubbling with CO2 gas and water vapor at 30°C. Without pretreating with CO2 gas and water vapor, the addition of HCl and water as alcoholic solution, even by very low concentrations, to the solution of the alcoholates caused undissolved white streak of locally hydrolyzed alcoholate which made the drawing fiber from the solution impossible. Pretreating the solution of alcoholate with CO2 gas and water vapor for longer than 15h allowed the addition of HCl and water with no undissolved precipitate, and made the solution spinnable. When the amount of water added after pretreatment was limited up to 0.5-0.6 of that required for the complete hydrolysis of the alcoholates, spinnability of the solution depended mainly on the amount of added HCl. Fibrous materials corresponding to the composition of 10TiO2⋅90SiO2, 30TiO2⋅70SiO2 and 50TiO2⋅50SiO2 could be drawn from the solutions pretreated for 20h only when the molar ratio of the added HCl to alcoholates was in the range between 1.0 and 4.0×10-4. By increase of pretreatment time, larger amount of HCl could be added to have spinnable solution, and time required for the solution to reach spinnable state shortened. Transparent glass fibers were obtained by heating the fibrous materials to 500°C.

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