Preparation of Oxide Fibers from Metal Alcoholates

KAMIYA Kanichi, SAKKA Sumio, ITO Satoshi

doi:10.2109/jcersj1950.85.988_599

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.

Preparation of Oxide Fibers from Metal Alcoholates

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