High-temperature-resistant ultra-light aluminum oxide ceramic fibers and sol-gel preparation method thereof
A kind of technology of alumina ceramics and high temperature resistance, which is applied in the synthesis and preparation of high temperature resistant ceramic fibers and the field of sol-gel preparation of alumina ceramic fibers, which can solve the problems of limited application, high density and high thermal conductivity, and achieve huge Application potential, inhibition of crystal transformation and growth, effect of uniform distribution
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[0030] One aspect of the embodiments of the present invention provides a method for preparing high-temperature-resistant ultra-light alumina ceramic fibers, including three key steps:
[0031] (1) Fully dissolve aluminum source, organosiloxane, water, and acid catalyst in an organic solvent, react at a certain temperature for a certain period of time, then add tantalum compound and hafnium chemical substance, and prepare spinning stock solution after stirring evenly;
[0032] (2) Configure an alkaline coagulation bath, continuously spin the spinning stock solution into the alkaline coagulation bath, and form alumina gel fibers through sol-gel chemical transformation;
[0033] (3) Perform solvent replacement at room temperature, then use supercritical fluid technology to dry the alumina gel fiber, and then calcinate step by step to prepare high-temperature-resistant ultra-light alumina ceramic fiber.
[0034] In some embodiments, the aluminum source includes any one or a combin...
Embodiment 1
[0065] (1) Preparation of spinning stock solution: Disperse 80g of aluminum powder and 50g of aluminum isopropoxide in 200g of ethanol, then add 5g of tetraethyl orthosilicate dropwise thereto, stir well, then add 1g of deionized water and 0.05g of hydrochloric acid , stirred and reacted at 80° C. for 24 hours, respectively added 0.1 g of tantalum powder and 5 g of hafnium dioxide to the composite solution, and stirred evenly to obtain a spinning stock solution.
[0066] (2) Preparation of coagulation bath: take 1L of ethanol, add 0.1g sodium hydroxide, stir for 5 hours to obtain a coagulation bath; control the temperature of the coagulation bath at 10°C, and then spin the spinning dope prepared in step (1) into In the coagulation bath, it is collected by a roller to obtain alumina gel fibers.
[0067] (3) Replace the above-mentioned alumina gel fiber with methanol for 3 times, each replacement time is 12 hours, then replace with supercritical methanol for 24 hours, then calci...
Embodiment 2
[0069] (1) Preparation of spinning stock solution: Disperse 100g of aluminum powder in 100g of methanol, then dropwise add 1g of methyl orthosilicate, stir well, then add 0.05g of deionized water and 0.01g of hydrochloric acid, and stir at 50°C After reacting for 20 hours, 1 g of lithium tantalate and 2.5 g of hafnium oxychloride hydrate were respectively added to the composite solution, and stirred evenly to prepare a spinning stock solution.
[0070] (2) Preparation of coagulation bath: take 1L of methanol, add 0.01g of sodium hydroxide, stir for 2 hours to obtain a coagulation bath; control the temperature of the coagulation bath at 50°C, and then spin the spinning dope prepared in step (1) into into the coagulation bath and collected by a roller to obtain alumina gel fibers.
[0071] (3) Replace the above-mentioned alumina gel fiber with ethanol for 4 times, each replacement time is 5 hours, then replace with supercritical ethanol for 5 hours, then calcined at 800°C for 10...
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