Aluminum oxide ceramic aerogel fibers and sol-gel spinning preparation method thereof
A technology of alumina ceramics and gel spinning, which is applied in the field of ceramics and can solve problems such as weak heat insulation and weight reduction
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[0027] One aspect of the embodiments of the present invention provides a method for preparing alumina ceramic airgel fibers by sol-gel spinning, which includes three key steps:
[0028] (1) Uniformly disperse the linear organosilicon oligomer and the aluminum source in the organic solution, add a catalyst, and react for a certain period of time to prepare a sol;
[0029] (2) spinning the sol in a coagulation bath to form a gel fiber;
[0030] (3) The gel fiber is replaced by a solvent, dried with a supercritical fluid, and finally calcined to prepare the continuous alumina ceramic airgel fiber.
[0031] In some embodiments, the organosilane oligomers include polydiethoxysiloxane, polydimethoxysiloxane, polymethylethoxysiloxane, polymethylmethoxysiloxane alkane, polyhexylethoxysiloxane, polyhexylmethoxysiloxane, alkoxysiloxane copolymer, and not limited thereto.
[0032] Further, the repeating unit of the silicone polymer is 5-20.
[0033] Further, the aluminum source includ...
Embodiment 1
[0054] (1) Synthesis of alumina ceramic precursor sol: take 1 mol of polydiethoxysiloxane with an average repeating unit number of 5, 8 mol of aluminum powder and 2 mol of aluminum nitrate nonahydrate, disperse them in 12 mol of methanol, and stir vigorously , and then add 0.01mol of potassium hydroxide, and stir at room temperature for 10 hours to obtain a precursor sol. The schematic diagram of the precursor structure can be found in figure 1 .
[0055] (2) Spinning: configure 1L ethanol as a coagulation bath, heat and maintain at 40°C, spin the above precursor sol into the coagulation bath and collect it with a roller to obtain alumina gel fibers.
[0056] (3) Solvent replacement, drying and calcination: the obtained alumina gel fiber was replaced in methanol for 3 times, and the replacement time was 5 hours each time. After the replacement, it was dried with supercritical methanol for 5 hours to obtain the alumina airgel fiber. Then calcined at 800°C for 10 minutes, and t...
Embodiment 2
[0058] (1) Synthesis of alumina ceramic precursor sol: take 1 mol of polydimethoxysiloxane with an average repeating unit of 8, 10 mol of aluminum chloride and 3 mol of aluminum sulfate, disperse them in 15 mol of butanol, stir well Add 0.03mol of ammonia water and stir at 50°C for 3 hours to obtain a precursor sol. For the schematic diagram of the precursor structure, see figure 1 .
[0059] (2) Spinning: Configure 2L of n-hexane as a coagulation bath, heat and maintain 50°C, spin the above precursor sol into the coagulation bath and collect it with a roller to obtain alumina gel fibers.
[0060] (3) Solvent replacement, drying and calcination: the obtained alumina gel fiber was replaced 4 times in ethanol, and the replacement time was 12 hours each time. After the replacement, supercritical ethanol was used to dry for 24 hours to obtain the alumina airgel fiber. Then calcined at 900°C for 30 minutes, and then calcined at 1300°C for 10 minutes to obtain an alumina ceramic ai...
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