Preparation method of si-al-c-o fiber

A si-al-c-o fiber technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of difficult control of high-temperature firing process conditions, complex and cumbersome synthesis process, uncontrollable aluminum content, etc., and achieve various properties The effect of stability, simple synthesis process, and high average tensile strength

Active Publication Date: 2021-04-06
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Another object of the present invention is to address the complex and cumbersome synthesis process of aluminum-containing precursors in the process of preparing aluminum-containing SiC fibers by the precursor conversion method, poor product uniformity, uncontrollable aluminum content, melt spinning, air non-melting treatment and high-temperature firing. It is difficult to control the process conditions and other problems, and a method for preparing Si-Al-C-O fibers with excellent performance is provided.

Method used

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  • Preparation method of si-al-c-o fiber
  • Preparation method of si-al-c-o fiber
  • Preparation method of si-al-c-o fiber

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0030] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0031] At 60°C, 15.00g of polycarbosilane (PCS) was dissolved in xylene to obtain a polycarbosilane solution; 1.00g of 8-hydroxyquinoline aluminum was dissolved in N,N-dimethylformamide (DMF) to obtain 8-Hydroxyquinoline aluminum solution. Mix the polycarbosilane solution and the 8-hydroxyquinoline aluminum solution to obtain a clear solution, and transfer it to a reaction kettle, place the reaction kettle in a high-temperature oven, raise the temperature to 280 ° C, and keep it warm for 1 hour. During the reaction, the reaction kettle The pressure is 0.5 ~ 2MPa, cooled to room temperature to obtain a solution of the synthesized product; distilled to obtain a light yellow and transparent resinous aluminum-containing precursor polyaluminocarbosilane, such as figure 1 shown.

[0032] (2) Preparation of Si-Al-C-O fibers

[0033] Under the condition of argon protection, the aluminum-containing prec...

Embodiment 2

[0037] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0038] Dissolve 15.00g polycarbosilane (PCS) in xylene to obtain polycarbosilane solution; dissolve 1.00g 8-hydroxyquinoline aluminum in N,N-dimethylformamide (DMF) to obtain 8-hydroxyquinoline aluminum Aluminum quinoline solution. Mix the polycarbosilane solution and the 8-hydroxyquinoline aluminum solution to obtain a clear solution, and transfer it to a reaction kettle, place the reaction kettle in a high-temperature oven, raise the temperature to 280 ° C, and keep it warm for 1 hour. During the reaction, the reaction kettle The pressure is 0.5-2MPa, cooling to room temperature to obtain a solution of the synthesized product; distillation to obtain aluminum-containing precursor polyaluminocarbosilane.

[0039] (2) Preparation of Si-Al-C-O fibers

[0040] Under the condition of argon protection, the aluminum-containing precursor prepared in step (1) was heated to 343 °C through a single-hole s...

Embodiment 3

[0044] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0045] Dissolve 15.00g polycarbosilane (PCS) in xylene to obtain polycarbosilane solution; dissolve 1.00g 8-hydroxyquinoline aluminum in N,N-dimethylformamide (DMF) to obtain 8-hydroxyquinoline aluminum Aluminum quinoline solution. Mix the polycarbosilane solution and the 8-hydroxyquinoline aluminum solution to obtain a clear solution, and transfer it to a reaction kettle, place the reaction kettle in a high-temperature oven, raise the temperature to 280 ° C, and keep it warm for 1 hour. During the reaction, the reaction kettle The pressure is 0.5-2MPa, cooling to room temperature to obtain a solution of the synthesized product; distillation to obtain aluminum-containing precursor polyaluminocarbosilane.

[0046] (2) Preparation of Si-Al-C-O fibers

[0047] Under the condition of argon protection, heat the aluminum-containing precursor polyaluminocarbosilane prepared in step (1) to 340°C through...

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Abstract

Preparation method of Si-Al-C-O fiber. The invention discloses a preparation method of polyaluminocarbosilane, comprising: uniformly mixing polyaluminocarbosilane solution and 8-hydroxyquinoline aluminum solution, and reacting for 0.5-2 MPa at a temperature of 230-300°C and a pressure of 0.5-2 MPa. 2h, distilled. The invention also discloses a method for further processing the polyaluminocarbosilane prepared by the above method to prepare Si-Al-C-O fibers. The aluminum-containing precursor prepared by the method of the present invention is more uniform than the precursor synthesized by the normal-pressure high-temperature solid phase, the aluminum content is controllable, the synthesis process is simpler, and the safety is high; the softening point of the synthesized aluminum-containing precursor is high, and it can be Good spinnability, high spinning stability, high yield after high-temperature firing; the prepared Si‑Al‑C‑O fiber is smooth, black and bright; the average diameter is small; the average tensile strength is high, and the performance is stable; it can be directly It is used as a reinforcement in high-temperature-resistant materials, and can also be further sintered at ultra-high temperature to obtain polycrystalline Si‑Al‑C fibers.

Description

technical field [0001] The invention belongs to the field of ceramic fiber materials, and in particular relates to a preparation method of Si-Al-C-O ceramic fiber materials. [0002] technical background [0003] Continuous thin-diameter SiC fibers are ideal for high-performance ceramic matrix composites due to their excellent properties such as high strength (1-4GPa), high modulus (150-400GPa), high temperature resistance (>1000°C), oxidation resistance and creep resistance. Enhanced (tough) body. Among them, the high temperature resistance of aluminum-containing SiC fibers is particularly outstanding. It can withstand high temperatures exceeding 1800 ° C and has a wide range of applications in high temperature fields. [0004] There are many scientific research institutions and companies researching aluminum-containing SiC fibers. Tyranno SA fiber studied by Ishikawa et al. (Ishikawa T, Kohtoku Y, Kumagawa K, et al. High-strength alkali-resistant sintered SiCfibrestabl...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G77/60D01F9/10
CPCC08G77/60D01F9/10
Inventor刘玉付储昭杰
OwnerSOUTHEAST UNIV