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Si-Al-C-O fiber preparation method

A si-al-c-o, fiber technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of difficult to control high-temperature firing process conditions, complex and tedious synthesis process, poor product uniformity, etc., and achieve stable performance. , The effect of simple synthesis process and controllable aluminum content

Active Publication Date: 2019-01-01
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] 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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Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0030] 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.

[0031] (2) Preparation of Si-Al-C-O fibers

[0032] Under the condition of argon protection, the aluminum-containing prec...

Embodiment 2

[0036] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0037] 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.

[0038] (2) Preparation of Si-Al-C-O fibers

[0039] 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

[0043] (1) Preparation of aluminum-containing precursor polyaluminocarbosilane

[0044] 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.

[0045] (2) Preparation of Si-Al-C-O fibers

[0046] 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

The invention provides a Si-Al-C-O fiber preparation method, and discloses a polyaluminocarbosilane preparation method, which comprises: uniformly mixing a polycarbosilane solution and an 8-hydroxyquinoline aluminum solution, carrying out a reaction for 0.5-2 h at a temperature of 230-300 DEGC under a pressure of 0.5-2 Mpa, and distilling. The invention further discloses a method for preparing Si-Al-C-O fiber by carrying out further treatment on the polyaluminocarbosilane prepared by the method. According to the present invention, the prepared aluminum-containing precursor has advantages of uniformity, controlled aluminum content, simple synthesis process and high safety compared to the precursor obtained through the normal pressure solid phase synthesis; the prepared aluminum-containing precursor has advantages of high softening point, good spinnability, high spinning stability and high yield after high temperature firing; and the prepared Si-Al-C-O fibers are smooth, black and bright, have characteristics of small average diameter, high average tensile strength and stable performance, can be directly used as the reinforcing body in high-temperature-resistant materials, and can befurther subjected to ultrahigh temperature sintering 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. technical background [0002] 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. [0003] 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 SiCfibrestable to2, 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60D01F9/10
CPCC08G77/60D01F9/10
Inventor 刘玉付储昭杰
Owner SOUTHEAST UNIV
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