Method for preparing silicone carbide fibre by thermochemical crosslinking and crosslinking apparatus therefor

A silicon carbide fiber, thermochemical cross-linking technology, applied in the direction of fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of low oxygen content in fibers, complex process, expensive equipment, etc., achieve less consumption, simple process, low cost effect

Inactive Publication Date: 2008-10-08
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Chemical vapor phase crosslinking (Y Hasssegawa, J Inorg Organomet Polym, 1991, 2(1), 161) can well transform the precursor fibrils from a linear structure to a network crosslinked structure, while effectively controlling the introduction of oxygen , but it has strict requirements on the choice of atmosphere and crosslinking agent; electron beam radiation crosslinking is an effective method for preparing commercial SiC fibers (Tadao Seguchi, Radiation PhySiCs and Chemistry, 2000, 57, 367-371; Seiji Kamimura, TadaoSeguchi, Kiyohito Okamura, Radiation PhySiCs and Chemistry, 1999, 54, 575-581), the crosslinking process is carried out under anhydrous and oxygen-free conditions, and the prepared fiber has low oxygen content, but its process is complicated, the equipment is expensive, and the cost higher

Method used

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  • Method for preparing silicone carbide fibre by thermochemical crosslinking and crosslinking apparatus therefor
  • Method for preparing silicone carbide fibre by thermochemical crosslinking and crosslinking apparatus therefor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Such as figure 1 As shown, the cross-linking device includes an inlet pipe 1, a gas flow control valve 2, a flange 3, a sealing steel sleeve 4, a quartz glass tube 5, a heating coil 6, a quartz boat 7 and an air outlet pipe 8, and the heating coil 6 is set on the quartz glass Outside the pipe 5, the air inlet pipe 1 and the air outlet pipe 8 are respectively connected to both ends of the quartz glass pipe 5 through the sealed steel sleeve 4, and the quartz boat 7 is placed in the quartz glass pipe; the sealed steel sleeve includes an inner steel sleeve 4-1 with external threads and the outer steel sleeve 4-2 of the internal thread, the sealing ring 4-3 is used to seal between the inner steel sleeve 4-1 and the outer steel sleeve 4-2; the air intake pipe 1 and the air outlet pipe 8 are respectively composed of two sections of large diameter and small diameter One end of the large-diameter pipe 1-1, 8-1 is connected to the outer steel sleeve 4-2 of the sealed steel sleeve...

Embodiment 2

[0033] Technological process is with embodiment 1. The content of water in THF is 0.08%, cross-linking agent adopts aluminum isopropoxide (AIP), the mass ratio of PCS and AIP is 100: 0.5, and AIP consumption is 5mg, and the total amount of THF is 17ml, and the average molecular weight of PCS is 2800 , the viscosity of the spinning slurry reaches 20Pa.s, the number of holes in the spinneret is 200, and the average diameter of each hole is 80μm. The spinning speed is 400m / s, the average diameter of the PCS precursor is 30μm, the cross-linking protective gas is nitrogen, the purity is 99.9%, and the gas flow rate is 1000L / min. The crosslinking temperature is controlled at 260°C, the crosslinking time is 20hrs, and the PCS crosslinked fiber with a weight loss rate of 2.68% and a crosslinking degree of 73.06% is obtained; the high-temperature furnace uses high-purity nitrogen as a protective gas with a purity of 99.9%. The heating rate is 2500L / min, the heating rate is 10℃ / min bel...

Embodiment 3

[0036] Technological process is with embodiment 1. The content of water in THF is 0.08%, cross-linking agent adopts titanium isopropoxide (TIP), the mass ratio of PCS and TIP is 100: 0.2, and TIP consumption is 2mg, and the total amount of THF is 22ml, and the average molecular weight of PCS is 3600 , the viscosity of the spinning slurry reaches 28Pa.s, the number of holes in the spinneret is 20, and the average diameter of each hole is 80μm. The spinning speed is 800m / s, the average diameter of the PCS precursor is 22μm, the cross-linking protective gas is nitrogen, the purity is 99.999%, and the gas flow rate is 200L / min. The crosslinking temperature is controlled at 180°C, the crosslinking time is 6hrs, and the PCS crosslinked fiber with a weight loss rate of 0.06% and a crosslinking degree of 6.2% is obtained; the high-temperature furnace uses high-purity nitrogen as a protective gas with a purity of 99.999%. 1500L / min, the heating rate is 15°C / min below 400°C and above 8...

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Abstract

A thermo-chemical cross-linking preparation method of silicone carbide fiber and a cross-linking device relates to a silicone carbide fiber, in particular to a method that the thermo-chemical cross-linking of organometallic compounds is used for the preparation of silicone carbide fiber and the cross-linking device of the method, which provides a thermo-chemical cross-linking preparation method of silicone carbide fiber and a cross-linking device of the method and provided with a quartz glass tube, an inlet tube, an outlet tube, a sealing steel sleeve, a gas flow control valve, a heating coil and a quartz boat. The heating coil is arranged outside of the quartz glass tube. The inlet and outlet tubes are respectively linked on both ends of the quartz glass tube through the sealing steel sleeve, and the quartz is disposed inside the quartz glass tube. The PCS and a cross-linking agent are dissolved in the trtrahydrofuran, and the slurry is produced. The slurry is in ageing and with the dry-spinning, thus the precursor fiber is produced. The precursor disposed into the quartz is then disposed into the cross-linking device for the thermo-chemical cross-linking. The PCS cross-linking fiber is obtained, which is then disposed into a high-temperature furnace for pyrolysis and sintering. Therefore, the silicon carbide fiber is produced.

Description

technical field [0001] The invention relates to a silicon carbide fiber, in particular to a method for preparing a silicon carbide (SiC) fiber by thermochemical crosslinking of an organometallic compound and a crosslinking device thereof. Background technique [0002] SiC fiber has the advantages of high strength, excellent heat resistance, oxidation resistance and high temperature creep resistance. Due to its outstanding performance, SiC fiber has become a key material for aerospace, national defense weaponry, nuclear radiation-resistant components and ceramic engines, and is also widely used in various civilian fields. [0003] There are many ways to prepare SiC fibers. At present, the most mature technology for preparing SiC fibers is based on the precursor method researched and developed by Yajima (Chemical Letters, 1975: 931; Chemical Letters, 1975: 551). This method first synthesizes polysilane through the polymerization of organosilane, and then through Polymer chai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10
Inventor 罗学涛郑淞生蔡靖刘春佳吴义伯严星煌于瑞敏
Owner XIAMEN UNIV
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