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Nitride fiber thermal cross-linking assisted atmosphere non-melting method

A nitride and thermal crosslinking technology, which is applied in the fields of fiber chemical characteristics, rayon chemical post-treatment, textiles and papermaking, etc., can solve the problems of unsatisfactory non-melting effect, high cost, and low cost, so as to improve the non-melting effect , Low production cost and high production efficiency

Active Publication Date: 2020-04-03
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides an atmosphere non-melting method assisted by thermal crosslinking of nitride fibers, which is used to overcome the defects in the prior art that may lead to the introduction of heterogeneous elements, high cost, unsatisfactory non-melting effect and long time. The method of the present invention It can take into account the non-melting efficiency and the degree of non-melting, and achieve a high degree of low softening point nitride fibrils, uniform non-melting, and low cost, laying the foundation for the subsequent preparation of high-performance nitride fibers

Method used

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  • Nitride fiber thermal cross-linking assisted atmosphere non-melting method

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Experimental program
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Effect test

Embodiment 1

[0036] The present invention provides a kind of atmosphere non-melting method assisted by thermal crosslinking of nitride fiber, comprising the following steps:

[0037] (1) Place 100g polyborosilazane fiber sample in a non-melting atmosphere furnace, vacuumize and replace with high-purity nitrogen, and repeat the operation three times;

[0038] (2) In a high-purity nitrogen atmosphere, the temperature is raised from room temperature to 50 °C at a rate of 1 °C / min, and then trichlorosilane active gas is introduced. The flow ratio of trichlorosilane to high-purity nitrogen is 1:5, and high-purity The flow rate of nitrogen is 1L / min;

[0039] (3) Raise the temperature from 50°C to 120°C at a rate of 0.25°C / min, and keep it at 120°C for 1 hour, then stop feeding the active gas;

[0040] (4) The temperature was raised from 120°C to 350°C at a rate of 1.0°C / min, and kept at 350°C for 2 hours, then heating was stopped and cooled to obtain infusible fibers.

[0041] The infusible f...

Embodiment 2

[0043] The present invention provides a kind of atmosphere non-melting method assisted by thermal crosslinking of nitride fiber, comprising the following steps:

[0044] (1) Place 100g polyborosilazane fiber sample in a non-melting atmosphere furnace, vacuumize and replace high-purity nitrogen, and repeat the operation three times;

[0045] (2) In a high-purity nitrogen atmosphere, the temperature is raised from room temperature to 50 °C at a rate of 10 °C / min, and then boron trichloride active gas is introduced. The flow ratio of boron trichloride and high-purity nitrogen is 1:10, The flow rate of high-purity nitrogen is 0.5L / min;

[0046] (3) Raise the temperature from 50°C to 100°C at a rate of 0.5°C / min, and keep it at 100°C for 1 hour, then stop feeding the active gas;

[0047] (4) Raise the temperature from 100°C to 300°C at a rate of 0.5°C / min, and keep it at 300°C for 2 hours, then stop heating and cool down to obtain infusible fibers.

[0048] The surface of the non...

Embodiment 3

[0050] The present invention provides a kind of atmosphere non-melting method assisted by thermal crosslinking of nitride fiber, comprising the following steps:

[0051] (1) 100g polysilazane fiber sample is placed in a non-melting atmosphere furnace, vacuumized and replaced with high-purity nitrogen, and repeat the operation four times;

[0052] (2) In a high-purity nitrogen atmosphere, the temperature is raised from room temperature to 60 °C at a rate of 5 °C / min, and then trichlorosilane active gas is introduced. The flow ratio of trichlorosilane to high-purity nitrogen is 1:1, and high-purity The flow rate of nitrogen is 2L / min;

[0053] (3) Raise the temperature from 50°C to 150°C at a rate of 1.0°C / min, and keep it at 150°C for 2 hours, then stop feeding the active gas;

[0054] (4) The temperature was raised from 150°C to 350°C at a rate of 2.0°C / min, and kept at 350°C for 1.5h, then the heating was stopped and cooled to obtain infusible fibers.

[0055] The surface o...

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Abstract

The invention discloses a nitride fiber thermal cross-linking assisted atmosphere non-melting method. The non-melting method comprises the following steps: (1) a nitride fibril sample is placed in a non-melting atmosphere furnace, and air is vacuumized and replaced with nitrogen; (2) the temperature in the non-melting atmosphere furnace increases from room temperature to 40-60 DEG C under a nitrogen atmosphere, then an active gas is introduced, and the flow ratio of the active gas to the nitrogen is (2:1)-(1:10); (3) the temperature in the non-melting atmosphere furnace is continuously raisedfrom 40 -60 DEG C to 100-150 DEG C, heat preservation is performed at 100-150 DEG C for 0.5-3 hours, and then the active gas introduction is stopped; (4) the temperature in the non-melting atmospherefurnace is continuously raised from 100-150 DEG C to 300-400 DEG C, heat preservation is performed at 300-400 DEG C for 0.5-2 hours, then, heating is terminated and cooling is performed to obtain non-molten fibers. Compared with a separate atmosphere non-melting cross-linking or thermal cross-linking method, the non-molten fibers obtained by the method provided by the invention are more uniform, and the cross-linking reaction degree is higher; and the process control, in comparison, is simpler and the production cost is lower.

Description

technical field [0001] The invention relates to the technical field of nitride fiber non-melting, in particular to an atmosphere non-melting method assisted by thermal crosslinking of nitride fiber. Background technique [0002] Nitride ceramic wave-transparent materials have the advantages of good high temperature stability, low high temperature ablation rate, low dielectric constant, small loss tangent and stable performance, and have great application prospects in the aerospace field. The continuous nitride ceramic fiber reinforced nitride ceramic wave-transparent composite material is one of the main research directions of high-temperature wave-transparent materials. This type of wave-transparent fiber mainly contains silicon nitride (Si 3 N 4 ) fiber, silicon boron nitrogen (carbon) (SiBN (C)) fiber and boron nitride (BN) fiber, etc. At present, the main method for preparing such nitride fibers is the polymer precursor conversion method, that is, firstly synthesize a ...

Claims

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Application Information

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IPC IPC(8): D01F9/08D01F11/00
CPCD01F9/08D01F11/00
Inventor 王兵邵长伟王军王浩王应德简科
Owner NAT UNIV OF DEFENSE TECH
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