Continuous silicon carbide fiber with beryllium gradient distribution and preparation method thereof
A technology of silicon carbide fiber and gradient distribution, applied in the direction of inorganic raw material artificial filament, etc., to achieve the effect of controllability and quality improvement
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Embodiment 1
[0036] Taking PSCS (molecular weight is 160) and beryllium acetylacetonate as raw materials, the mass proportion of the two (the proportioning described in the following examples is the mass proportion) is beryllium acetylacetonate:PSCS=10:100, 420°C of reaction temperature, The pyrolysis temperature was 500°C, and after holding the reaction for 6 hours, it was dissolved in xylene and filtered, and the filtrate was distilled under reduced pressure at 350°C for 30 minutes to obtain PBCS with a softening point of 195°C and a beryllium content of 1.31wt%. PBCS was added to the melt spinning device and degassed under the protection of high-purity nitrogen, at 258 ° C, 4 × 10 5 Under Pa pressure, carry out melt spinning with 300m / min speed, make the PBCS precursor that diameter is 20 μ m;
[0037] Put the above-mentioned fibers in a non-melting treatment device, pass through the air containing beryllium (the beryllium is provided by beryllium acetylacetonate); heat to 185°C at a he...
Embodiment 2
[0043] Using PCS (molecular weight 300) and beryllium as raw materials, beryllium: PCS = 5:100, the reaction temperature is 430 ° C, the cracking temperature is 490 ° C, and after the reaction time of 4 hours, it is dissolved and filtered in xylene, and the filtrate is dissolved at 350 ° C. ℃ for 1 hour under reduced pressure to obtain a softening point of 202 ℃, PBCS containing 0.61wt% beryllium; PBCS is added to the melt spinning device and degassed under the protection of high-purity nitrogen, at 268 ℃, 4.5 × 10 5 Under Pa pressure, carry out melt spinning with 350m / min speed, make the PBCS precursor that diameter is 18 μ m;
[0044] Infuse beryllium-containing air (the beryllium is provided by beryllium); heat up to 180°C at a rate of 10°C per hour, keep warm for 2 hours and cool to room temperature to obtain PBCS non-melting fibers. In the air containing beryllium, the molar ratio of Be to O is 0.2-0.8:1. During the non-melting process, the content of Be in the air gradua...
Embodiment 3
[0050] Using LPS (molecular weight of 150) and beryllium acetylacetonate as raw materials, beryllium acetylacetonate: LPS = 15:100, reaction temperature 400°C, cracking temperature 550°C, heat preservation reaction time 8h, dissolved in xylene, filtered, the filtrate at 340 °C for 1 hour under reduced pressure distillation to prepare PBCS with a softening point of 181 °C and a beryllium content of 1.53 wt%. PBCS was added to the melt spinning device and degassed under the protection of high-purity nitrogen, at 249 ° C, 4 × 10 5 Under Pa pressure, carry out melt spinning with 280m / min speed, make the PBCS precursor that diameter is 22 μm;
[0051] Infuse beryllium-containing air (the beryllium is provided by beryllium acetylacetonate); heat to 185°C at a rate of 10°C per hour, keep warm for 2 hours and cool to room temperature to obtain PBCS non-melting fibers. In the air containing beryllium, the molar ratio of Be to O is 0.5:1. Obtain PBCS non-melting fibers.
[0052] Put ...
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