Preparation method for aluminum-containing continuous silicon nitride fibers

A technology of silicon nitride fibers and polycarbosilane fibers, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of reducing the mechanical strength and quality loss of fibers, and achieve the effects of low cost, simple preparation process and equipment

Inactive Publication Date: 2015-10-21
SUZHOU IND PARK HIGH PERFORMANCE CERAMIC FIBER ENG CENT CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Under the protection of nitrogen, its operating temperature can reach up to 1600°C, but in an aerobic environment, B and O 2 The reaction produces B 2 o 3 , when T>1500℃, B 2 o 3 Volatilization leads to mass loss and the formation of holes, which greatly reduces the mechanical strength of the fiber. Obviously, this is not good for the use of silicon nitride fibers in high temperature environments.

Method used

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  • Preparation method for aluminum-containing continuous silicon nitride fibers
  • Preparation method for aluminum-containing continuous silicon nitride fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The polyaluminocarbosilane fiber is treated at 180°C where the air does not melt, and the non-melting aluminum-containing polycarbosilane fiber with a non-melting degree of 65% can be obtained. Place aluminum-containing non-melting polycarbosilane fibers in a high-temperature sintering furnace, feed pure nitrogen, and raise the temperature at a rate of 270°C / h, with a nitrogen flow rate of 10L / min. Start at 200°C, feed ammonia gas, raise the temperature to 800°C at a rate of 120°C / min, keep warm for 1h, and the flow rate of ammonia gas is 5L / min. Then, under the protection of high-purity nitrogen, the temperature continues to rise at a rate of 300°C / min, and the firing is completed at 1500°C under high-temperature conditions, and the flow rate of nitrogen is 15L / min. From figure 1 It can be seen from the figure that the obtained Si-Al-N-O fiber has a diameter of 12.3um, a strength of 1.40GPa, an aluminum content of 0.9%, and a strength retention rate of 65% after being...

Embodiment 2

[0021] The aluminum-containing non-melting polycarbosilane fiber prepared according to the method of Example 1 was placed in a high-temperature sintering furnace, and nitrogen gas was introduced, and the temperature was raised at a rate of 250° C. / h, and the flow rate of nitrogen gas was 10 L / min. Start at 300°C, feed the mixed gas of ammonia and nitrogen, raise the temperature to 800°C at a rate of 150°C / min, keep warm for 2h, the volume concentration of ammonia gas is 50%, and the flow rate is 8L / min. Then under the protection of high-purity nitrogen, continue to heat up at a rate of 300°C / min, and complete the firing under high temperature conditions at 1450°C. The nitrogen flow rate is 20L / min, and the obtained Si-Al-N-O fiber has a diameter of 11.9um and a strength of 1.44GPa, the aluminum content is 0.7%, and the strength retention rate is 69% after being treated in air at 1500°C for 1 hour.

Embodiment 3

[0023] The aluminum-containing non-melting polycarbosilane fiber prepared according to the method of Example 1 was placed in a high-temperature sintering furnace, fed with nitrogen, and the temperature was raised at a rate of 300° C. / h, and the nitrogen flow rate was 10 L / min. Start at 400°C, feed the mixed gas of ammonia and argon, raise the temperature to 800°C at a rate of 100°C / min, keep warm for 1.5h, the volume concentration of ammonia gas is 30%, and the flow rate is 5L / min. Then under the protection of high-purity nitrogen, continue to heat up at a rate of 300°C / min, and complete the firing under high-temperature conditions at 1400°C. The nitrogen flow rate is 15L / min, and the obtained Si-Al-N-O fiber has a diameter of 11.5um and a strength of 1.53GPa, the aluminum content is 0.8%, and the strength retention rate is 51% after being treated in air at 1500°C for 1 hour.

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Abstract

The invention discloses a preparation method for aluminum-containing continuous silicon nitride fibers. The method includes the steps that 1, air curing treatment is performed on aluminum-containing polycarbosilane fibers; 2, nitrogenization is performed on the aluminum-containing infusible polycarbosilane fibers under the atmosphere of pure ammonia gas or a nixed atmosphere of ammonia gas, nitrogen gas and argon gas; 3, high-temperature sintering is performed under the atmosphere of nitrogen gas or argon gas. The aluminum-containing continuous silicon nitride fibers prepared through the method solve the problem that B2O3 volatilization happens on B-containing continuous silicon nitride fibers at the temperature above 1500 DEG C in an aerobic environment, holes are formed, and consequently the strength of the fibers is sharply reduced; compared with a precursor method, the problems that materials are not resistant to water and air and prone to decomposition are solved, and the aluminum-containing continuous silicon nitride fibers have better high temperature resistance and high-temperature oxidation resistance; in addition, the preparation process and equipment are simple, the cost is low, and industrial volume production is easy to achieve.

Description

technical field [0001] The invention relates to a method for preparing aluminum-containing continuous silicon nitride fiber, which belongs to the technical field of high-tech material preparation. Background technique [0002] As a high-performance fiber, silicon nitride fiber has excellent properties such as high strength, high toughness, high thermal conductivity, corrosion resistance, thermal shock resistance, oxidation resistance, low thermal expansion coefficient, and low density. It is used in aviation, aerospace and automotive engines, etc. field has received widespread attention. Similar to silicon carbide fiber, the introduction of other elements into silicon nitride fiber can further significantly improve its temperature resistance and high temperature oxidation resistance, among which B element has been studied more and more deeply. [0003] Introducing a small amount of B into silicon nitride fibers can significantly increase the crystallization temperature of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10
Inventor 冯春祥马小民董伯举陈虎田西锋李凯娜
Owner SUZHOU IND PARK HIGH PERFORMANCE CERAMIC FIBER ENG CENT CO LTD
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