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Polycarbosilane Fiber Low Oxygen Non-melting Method

A polycarbosilane fiber and fiber technology, which is applied in the field of high-performance ceramic fiber preparation, can solve the problems of poor uniformity of infusibility of polycarbosilane fibers, affecting the high temperature resistance and oxidation resistance of silicon carbide fibers, and increasing fiber manufacturing costs. , to achieve the effect of facilitating batch preparation, increasing fiber cost and increasing equipment cost

Active Publication Date: 2017-04-26
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the air non-melting method is the simplest and cheapest method, but at the same time, a large amount of oxygen is introduced, which seriously affects the high temperature resistance and oxidation resistance of silicon carbide fibers; the ultraviolet light non-melting method must require UV-active groups in polycarbosilane, It is not suitable for conventional polycarbosilane; electron beam irradiation non-melting method and ray non-melting method require expensive electron beam generating equipment and ray generating equipment, which greatly increases the cost of fiber manufacturing
Chemical vapor phase non-melting is achieved through gas-solid reaction. On the one hand, the softening point of polycarbosilane raw materials is required to be higher than 250°C. On the other hand, the non-melting degree and uniformity of polycarbosilane fibers are very large. It depends on the distribution of airflow field and temperature field. At different positions of polycarbosilane fibers, the atmosphere concentration and temperature are very different, which often results in poor uniformity of non-melting degree of polycarbosilane fibers.

Method used

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  • Polycarbosilane Fiber Low Oxygen Non-melting Method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Winding polycarbosilane fiber precursors onto polycarbosilane fiber precursor cylinders, winding 4 cylinders in total, and the weight of each cylinder of precursor filaments is 100 g. The raw silk cylinder adopts a stainless steel mesh cylinder with a diameter of 250mm, a length of 400mm, and a mesh size of 1cm; (2) The polycarbosilane fiber precursor is placed in an oven with an air inlet and outlet system and a blast system. The way to place polycarbosilane fiber precursors is to put 4 precursor tubes on 4 stainless steel rods with a length of 1000mm and a port of 20×20mm respectively, place two tubes on each rod, and then place the two ends of the stainless steel rods on the (3) Turn on the blast system, raise the temperature to 130°C at a rate of 180°C / h, and keep the temperature constant for 1 hour to remove the adsorbed water in the fiber; (4) Raise the temperature to 175°C at a rate of 30°C / h , constant temperature 2h; (5) pass into nitrogen in blast oven, ni...

Embodiment 2

[0033] (1) Winding polycarbosilane fiber precursors onto polycarbosilane fiber precursor cylinders, winding 4 cylinders in total, and the weight of each cylinder of precursor filaments is 200 g. The raw silk cylinder adopts a stainless steel mesh cylinder with a diameter of 300mm, a length of 350mm, and a mesh size of 1cm; (2) The polycarbosilane fiber precursor is placed in an oven with an air inlet and outlet system and a blast system. The way to place polycarbosilane fiber precursors is to put 4 precursor tubes on 4 stainless steel rods with a length of 1000mm and a port of 20×20mm respectively, place two tubes on each rod, and then place the two ends of the stainless steel rods on the (3) Turn on the blower system, raise the temperature to 130°C at a rate of 150°C / h, and keep the temperature constant for 1 hour to remove the adsorbed water in the fiber; (4) Raise the temperature to 175°C at a rate of 30°C / h , constant temperature for 2h; (5) feed nitrogen into the blast ov...

Embodiment 3

[0035] (1) Winding polycarbosilane fiber precursors onto polycarbosilane fiber precursor cylinders, winding 4 cylinders in total, and the weight of each cylinder of precursor filaments is 200 g. The raw silk cylinder adopts a stainless steel mesh cylinder with a diameter of 350mm, a length of 350mm, and a mesh size of 1cm; (2) The polycarbosilane fiber precursor is placed in an oven with an air inlet and outlet system and a blast system. The way to place polycarbosilane fiber precursors is to put 4 precursor tubes on 4 stainless steel rods with a length of 1000mm and a port of 20×20mm respectively, place two tubes on each rod, and then place the two ends of the stainless steel rods on the (3) Turn on the blower system, raise the temperature to 140°C at a rate of 150°C / h, and keep the temperature constant for 2 hours to remove the adsorbed water in the fiber; (4) Heat up to 180°C at a rate of 20°C / h , constant temperature for 3h; (5) feed nitrogen into the blast oven, nitrogen ...

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Abstract

The invention relates to a polycarbosilane fiber low-oxygen non-melting method which comprises the following steps: winding a raw polycarbosilane fiber on a raw polycarbosilane fiber cylinder, putting in a drying oven provided with a gas inlet / outlet system and a blast system, heating to 130-140 DEG C at the rate of 120-180 DEG C / hour, keeping the temperature for 1-2 hours, removing the adsorbed moisture, heating to 175-180 DEG C at the rate of 10-30 DEG C / hour, and keeping the temperature for 2-3 hours; introducing nitrogen into the blast drying oven while continuing heating to 195-210 DEG C at the rate of 5-10 DEG C / hour, and keeping the temperature for 1-2 hours; and stopping heating, and naturally cooling to obtain the low-oxygen polycarbosilane non-molten fiber. The high-linearity polycarbosilane with lower softening point can be adopted, so the raw fiber has high quality. The non-melting technique is simple to control and lower in cost, and can perform mass production of the low-oxygen polycarbosilane non-molten fiber.

Description

technical field [0001] The invention belongs to the field of preparation of high-performance ceramic fibers, and in particular relates to a low-oxygen non-melting method for polycarbosilane fibers. Background technique [0002] Polycarbosilane fiber is an organic polymer fiber prepared from polycarbosilane by melt spinning, and it is also the precursor for preparing silicon carbide ceramic fiber. In order to avoid the melting of the raw silk during the inorganicization process, it must be cross-linked to form a three-dimensional network structure before the raw silk is melted, and this process is non-melting. The polycarbosilane fiber can keep the shape of the fiber during the process of inorganicization at high temperature after being infused. The non-melting method of polycarbosilane plays an extremely important role in the composition, structure and properties of SiC fibers. [0003] At present, polycarbosilane fiber non-melting methods include air non-melting method, u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M11/58D06M101/30
Inventor 简科王军王浩宋永才邵长伟王小宙苟燕子
Owner NAT UNIV OF DEFENSE TECH