Preparation method of C/C-SiC composite material

A composite material and curing treatment technology, which is applied in the field of C/C composite material preparation, can solve the problems of high equipment requirements, easy foaming, and high cost, and achieve the effects of reducing production costs, preventing damage, and improving performance

Inactive Publication Date: 2014-04-09
湖南中坚科技有限公司
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Problems solved by technology

[0003] The preparation process of C / C-SiC composite materials, including the formation of C / C preform and the addition of SiC phase, among them, the preparation method of C / C preform is mainly chemical deposition method (CVI) and polymer liquid The phase impregnation method (PIP), among which the CVI process is the most widely used, but its process is complicated, the production cycle is long, the efficiency is low, and the production cost remains high; and the PIP process, due to the cheap raw materials, simple process and short production cycle, therefore The cost is low, but during the process, it is easy to cause closed pores on the surface of the C / C preform, so that the subsequent SiC phase cannot be formed smoothly
The processes for forming SiC matrix phase mainly include CVI process, molten silicon infiltration (RMI) process and precursor impregnation cracking (PIP) process. Among them, CVI and PIP processes have the disadvantages of long preparation period and high production cost. Among them, PIP process Therefore, there are reasons for the long preparation cycle and high production cost: (1) The precursor used is polycarbosilane (PCS), and the preparation cost of PCS is high. The preparation of PCS requires two steps, first through dichlorodimethyl Polydimethylsilane is synthesized and then converted from polydimethylsilane at 800°C under high temperature and high pressure, which requires high equipment and complicated operation, so the cost is also high; (2) PCS is directly cracked at 1250°C and is easy to foam , the porosity of the obtained composite material reaches 80%. In order to reduce the porosity, the cracking time can only be prolonged. Therefore, this process not only requires a long cracking cycle, but also has extremely difficult control problems.
Although the cost of the RMI process is low, the damage to the fiber is large during the preparation process, which affects the performance of the composite material

Method used

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  • Preparation method of C/C-SiC composite material
  • Preparation method of C/C-SiC composite material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] step one

[0038] Set the density to 0.42g / cm 3 The carbon felt is placed in a vacuum high-pressure impregnator, and the impregnating agent is firstly vacuum impregnated under the condition of ≤0.001MPa for 1 hour, then pressure impregnated under 2MPa for 2 hours, and then cured and carbonized under the protection of nitrogen , the impregnating agent used includes by mass parts: 10 parts of thermoplastic phenolic resin, 1 part of hexamethylenetetramine, and 110 parts of ethanol; the temperature of the curing treatment is 200 ° C, and the curing time is 6 hours; the carbonization treatment The temperature is 800°C, and the carbonization treatment time is 1.5h; this step is used to form a thin and dense C coating to protect the carbon fibers.

[0039] step two

[0040] Repeat vacuum high pressure impregnation, curing treatment and carbonization treatment 3 times to obtain a density of 1.22g / cm 3 The C / C porous prefabricated body; when vacuum high-pressure impregnation ...

Embodiment 2

[0045] step one

[0046] Set the density to 0.48g / cm 3 The carbon felt is placed in a vacuum high-pressure impregnator, and the impregnating agent is firstly vacuum impregnated under the condition of ≤0.001MPa for 1.5h, then pressure impregnated under 2.5MPa for 3h, and then under the protection of nitrogen, the curing treatment and For carbonization treatment, the impregnating agent used includes in parts by mass: 10 parts of thermoplastic phenolic resin, 0.6 parts of hexamethylenetetramine, and 106 parts of ethanol; the temperature of the curing treatment is 400°C, and the curing time is 8h; The temperature of the carbonization treatment is 900°C, and the time of the carbonization treatment is 1.5h; this step is used to form a thin and dense C coating to protect the carbon fibers.

[0047] step two

[0048] Repeat vacuum high-pressure impregnation, curing treatment, and carbonization treatment 3 times to obtain a density of 1.26g / cm 3 The C / C porous prefabricated body; wh...

Embodiment 3

[0052] step one

[0053] Set the density to 0.54g / cm 3 The carbon felt is placed in a vacuum high-pressure impregnator, and the impregnating agent is firstly vacuum impregnated under the condition of ≤0.001MPa for 1.5h, and then pressure impregnated under 3MPa for 3h, and then solidified and carbonized under the protection of nitrogen For the treatment, the impregnating agent used includes in parts by mass: 10 parts of thermoplastic phenolic resin, 0.8 parts of hexamethylenetetramine, and 110 parts of ethanol; the temperature of the curing treatment is 300°C, and the curing time is 10 hours; the carbonization The treatment temperature is 1000°C, and the carbonization treatment time is 2 hours; this step is used to form a thin and dense C coating to protect the carbon fibers.

[0054] step two

[0055] Repeat vacuum high pressure impregnation, curing treatment and carbonization treatment 3 times to obtain a density of 1.30g / cm 3 The C / C porous prefabricated body; when vacuum...

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Abstract

The invention discloses a preparation method of a C / C-SiC composite material, and belongs to the technical field of preparation of C / C composite materials. The method comprises the following steps: putting a carbon felt of which the density is 0.4-0.55g / cm<3> into an impregnant to steep under a protective atmosphere; carrying out curing treatment and carbonization treatment; repeating vacuum impregnation, pressure impregnation, curing treatment and carbonization treatment and putting the obtained preform into a polyaniline methyl silane solution to steep after a C / C porous preform of which the density is 1.2-1.3g / cm<3> is obtained; carrying out curing treatment; repeating the steeping and curing technologies for 2-3 times, and then cracking under the protective atmosphere; and repeating the steeping, curing and cracking technologies until the C / C-SiC composite material of which the density is 1.9-2.1g / cm<3> is obtained according to the system of cracking once after steeping and curing for 2-3 times. The preparation method is short in preparation cycle, and low in cost, and the obtained C / C-SiC composite material is excellent in performance, and convenient to achieve industrial production.

Description

technical field [0001] The invention discloses a preparation method of a C / C-SiC composite material, which belongs to the technical field of C / C composite material preparation. Background technique [0002] C / C-SiC composite material has low density, good thermal conductivity, good oxidation resistance, high and stable friction coefficient, strong wear resistance, and excellent mechanical properties. It is a kind of material that can be used normally at 1650 °C A new type of high-temperature structural material, and because its friction performance is not affected by weather changes, it is also a friction material with broad development prospects. [0003] The preparation process of C / C-SiC composite materials, including the formation of C / C preform and the addition of SiC phase, among them, the preparation method of C / C preform is mainly chemical deposition method (CVI) and polymer liquid The phase impregnation method (PIP), among which the CVI process is the most widely u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/83C04B35/565C04B35/80C04B35/622
Inventor 李效东熊伟钟丹陈林涛
Owner 湖南中坚科技有限公司
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