CN105622142A - Preparation method of ethanol dispersed vanadium boride silicon carbide-carbon fiber friction material - Google Patents

Preparation method of ethanol dispersed vanadium boride silicon carbide-carbon fiber friction material Download PDF

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CN105622142A
CN105622142A CN201610014326.9A CN201610014326A CN105622142A CN 105622142 A CN105622142 A CN 105622142A CN 201610014326 A CN201610014326 A CN 201610014326A CN 105622142 A CN105622142 A CN 105622142A
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carbon fiber
vanadium boride
silicon
siliconising
fiber blanket
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CN105622142B (en
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唐竹兴
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Shandong University of Technology
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Abstract

The invention provides a preparation method of an ethanol dispersed vanadium boride silicon carbide-carbon fiber friction material. The preparation method is characterized in that graphited carbon fiber blanket with the density being 0.1 to 1.8g/cm<3> is subjected to carburizing treatment; then, ethanol dispersed vanadium boride filling treatment is performed; next, silicon carbide deposition treatment is performed; then, embedding siliconing treatment is performed; next, nitridation treatment is performed in nitrogen atmosphere to obtain the ethanol dispersed vanadium boride silicon carbide-carbon fiber friction material. The graphited carbon fiber blanket is used; the friction material preparation is realized through the steps of carburization, vanadium boride filling, silicon carbide deposition, embedding siliconing, nitridation and the like; the prepared friction material has high intensity, high toughness and high friction performance, and belongs to a friction material adapting to various climate conditions.

Description

The preparation method of ethanol dispersion vanadium boride silicon carbide?carbon fiber friction material
Technical field
The preparation method that the present invention relates to the friction material of a kind of carbon fiber and ceramic material compound, belongs to technical field of composite preparation.
Background technology
What friction material currently mainly adopted is carbon fiber and carbon (C/C) composite, owing to the anti-wear performance of C/C composite is relatively low, and the preparation method that people are seeking the higher friction material of anti-wear performance. It addition, C/C composite is in a humid environment, its frictional behaviour can reduce, and brings serious potential safety hazard to using.
Summary of the invention
It is an object of the invention to provide and a kind of can overcome drawbacks described above, realize preparation higher intensity, higher frictional behaviour and adapt to the preparation method of friction material of various weather conditions. Its technical scheme is:
The preparation method of ethanol dispersion vanadium boride silicon carbide?carbon fiber friction material, it is characterised in that be 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket carries out ethanol dispersion vanadium boride filling and processes after carrying out Carburization Treatment, it is deposited carborundum again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares ethanol dispersion vanadium boride silicon carbide?carbon fiber friction material, specifically comprises the following steps that
(1) it is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing gas of propane flammable gas and nitrogen at 900 ~ 1100 DEG C of temperature, propane flammable gas: the mol ratio of nitrogen is 1:4 ~ 6, and flow-control is at 50 ~ 600ml/min, and Carburization Treatment obtains carburizing carbon fiber blanket in 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is immersed in the ethanol slurry that granularity is 5 ~ 20% vanadium borides less than 0.3 ��m of content, be placed in ultrasonic cleaner to fill vanadium boride and process 30 ~ 50 minutes and take out dried preparing and fill vanadium boride carbon fiber blanket;
(3) above-mentioned filling vanadium boride carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixing gas of trichloromethyl silane gas, hydrogen and argon, depositing silicon silicon processes 10 ~ 24 hours and obtains depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl silane gas: hydrogen: the mol ratio of argon is 1:3 ~ 5:3 ~ 5, flow is 50 ~ 600ml/min;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum is imbedded in siliconising material, under vacuum atmosphere, at the temperature of 1500 ~ 1800 DEG C, siliconising processes 3 ~ 5 hours prepared siliconising carbon fiber blankets, wherein, siliconising material is silica flour 30 ~ 50% and the polyvinyl alcohol water solution Homogeneous phase mixing that additional 5 ~ 15% concentration of mixture are 0.2 ~ 0.6% that diameter is 0.5 ~ 3mm carbon granule 50 ~ 70% prepares after drying;
(5) by above-mentioned siliconising carbon fiber blanket 10 ~ 24 hours prepared ethanol dispersion vanadium boride silicon carbide?carbon fiber friction materials of nitrogen treatment at the temperature of 1350 ~ 1700 DEG C.
Compared with prior art, its advantage is the present invention:
1, the carbon fiber blanket that the present invention uses is graphited carbon fiber blanket, or graphited needled carbon tapetum fibrosum, or graphited weaving carbon fiber cloth, or graphited 3 D weaving carbon fiber knits block;
2, friction material prepared by the present invention is by graphited carbon fiber and carborundum, vanadium boride, a kind of high intensity of silicon nitride compound, high frictional behaviour, the friction material that adapts under various weather conditions;
3, by carburizing, fill vanadium boride, depositing silicon silicon, embedment siliconising and the step such as nitrogenize and realize the preparation of friction material, carburizing and two steps of depositing silicon silicon be in order to protect carbon fiber surface not to be damaged and carbon fiber surface give carbon coating and coat of silicon carbide, because coat of silicon carbide can stop the infiltration of silicon steam in the process of siliconising, coat of silicon carbide is once seepage, carbide coatings and silicon steam reaction generate carborundum and stop silicon steam further, thus protecting carbon fiber surface not to be damaged;
4, carbon fiber blanket has the significantly high porosity, depend merely on carburizing and depositing silicon silicon may require that and is lot more time to reach densification, manufacturing cost is significantly high, the space adopting the method filling carbon fiber blanket filling vanadium boride and embedment siliconising will be very convenient, time saving and energy saving, fill vanadium boride simultaneously and can improve the anti-wear performance of friction material further;
5, the present invention utilizes the pliability of carburizing carbon fiber, microvesicle is produced by hyperacoustic ethanol slurry that acts on, when acoustic pressure or the sound intensity arrive to a certain degree, microvesicle will expand rapidly, then closing suddenly again, the moment of microvesicle Guan Bi produces shock wave, makes to produce around microvesicle the pressure of about 1012pa, force vanadium boride granule to be filled in the space of carbon fiber blanket, reach the purpose of calking;
6, the dispersion vanadium boride filling of ethanol slurry is adopted to process, it is possible to being effectively improved vanadium boride granule suspendability, improve charging efficiency, vanadium boride granule is firmly combined together by the silicon nitride formed in nitrogen treatment process;
7, due to penetrate into metallic silicon fusing point relatively low be about 1420 DEG C, the temperature of friction material work surface is instantaneous up to nearly 2000 DEG C, metallic silicon is nitrogenized generation silicon nitride, form the friction material of microcellular structure, the tolerable temperature of friction material work surface can be increased substantially, improve the service life of friction material.
Detailed description of the invention
Embodiment 1
(1) it is 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing gas of propane flammable gas and nitrogen at 900 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:4, flow-control is at 50ml/min, and Carburization Treatment obtains carburizing carbon fiber blanket in 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is immersed in the ethanol slurry that granularity is 5% vanadium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill vanadium boride process 50 minutes, take out dried preparing and fill vanadium boride carbon fiber blanket;
(3) above-mentioned filling vanadium boride carbon fiber blanket is passed at 900 DEG C of temperature the mixing gas of trichloromethyl silane gas, hydrogen and argon, trichloromethyl silane gas: hydrogen: the mol ratio of argon is 1:5:5, flow-control is at 50ml/min, and depositing silicon silicon processes 24 hours and obtains depositing silicon silicon-carbon tapetum fibrosum;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum is imbedded in siliconising material, 5 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1500 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 30% and diameter to be additional 5% concentration of 0.5mm carbon granule 70% be 0.2% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 10 hours prepared vanadium boride silicon carbide?carbon fiber friction materials of nitrogen treatment at the temperature of 1700 DEG C.
Embodiment 2
(1) it is 0.8g/cm by density3Graphited carbon fiber blanket passes into the mixing gas of propane flammable gas and nitrogen at 1000 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:5, flow-control is at 350ml/min, and Carburization Treatment obtains carburizing carbon fiber blanket in 18 hours;
(2) above-mentioned carburizing carbon fiber blanket is immersed in the ethanol slurry that granularity is 12% vanadium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill vanadium boride process 40 minutes, take out dried preparing and fill vanadium boride carbon fiber blanket;
(3) above-mentioned filling vanadium boride carbon fiber blanket is passed at 1000 DEG C of temperature the mixing gas of trichloromethyl silane gas, hydrogen and argon, trichloromethyl silane gas: hydrogen: the mol ratio of argon is 1:4:4, flow-control is at 350ml/min, and depositing silicon silicon processes 18 hours and obtains depositing silicon silicon-carbon tapetum fibrosum;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum is imbedded in siliconising material, 4 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1650 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 40% and diameter to be additional 10% concentration of 2mm carbon granule 60% be 0.4% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 18 hours prepared vanadium boride silicon carbide?carbon fiber friction materials of nitrogen treatment at the temperature of 1550 DEG C.
Embodiment 3
(1) it is 0.1g/cm by density3Graphited carbon fiber blanket passes into the mixing gas of propane flammable gas and nitrogen at 1100 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:6, flow-control is at 600ml/min, and Carburization Treatment obtains carburizing carbon fiber blanket in 10 hours;
(2) above-mentioned carburizing carbon fiber blanket is immersed in the ethanol slurry that granularity is 20% vanadium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill vanadium boride process 30 minutes, take out dried preparing and fill vanadium boride carbon fiber blanket;
(3) above-mentioned filling vanadium boride carbon fiber blanket is passed at 1100 DEG C of temperature the mixing gas of trichloromethyl silane gas, hydrogen and argon, trichloromethyl silane gas: hydrogen: the mol ratio of argon is 1:3:3, flow-control is at 600ml/min, and depositing silicon silicon processes 10 hours and obtains depositing silicon silicon-carbon tapetum fibrosum;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum is imbedded in siliconising material, 3 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1800 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 50% and diameter to be additional 15% concentration of 3mm carbon granule 50% be 0.6% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 24 hours prepared vanadium boride silicon carbide?carbon fiber friction materials of nitrogen treatment at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of ethanol dispersion vanadium boride silicon carbide?carbon fiber friction material, it is characterised in that be 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket carries out ethanol dispersion vanadium boride filling and processes after carrying out Carburization Treatment, it is deposited carborundum again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares ethanol dispersion vanadium boride silicon carbide?carbon fiber friction material, specifically comprises the following steps that
(1) it is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing gas of propane flammable gas and nitrogen at 900 ~ 1100 DEG C of temperature, propane flammable gas: the mol ratio of nitrogen is 1:4 ~ 6, and flow-control is at 50 ~ 600ml/min, and Carburization Treatment obtains carburizing carbon fiber blanket in 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is immersed in the ethanol slurry that granularity is 5 ~ 20% vanadium borides less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill vanadium boride process 30 ~ 50 minutes, take out dried preparing and fill vanadium boride carbon fiber blanket;
(3) above-mentioned filling vanadium boride carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixing gas of trichloromethyl silane gas, hydrogen and argon, depositing silicon silicon processes 10 ~ 24 hours and obtains depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl silane gas: hydrogen: the mol ratio of argon is 1:3 ~ 5:3 ~ 5, flow is 50 ~ 600ml/min;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum is imbedded in siliconising material, under vacuum atmosphere, at the temperature of 1500 ~ 1800 DEG C, siliconising processes 3 ~ 5 hours prepared siliconising carbon fiber blankets, wherein, siliconising material is silica flour 30 ~ 50% and the polyvinyl alcohol water solution Homogeneous phase mixing that additional 5 ~ 15% concentration of mixture are 0.2 ~ 0.6% that diameter is 0.5 ~ 3mm carbon granule 50 ~ 70% prepares after drying;
(5) by above-mentioned siliconising carbon fiber blanket 10 ~ 24 hours prepared ethanol dispersion vanadium boride silicon carbide?carbon fiber friction materials of nitrogen treatment at the temperature of 1350 ~ 1700 DEG C.
CN201610014326.9A 2016-01-11 2016-01-11 Ethyl alcohol disperses the preparation method of vanadium boride silicon carbide―carbon fiber friction material Expired - Fee Related CN105622142B (en)

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CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN103342570A (en) * 2013-07-11 2013-10-09 山东宝纳新材料有限公司 Method for preparing C/SiC composite material through low-cost fused silicon impregnation method
CN103724035A (en) * 2013-07-23 2014-04-16 太仓派欧技术咨询服务有限公司 Densification method for carbon fiber reinforced silicon carbonitride ceramic composite material

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