CN105481433B - Ethanol disperses the preparation method of zirconium boride carborundum carbon fiber friction material - Google Patents

Ethanol disperses the preparation method of zirconium boride carborundum carbon fiber friction material Download PDF

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CN105481433B
CN105481433B CN201610014320.1A CN201610014320A CN105481433B CN 105481433 B CN105481433 B CN 105481433B CN 201610014320 A CN201610014320 A CN 201610014320A CN 105481433 B CN105481433 B CN 105481433B
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carbon fiber
zirconium boride
silicon
friction material
ethanol
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CN105481433A (en
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唐竹兴
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Shandong University of Technology
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Abstract

Ethanol disperses the preparation method of zirconium boride carborundum carbon fiber friction material, it is characterised in that by density is 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out the scattered zirconium boride filling processing of ethanol after carrying out Carburization Treatment, depositing silicon silicon processing is carried out again, carry out being embedded to siliconising processing again, then the scattered zirconium boride carborundum carbon fiber friction material of ethanol is made in nitrogen treatment in nitrogen atmosphere.The present invention is to realize the preparation of friction material by carburizing, filling zirconium boride, depositing silicon silicon, the embedment step such as siliconising and nitridation using graphitized carbon fibre blanket, prepared friction material high intensity, high tenacity, high frictional behaviour, are the friction materials for adapting to various weather conditions.

Description

Ethanol disperses the preparation method of zirconium boride silicon carbide―carbon fiber friction material
Technical field
The present invention relates to a kind of preparation method of the compound friction material of carbon fiber and ceramic material, belong to composite system Standby technical field.
Background technology
Friction material is at present mainly using carbon fiber and carbon（C/C）Composite is wear-resisting due to C/C composites Performance is relatively low, and people are seeking the preparation method of the higher friction material of anti-wear performance.In addition, C/C composites exist In moist environment, its frictional behaviour can be reduced, and serious potential safety hazard is brought to using.
The content of the invention
It can overcome drawbacks described above it is an object of the invention to provide one kind, realize preparation higher intensity, higher frictional behaviour And adapt to the preparation method of the friction material of various weather conditions.Its technical scheme is：
Ethanol disperses the preparation method of zirconium boride silicon carbide―carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out the scattered zirconium boride filling processing of ethanol after carrying out Carburization Treatment, then carries out deposition carbon SiClx processing, then carry out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made ethanol disperse zirconium boride carborundum- Carbon fiber friction material, comprise the following steps that：
（1）It is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket be passed through at a temperature of 900 ~ 1100 DEG C propane flammable gas and The mixed gas of nitrogen, propane flammable gas:The mol ratio of nitrogen is 1:4 ~ 6, flow control in 50 ~ 600ml/min, Carburization Treatment 10 ~ Obtain carburizing carbon fiber blanket within 24 hours；
（2）Above-mentioned carburizing carbon fiber blanket is immersed into granularity to be less than in the ethanol slurry that 0.3 μm of content is 5 ~ 20% zirconium borides, It is placed in ultrasonic cleaner to fill after zirconium boride processing taking-up in 30 ~ 50 minutes is dried and filling zirconium boride carbon fiber blanket is made；
（3）Above-mentioned filling zirconium boride carbon fiber blanket is passed through trichloromethyl silane gas, hydrogen at a temperature of 900 ~ 1100 DEG C With the mixed gas of argon gas, depositing silicon silicon handles 10 ~ 24 hours and obtains depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl Silane gas:Hydrogen:The mol ratio of argon gas is 1:3~5:3 ~ 5, flow is 50 ~ 600ml/min；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, 1500 ~ 1800 DEG C of the temperature under vacuum atmosphere Lower siliconising handles 3 ~ 5 hours obtained siliconising carbon fiber blankets, wherein, siliconising material is silica flour 30 ~ 50% and a diameter of 0.5 ~ 3mm carbon granules It is made after the uniform combination drying of polyvinyl alcohol water solution that 50 ~ 70% additional 5 ~ 15% concentration of mixture is 0.2 ~ 0.6%；
（5）By above-mentioned siliconising carbon fiber blanket, 10 ~ 24 hours obtained ethanol of nitrogen treatment divides at a temperature of 1350 ~ 1700 DEG C Dissipate zirconium boride silicon carbide―carbon fiber friction material.
Compared with prior art, its advantage is the present invention：
1st, the carbon fiber blanket that uses of the present invention is graphited carbon fiber blanket, or graphited needled carbon tapetum fibrosum, or stone The weaving carbon fiber cloth of inkization, or graphited 3 D weaving carbon fiber knit block；
2nd, friction material prepared by the present invention is compound by graphited carbon fiber and carborundum, zirconium boride, silicon nitride A kind of friction material under high intensity, high frictional behaviour, the various weather conditions of adaptation；
3rd, the system of friction material is realized by carburizing, filling zirconium boride, depositing silicon silicon, the embedment step such as siliconising and nitridation It is standby, two steps of carburizing and depositing silicon silicon be in order to protect carbon fiber surface not to be damaged and carbon fiber surface assign charcoal Coating and coat of silicon carbide, because coat of silicon carbide can stop the infiltration of silicon steam, coat of silicon carbide one during siliconising Denier seepage, carbide coatings and silicon steam reaction generation carborundum further stop silicon steam, so as to protect carbon fiber surface not by Destroy；
4th, carbon fiber blanket has the very high porosity, depends merely on carburizing and depositing silicon silicon may require that and be lot more time to reach Densification, manufacturing cost is very high, will be very using the space of filling zirconium boride and the method filling carbon fiber blanket for being embedded to siliconising It is convenient, it is time saving and energy saving, while fill zirconium boride and can further improve the anti-wear performance of friction material；
5th, the present invention utilizes the pliability of carburizing carbon fiber, and microvesicle is produced by the ethanol slurry that acts on of ultrasonic wave, when When acoustic pressure or the sound intensity are reached to a certain degree, microvesicle will expand rapidly, and then closure, the moment of microvesicle closure produce suddenly again Shock wave, make the pressure that about 1012pa is produced around microvesicle, zirconium boride particle is forced to be filled into the space of carbon fiber blanket, reached To the purpose of calking；
6th, zirconium boride filling processing is disperseed using ethanol slurry, zirconium boride particle suspendability can be effectively improved, improved Zirconium boride particle is firmly combined together by charging efficiency, the silicon nitride formed during nitrogen treatment；
7th, it is 1420 DEG C or so because the metallic silicon fusing point of infiltration is relatively low, the temperature of friction material working face is instantaneously up near 2000 DEG C, metallic silicon is nitrogenized into generation silicon nitride, the friction material of microcellular structure is formed, friction material work can be increased substantially Make the tolerable temperature in face, improve the service life of friction material.
Embodiment
Embodiment 1
（1）It is 1.8g/cm by density3Graphited carbon fiber blanket is passed through the mixed of propane flammable gas and nitrogen at a temperature of 900 DEG C Close gas, propane flammable gas:The mol ratio of nitrogen is 1:4, flow control obtains carburizing carbon in 24 hours in 50ml/min, Carburization Treatment Tapetum fibrosum；
（2）Above-mentioned carburizing carbon fiber blanket is immersed into granularity and is less than 0.3 μm of content in the ethanol slurry of 5% zirconium boride, to be placed in Zirconium boride is filled in ultrasonic cleaner to handle 50 minutes, takes out and filling zirconium boride carbon fiber blanket is made after drying；
（3）Above-mentioned filling zirconium boride carbon fiber blanket is passed through trichloromethyl silane gas, hydrogen and argon gas at a temperature of 900 DEG C Mixed gas, trichloromethyl silane gas:Hydrogen:The mol ratio of argon gas is 1:5:5, flow control is in 50ml/min, deposition carbon SiClx handles 24 hours and obtains depositing silicon silicon-carbon tapetum fibrosum；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, oozed under vacuum atmosphere at a temperature of 1500 DEG C 5 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is silica flour 30% and additional 5% concentration of a diameter of 0.5mm carbon granules 70% is 0.2% polyvinyl alcohol water solution is dried after uniformly mixing and is made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1700 DEG C 10 hours obtained zirconium boride carborundum of nitrogen treatment- Carbon fiber friction material.
Embodiment 2
（1）It is 0.8g/cm by density3Graphited carbon fiber blanket is passed through the mixed of propane flammable gas and nitrogen at a temperature of 1000 DEG C Close gas, propane flammable gas:The mol ratio of nitrogen is 1:5, flow control obtains carburizing in 18 hours in 350ml/min, Carburization Treatment Carbon fiber blanket；
（2）Above-mentioned carburizing carbon fiber blanket is immersed into granularity and is less than 0.3 μm of content in the ethanol slurry of 12% zirconium boride, to put Zirconium boride is filled in ultrasonic cleaner to handle 40 minutes, takes out and filling zirconium boride carbon fiber blanket is made after drying；
（3）Above-mentioned filling zirconium boride carbon fiber blanket is passed through trichloromethyl silane gas, hydrogen and argon at a temperature of 1000 DEG C The mixed gas of gas, trichloromethyl silane gas:Hydrogen:The mol ratio of argon gas is 1:4:4, flow control is in 350ml/min, deposition Carborundum handles 18 hours and obtains depositing silicon silicon-carbon tapetum fibrosum；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, oozed under vacuum atmosphere at a temperature of 1650 DEG C 4 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is silica flour 40% and additional 10% concentration of a diameter of 2mm carbon granules 60% is 0.4% polyvinyl alcohol water solution is dried after uniformly mixing and is made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1550 DEG C 18 hours obtained zirconium boride carborundum of nitrogen treatment- Carbon fiber friction material.
Embodiment 3
（1）It is 0.1g/cm by density3Graphited carbon fiber blanket is passed through the mixed of propane flammable gas and nitrogen at a temperature of 1100 DEG C Close gas, propane flammable gas:The mol ratio of nitrogen is 1:6, flow control obtains carburizing in 10 hours in 600ml/min, Carburization Treatment Carbon fiber blanket；
（2）Above-mentioned carburizing carbon fiber blanket is immersed into granularity and is less than 0.3 μm of content in the ethanol slurry of 20% zirconium boride, to put Zirconium boride is filled in ultrasonic cleaner to handle 30 minutes, takes out and filling zirconium boride carbon fiber blanket is made after drying；
（3）Above-mentioned filling zirconium boride carbon fiber blanket is passed through trichloromethyl silane gas, hydrogen and argon at a temperature of 1100 DEG C The mixed gas of gas, trichloromethyl silane gas:Hydrogen:The mol ratio of argon gas is 1: 3:3, flow is controlled in 600ml/min, is sunk Carbon distribution SiClx handles 10 hours and obtains depositing silicon silicon-carbon tapetum fibrosum；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, oozed under vacuum atmosphere at a temperature of 1800 DEG C 3 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is silica flour 50% and additional 15% concentration of a diameter of 3mm carbon granules 50% is 0.6% polyvinyl alcohol water solution is dried after uniformly mixing and is made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1350 DEG C 24 hours obtained zirconium boride carborundum of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. ethanol disperses the preparation method of zirconium boride silicon carbide―carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out the scattered zirconium boride filling processing of ethanol after carrying out Carburization Treatment, then carries out deposition carbon SiClx processing, then carry out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made ethanol disperse zirconium boride carborundum- Carbon fiber friction material, comprise the following steps that：
（1）It is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket is passed through propane flammable gas and nitrogen at a temperature of 900 ~ 1100 DEG C Mixed gas, propane flammable gas:The mol ratio of nitrogen is 1:4 ~ 6, flow control is small in 50 ~ 600ml/min, Carburization Treatment 10 ~ 24 When obtain carburizing carbon fiber blanket；
（2）Above-mentioned carburizing carbon fiber blanket is immersed into granularity and is less than 0.3 μm of content in the ethanol slurry of 5 ~ 20% zirconium borides, to be placed in Zirconium boride is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, takes out and filling zirconium boride carbon fiber blanket is made after drying；
（3）Above-mentioned filling zirconium boride carbon fiber blanket is passed through trichloromethyl silane gas, hydrogen and argon at a temperature of 900 ~ 1100 DEG C The mixed gas of gas, depositing silicon silicon handle 10 ~ 24 hours and obtain depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl silane Gas:Hydrogen:The mol ratio of argon gas is 1:3~5:3 ~ 5, flow is 50 ~ 600ml/min；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, oozed under vacuum atmosphere at a temperature of 1500 ~ 1800 DEG C Silicon handles 3 ~ 5 hours obtained siliconising carbon fiber blankets, wherein, siliconising material be silica flour 30 ~ 50% and a diameter of 0.5 ~ 3mm carbon granules 50 ~ It is made after the uniform combination drying of polyvinyl alcohol water solution that 70% additional 5 ~ 15% concentration of mixture is 0.2 ~ 0.6%；
（5）By above-mentioned siliconising carbon fiber blanket, 10 ~ 24 hours obtained ethanol of nitrogen treatment disperses boron at a temperature of 1350 ~ 1700 DEG C Change zirconium silicon carbide―carbon fiber friction material.
CN201610014320.1A 2016-01-11 2016-01-11 Ethanol disperses the preparation method of zirconium boride carborundum carbon fiber friction material Expired - Fee Related CN105481433B (en)

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CN103922777A (en) * 2014-04-09 2014-07-16 上海大学 Method for preparing carbon/carbon-silicon carbide composite material for bearings
CN104909790A (en) * 2015-05-26 2015-09-16 中国科学院上海硅酸盐研究所 Two-dimensional fiber/boron nitride nanotube multistage reinforcement and preparation method thereof

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CN103922777A (en) * 2014-04-09 2014-07-16 上海大学 Method for preparing carbon/carbon-silicon carbide composite material for bearings
CN104909790A (en) * 2015-05-26 2015-09-16 中国科学院上海硅酸盐研究所 Two-dimensional fiber/boron nitride nanotube multistage reinforcement and preparation method thereof

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