CN105481444B - The preparation method of resin dispersion tungsten boride silicon carbide―carbon fiber friction material - Google Patents

The preparation method of resin dispersion tungsten boride silicon carbide―carbon fiber friction material Download PDF

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CN105481444B
CN105481444B CN201610014354.0A CN201610014354A CN105481444B CN 105481444 B CN105481444 B CN 105481444B CN 201610014354 A CN201610014354 A CN 201610014354A CN 105481444 B CN105481444 B CN 105481444B
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carbon fiber
silicon
tungsten boride
friction material
siliconising
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CN105481444A (en
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唐竹兴
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Shandong University of Technology
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Abstract

The preparation method of resin dispersion tungsten boride carborundum carbon fiber friction material, which is characterized in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out resin dispersion tungsten boride filling processing after carrying out Carburization Treatment, depositing silicon silicon processing is carried out again, embedment siliconising processing is carried out again, and then resin dispersion tungsten boride carborundum carbon fiber friction material is made in nitrogen treatment in nitrogen atmosphere.The present invention be using graphitized carbon fibre blanket by carburizing, filling tungsten boride, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material preparation, prepared friction material high intensity, high tenacity, high frictional behaviour adapt to the friction material of various weather conditions.

Description

The preparation method of resin dispersion tungsten boride silicon carbide―carbon fiber friction material
Technical field
The present invention relates to a kind of preparation methods of the compound friction material of carbon fiber and ceramic material, belong to composite material system Standby technical field.
Background technology
Friction material is at present mainly using carbon fiber and carbon（C/C）Composite material is wear-resisting due to C/C composite materials Performance is relatively low, and people are seeking the preparation method of the higher friction material of wear-resisting property.In addition, C/C composite materials exist In moist environment, its frictional behaviour can reduce, and serious security risk is brought to using.
Invention content
Drawbacks described above, realization can be overcome to prepare higher intensity, higher frictional behaviour the purpose of the present invention is to provide a kind of And adapt to the preparation method of the friction material of various weather conditions.Its technical solution is：
The preparation method of resin dispersion tungsten boride silicon carbide―carbon fiber friction material be by density be 0.1 ~ 1.8 g/cm3 Graphited carbon fiber blanket carries out resin dispersion tungsten boride filling processing, then carry out at depositing silicon silicon after carrying out Carburization Treatment Reason, then embedment siliconising processing is carried out, then resin dispersion tungsten boride silicon carbide―carbon fiber is made in nitrogen treatment in nitrogen atmosphere Friction material is as follows：
（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 molar 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 granularity to be less than in the resin slurry that 0.3 μm of content is 5 ~ 20% tungsten borides, It is placed in ultrasonic cleaner and fills tungsten boride processing 30 ~ 50 minutes, filling tungsten boride carbon fiber blanket is made after taking out drying, Middle resin slurry is the ethanol solution containing phenolic resin 5 ~ 20%；
（3）Above-mentioned filling tungsten 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 molar 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 50 ~ 70% additional 5 ~ 15% a concentration of uniform combination drying of 0.2 ~ 0.6% polyvinyl alcohol water solution of mixture；
（5）By above-mentioned siliconising carbon fiber blanket, 10 ~ 24 hours obtained resins of nitrogen treatment divide at a temperature of 1350 ~ 1700 DEG C Dissipate tungsten boride silicon carbide―carbon fiber friction material.
Compared with prior art, the present invention its advantage is：
1st, the carbon fiber blanket that the present invention uses is graphited carbon fiber blanket or graphited needled carbon tapetum fibrosum or stone The weaving carbon fiber cloth or graphited 3 D weaving carbon fiber of inkization knit block；
2nd, friction material prepared by the present invention is high-strength by the compound one kind of carbon fiber and silicon carbide, tungsten boride, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3rd, by carburizing, filling tungsten boride, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material system Standby, two steps of carburizing and depositing silicon silicon are the charcoals assigned in order to which carbon fiber surface is protected not to be damaged in carbon fiber surface 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 leaks, and carbide coatings and silicon steam reaction generation silicon carbide further stop silicon steam, so as to protect carbon fiber surface not by It destroys；
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, manufacture cost is very high, will be very using the gap of filling tungsten 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 tungsten boride and can further improve the wear-resisting property of friction material；
5th, the present invention utilizes the flexibility of carburizing carbon fiber, and microvesicle is generated by the resin 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, then be closed suddenly again, and the moment that microvesicle is closed generates Shock wave makes to generate the pressure of about 1012pa around microvesicle, and the pressure of boronation tungsten particle is filled into the gap of carbon fiber blanket, is reached To the purpose of calking；
6th, using resin slurry dispersion tungsten boride filling processing, boronation tungsten particle suspendability can be effectively improved, is improved Charging efficiency, the activated carbon formed after resin high temperature carbonization wraps up boronation tungsten particle, anti-with silicon steam during siliconising Silicon carbide should be formed, boronation tungsten particle is firmly combined together by generation silicon carbide；
7th, it is 1420 DEG C or so since the metallic silicon fusing point of infiltration is relatively low, the temperature of friction material working face is instantaneously up near 2000 DEG C, generation silicon nitride will be nitrogenized in metallic silicon, and form the friction material of microcellular structure, friction material can be increased substantially The tolerable temperature of working face improves the service life of friction material.
Specific 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 molar 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 resin slurry of 5% tungsten boride, to be placed in Tungsten boride is filled in ultrasonic cleaner to handle 50 minutes, and filling tungsten boride carbon fiber blanket, resin slurry is made after taking out drying For the ethanol solution containing phenolic resin 5%；
（3）Above-mentioned filling tungsten 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 molar 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, is oozed at a temperature of 1500 DEG C under vacuum atmosphere 5 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 30% and a diameter of 0.5mm carbon granules 70% additional 5% 0.2% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1700 DEG C 10 hours obtained tungsten boride silicon carbide 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 molar 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 resin slurry of 12% tungsten boride, to put Tungsten boride is filled in ultrasonic cleaner to handle 40 minutes, and filling tungsten boride carbon fiber blanket, paste resin is made after taking out drying Expect for the ethanol solution containing phenolic resin 12%；
（3）Above-mentioned filling tungsten 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 molar ratio of argon gas is 1:4:4, flow control is in 350ml/min, deposition Silicon carbide 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, is oozed at a temperature of 1650 DEG C under vacuum atmosphere 4 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 40% and a diameter of 2mm carbon granules 60% additional 10% 0.4% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1550 DEG C 18 hours obtained tungsten boride silicon carbide 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 molar 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 resin slurry of 20% tungsten boride, to put Tungsten boride is filled in ultrasonic cleaner to handle 30 minutes, and filling tungsten boride carbon fiber blanket, paste resin is made after taking out drying Expect for the ethanol solution containing phenolic resin 20%；
（3）Above-mentioned filling tungsten 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 molar ratio of argon gas is 1: 3:3, flow control is sunk in 600ml/min 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, is oozed at a temperature of 1800 DEG C under vacuum atmosphere 3 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 50% and a diameter of 3mm carbon granules 50% additional 15% 0.6% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1350 DEG C 24 hours obtained tungsten boride silicon carbide of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. the preparation method of resin dispersion tungsten boride silicon carbide―carbon fiber friction material, which is characterized in that by density for 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out resin dispersion tungsten boride filling processing, then carry out deposition carbon after carrying out Carburization Treatment SiClx processing, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made resin dispersion tungsten boride silicon carbide- Carbon fiber friction material is as follows：
（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 molar ratio of nitrogen is 1:4 ~ 6, in 50 ~ 600ml/min, Carburization Treatment 10 ~ 24 is small for flow control 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 resin slurry of 5 ~ 20% tungsten borides, to be placed in Tungsten boride is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, filling tungsten boride carbon fiber blanket is made after taking out drying, wherein setting Fat slurry is the ethanol solution containing phenolic resin 5 ~ 20%；
（3）Above-mentioned filling tungsten 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 molar 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, is oozed at a temperature of 1500 ~ 1800 DEG C under vacuum atmosphere Silicon handles 3 ~ 5 hours obtained siliconising carbon fiber blankets, wherein, siliconising material for silica flour 30 ~ 50% and a diameter of 0.5 ~ 3mm carbon granules 50 ~ It is made after 70% additional 5 ~ 15% a concentration of uniform combination drying of 0.2 ~ 0.6% polyvinyl alcohol water solution of mixture；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1350 ~ 1700 DEG C 10 ~ 24 hours obtained resin dispersion boron of nitrogen treatment Change tungsten silicon carbide―carbon fiber friction material.
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