CN105481421B - Close the preparation method that fat disperses zirconium boride silicon carbide―carbon fiber friction material - Google Patents

Close the preparation method that fat disperses zirconium boride silicon carbide―carbon fiber friction material Download PDF

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CN105481421B
CN105481421B CN201610014281.5A CN201610014281A CN105481421B CN 105481421 B CN105481421 B CN 105481421B CN 201610014281 A CN201610014281 A CN 201610014281A CN 105481421 B CN105481421 B CN 105481421B
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carbon fiber
zirconium boride
silicon
fat
friction material
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CN105481421A (en
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唐竹兴
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Shandong University of Technology
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Abstract

It closes fat and disperses the preparation method of zirconium boride carborundum carbon fiber friction material, which is characterized in that by density be 0.1 ~ 1.8g/cm3Conjunction fat, which is carried out, after graphited carbon fiber blanket progress Carburization Treatment disperses zirconium boride filling processing, depositing silicon silicon processing is carried out again, carry out again embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse zirconium boride carborundum carbon fiber friction material.The present invention be using graphitized carbon fibre blanket by carburizing, filling zirconium boride, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material preparation, prepared friction material high intensity, high tenacity, high frictional behaviour are the friction materials adapted under various weather conditions.

Description

Close the preparation method that fat disperses zirconium 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.
The content of the invention
It is an object of the invention to provide a kind of drawbacks described above, realization can be overcome to prepare higher intensity, higher frictional behaviour And adapt to the preparation method of the friction material of various weather conditions.Its technical solution is：
Close fat disperse zirconium boride silicon carbide―carbon fiber friction material preparation method be by density be 0.1 ~ 1.8 g/cm3 Conjunction fat is carried out after graphited carbon fiber blanket progress Carburization Treatment and disperses zirconium boride filling processing, then is carried out at depositing silicon silicon Reason, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse zirconium boride silicon carbide―carbon fiber 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 ~ 24 obtain carburizing carbon fiber blanket when small；
（2）Above-mentioned carburizing carbon fiber blanket is immersed granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 5 ~ 20% zirconium borides, It is placed in ultrasonic cleaner and fills zirconium boride processing 30 ~ 50 minutes, filling zirconium boride carbon fiber blanket is made after taking out drying, The middle fat slurry that closes is containing the ethanol solution for closing fat 5 ~ 20%；
（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 processing 10 ~ 24 obtains depositing silicon silicon-carbon tapetum fibrosum when small, 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 in vacuum atmosphere Siliconising carbon fiber blanket is made when small in lower siliconising processing 3 ~ 5, 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）Above-mentioned siliconising carbon fiber blanket when nitrogen treatment 10 ~ 24 is small at a temperature of 1350 ~ 1700 DEG C is made and closes fat point Dissipate zirconium 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 carborundum, zirconium boride, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3rd, by carburizing, filling zirconium boride, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material system It is standby, two steps of carburizing and depositing silicon silicon be in order to carbon fiber surface is protected 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 leaks, and carbide coatings and silicon steam reaction generation carborundum further stop silicon steam, so as to protect carbon fiber surface from 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 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 wear-resisting property of friction material；
5th, the present invention utilizes the flexibility of carburizing carbon fiber, generates microvesicle in the slurry by the effect of ultrasonic wave, works as sound When 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 punching Ripple is hit, makes the pressure that about 1012Pa is generated around microvesicle, the pressure of zirconium boride particle is filled into the gap of carbon fiber blanket, is reached The purpose of calking.
6th, zirconium boride filling processing is disperseed using conjunction fat slurry, zirconium boride particle suspendability can be effectively improved, improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed wraps up zirconium boride particle, anti-with silicon steam during siliconising Carborundum should be formed, zirconium boride particle is firmly combined together by generation carborundum；
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, 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 performance and used 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 is in 50ml/min, acquisition carburizing carbon when Carburization Treatment 24 is small Tapetum fibrosum；
（2）Above-mentioned carburizing carbon fiber blanket is immersed granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 5% zirconium boride, is placed in Zirconium boride is filled in ultrasonic cleaner to handle 50 minutes, and filling zirconium boride carbon fiber blanket is made after taking out drying, closes fat slurry For containing the ethanol solution for closing fat 5%；
（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 molar ratio of argon gas is 1:5:5, flow control is in 50ml/min, deposition carbon SiClx processing 24 obtains depositing silicon silicon-carbon tapetum fibrosum when small；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1500 DEG C Siliconising carbon fiber blanket is made in silicon 5 when small, wherein, siliconising material is silica flour 30% and 70% additional 5% concentration of a diameter of 0.5mm carbon granules is 0.2% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 10 is small at a temperature of 1700 DEG C zirconium boride carborundum- 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 350ml/min, Carburization Treatment 18 when small Carbon fiber blanket；
（2）Above-mentioned carburizing carbon fiber blanket is immersed granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 12% zirconium boride, is put Zirconium boride is filled in ultrasonic cleaner to handle 40 minutes, and filling zirconium boride carbon fiber blanket is made after taking out drying, closes fat slurry Expect for containing the ethanol solution for closing fat 12%；
（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 molar ratio of argon gas is 1:4:4, flow control is in 350ml/min, deposition Carborundum processing 18 obtains depositing silicon silicon-carbon tapetum fibrosum when small；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1650 DEG C Siliconising carbon fiber blanket is made in silicon 4 when small, wherein, siliconising material is silica flour 40% and 60% additional 10% concentration of a diameter of 2mm carbon granules is 0.4% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 18 is small at a temperature of 1550 DEG C zirconium boride carborundum- 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 600ml/min, Carburization Treatment 10 when small Carbon fiber blanket；
（2）Above-mentioned carburizing carbon fiber blanket is immersed granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 20% zirconium boride, is put Zirconium boride is filled in ultrasonic cleaner to handle 30 minutes, and filling zirconium boride carbon fiber blanket is made after taking out drying, closes fat slurry Expect for containing the ethanol solution for closing fat 20%；
（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 molar ratio of argon gas is 1: 3:3, flow control is sunk in 600ml/min Carbon distribution SiClx processing 10 obtains depositing silicon silicon-carbon tapetum fibrosum when small；
（4）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1800 DEG C Siliconising carbon fiber blanket is made in silicon 3 when small, wherein, siliconising material is silica flour 50% and 50% additional 15% concentration of a diameter of 3mm carbon granules is 0.6% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 24 is small at a temperature of 1350 DEG C zirconium boride carborundum- Carbon fiber friction material.

Claims (1)

1. closing fat disperses the preparation method of zirconium boride silicon carbide―carbon fiber friction material, which is characterized in that by density for 0.1 ~ 1.8g/cm3Conjunction fat is carried out after graphited carbon fiber blanket progress Carburization Treatment and disperses zirconium boride filling processing, then carries out deposition carbon SiClx processing, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse zirconium boride carborundum- 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 granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 5 ~ 20% zirconium borides, is placed in Zirconium boride is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, filling zirconium boride carbon fiber blanket is made after taking out drying, wherein closing Fat slurry is containing the ethanol solution for closing fat 5 ~ 20%；
（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 processing 10 ~ 24 obtain depositing silicon silicon-carbon tapetum fibrosum when small, 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 in vacuum atmosphere at a temperature of 1500 ~ 1800 DEG C Siliconising carbon fiber blanket is made when small in silicon processing 3 ~ 5, wherein, siliconising material for 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）Conjunction fat is made when nitrogen treatment 10 ~ 24 is small at a temperature of 1350 ~ 1700 DEG C for above-mentioned siliconising carbon fiber blanket and disperses boron Change zirconium silicon carbide―carbon fiber friction material.
CN201610014281.5A 2016-01-11 2016-01-11 Close the preparation method that fat disperses zirconium boride silicon carbide―carbon fiber friction material Expired - Fee Related CN105481421B (en)

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