CN106957181B - The preparation method of resin dispersion hafnium carbide silicon carbide―carbon fiber friction material - Google Patents

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

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CN106957181B
CN106957181B CN201610014355.5A CN201610014355A CN106957181B CN 106957181 B CN106957181 B CN 106957181B CN 201610014355 A CN201610014355 A CN 201610014355A CN 106957181 B CN106957181 B CN 106957181B
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carbon fiber
silicon
carbide
friction material
hafnium carbide
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CN106957181A (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 hafnium carbide silicon carbide―carbon fiber friction material, which is characterized in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out resin dispersion hafnium carbide 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 hafnium carbide silicon carbide―carbon fiber friction material is made in nitrogen treatment in nitrogen atmosphere.The present invention be using graphitized carbon fibre blanket by carburizing, filling hafnium carbide, 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 hafnium carbide 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 technique
Friction material is wear-resisting due to C/C composite material at present mainly using carbon fiber and carbon (C/C) composite material 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 material exists In moist environment, its frictional behaviour can be reduced, and bring serious security risk to using.
Summary of the invention
Drawbacks described above, realization preparation higher intensity, higher frictional behaviour can be overcome 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 are as follows:
It is 0.1 ~ 1.8 g/cm that the preparation method of resin dispersion hafnium carbide silicon carbide―carbon fiber friction material, which is by density,3 Graphited carbon fiber blanket carries out resin dispersion hafnium carbide filling processing after carrying out Carburization Treatment, then carries out at depositing silicon silicon Reason, then embedment siliconising processing is carried out, then resin dispersion hafnium carbide silicon carbide―carbon fiber is made in nitrogen treatment in nitrogen atmosphere Friction material, the specific steps are as follows:
It (1) 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 hours acquisition carburizing carbon fiber blankets；
(2) above-mentioned carburizing carbon fiber blanket is immersed in the resin slurry that less than 0.3 μm content of granularity is 5 ~ 20% hafnium carbides, It is placed in ultrasonic cleaner and fills hafnium carbide processing 30 ~ 50 minutes, filling hafnium carbide 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 hafnium carbide 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 acquisition depositing silicon silicon-carbon tapetum fibrosums, wherein trichloromethyl Silane gas: hydrogen: the molar ratio of argon gas is 1:3 ~ 5:3 ~ 5, and 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 silicon powder 30 ~ 50% and diameter is 0.5 ~ 3mm carbon granule Additional 5 ~ 15% concentration of 50 ~ 70% mixture is obtained after the uniform combination drying of 0.2 ~ 0.6% polyvinyl alcohol water solution；
(5) at a temperature of 10 ~ 24 hours obtained resins point of nitrogen treatment by above-mentioned siliconising carbon fiber blanket at 1350 ~ 1700 DEG C Dissipate hafnium carbide silicon carbide―carbon fiber friction material.
Compared with the existing technology, the present invention has the following advantages:
1, 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；
2, friction material prepared by the present invention is high-strength by the compound one kind of carbon fiber and silicon carbide, hafnium carbide, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3, by carburizing, filling hafnium carbide, 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 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 leakage, carbide coatings and silicon steam reaction generate silicon carbide and further stop silicon steam, thus protect carbon fiber surface not by It destroys；
4, carbon fiber blanket has the very high porosity, and depending 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 gap of filling hafnium carbide and the method filling carbon fiber blanket for being embedded to siliconising It is convenient, it is time saving and energy saving, while filling hafnium carbide and can further increase the wear-resisting property of friction material；
5, the present invention utilizes the flexibility of carburizing carbon fiber, generates microvesicle 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, and then closure, the moment of microvesicle closure generate suddenly again Shock wave makes the pressure that about 1012pa is generated around microvesicle, and the pressure of hafnium carbide particle is filled into the gap of carbon fiber blanket, is reached To the purpose of calking；
6, using resin slurry dispersion hafnium carbide filling processing, it can effectively improve hafnium carbide particle suspendability, improve Charging efficiency, the active carbon formed after resin high temperature carbonization wraps up hafnium carbide particle, anti-with silicon steam during siliconising Silicon carbide should be formed, silicon carbide is generated and is firmly combined together hafnium carbide particle；
It 7, is 1420 DEG C or so since the metallic silicon fusing point of infiltration is lower, the temperature of friction material working face is instantaneously up to close 2000 DEG C, it will be nitrogenized in metallic silicon and generate silicon nitride, and formed 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
It (1) 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, and flow control is in 50ml/min, 24 hours acquisition carburizing carbon of Carburization Treatment Tapetum fibrosum；
(2) above-mentioned carburizing carbon fiber blanket is immersed in the hafnium carbide resin slurry that less than 0.3 μm content of granularity is 5%, is placed in Hafnium carbide is filled in ultrasonic cleaner to handle 50 minutes, and filling hafnium carbide carbon fiber blanket, resin slurry is made after taking out drying For the ethanol solution containing phenolic resin 5%；
(3) above-mentioned filling hafnium carbide 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, and flow control deposits carbon in 50ml/min SiClx handles 24 hours acquisition depositing silicon silicon-carbon tapetum fibrosums；
(4) by above-mentioned depositing silicon silicon-carbon tapetum fibrosum be embedded to siliconising material in, under vacuum atmosphere 1500 DEG C at a temperature of seep Silicon 5 hours obtained siliconising carbon fiber blankets, wherein siliconising material is silicon powder 30% and diameter is that additional 5% concentration of 0.5mm carbon granule 70% is 0.2% polyvinyl alcohol water solution is dry after evenly mixing to be made；
(5) the at a temperature of nitrogen treatment 10 hours obtained hafnium carbide silicon carbide-by above-mentioned siliconising carbon fiber blanket at 1700 DEG C Carbon fiber friction material.
Embodiment 2
It (1) 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, and flow control is in 350ml/min, Carburization Treatment acquisition carburizing in 18 hours Carbon fiber blanket；
(2) above-mentioned carburizing carbon fiber blanket is immersed in the hafnium carbide resin slurry that less than 0.3 μm content of granularity is 12%, is set Hafnium carbide is filled in ultrasonic cleaner to handle 40 minutes, and filling hafnium carbide carbon fiber blanket, paste resin is made after taking out drying Material is the ethanol solution containing phenolic resin 12%；
(3) above-mentioned filling hafnium carbide 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, and flow control is in 350ml/min, deposition Silicon carbide handles 18 hours acquisition depositing silicon silicon-carbon tapetum fibrosums；
(4) by above-mentioned depositing silicon silicon-carbon tapetum fibrosum be embedded to siliconising material in, under vacuum atmosphere 1650 DEG C at a temperature of seep Silicon 4 hours obtained siliconising carbon fiber blankets, wherein siliconising material is silicon powder 40% and diameter is that additional 10% concentration of 2mm carbon granule 60% is 0.4% polyvinyl alcohol water solution is dry after evenly mixing to be made；
(5) the at a temperature of nitrogen treatment 18 hours obtained hafnium carbide silicon carbide-by above-mentioned siliconising carbon fiber blanket at 1550 DEG C Carbon fiber friction material.
Embodiment 3
It (1) 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, and flow control is in 600ml/min, Carburization Treatment acquisition carburizing in 10 hours Carbon fiber blanket；
(2) above-mentioned carburizing carbon fiber blanket is immersed in the hafnium carbide resin slurry that less than 0.3 μm content of granularity is 20%, is set Hafnium carbide is filled in ultrasonic cleaner to handle 30 minutes, and filling hafnium carbide carbon fiber blanket, paste resin is made after taking out drying Material is the ethanol solution containing phenolic resin 20%；
(3) above-mentioned filling hafnium carbide 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, and flow control is sunk in 600ml/min Carbon distribution SiClx handles 10 hours acquisition depositing silicon silicon-carbon tapetum fibrosums；
(4) by above-mentioned depositing silicon silicon-carbon tapetum fibrosum be embedded to siliconising material in, under vacuum atmosphere 1800 DEG C at a temperature of seep Silicon 3 hours obtained siliconising carbon fiber blankets, wherein siliconising material is silicon powder 50% and diameter is that additional 15% concentration of 3mm carbon granule 50% is 0.6% polyvinyl alcohol water solution is dry after evenly mixing to be made；
(5) the at a temperature of nitrogen treatment 24 hours obtained hafnium carbide silicon carbide-by above-mentioned siliconising carbon fiber blanket at 1350 DEG C Carbon fiber friction material.

Claims (1)

1. the preparation method of resin dispersion hafnium carbide silicon carbide―carbon fiber friction material, which is characterized in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out resin dispersion hafnium carbide filling processing after carrying out Carburization Treatment, then carries out deposition carbon SiClx processing, then embedment siliconising processing is carried out, then resin dispersion hafnium carbide silicon carbide-is made in nitrogen treatment in nitrogen atmosphere Carbon fiber friction material, the specific steps are as follows:
It (1) 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 be 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 in the resin slurry that less than 0.3 μm content of granularity is 5 ~ 20% hafnium carbides, is placed in Hafnium carbide is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, filling hafnium carbide carbon fiber blanket is made after taking out drying, wherein setting Rouge slurry is the ethanol solution containing phenolic resin 5 ~ 20%；
(3) above-mentioned filling hafnium carbide 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 acquisition depositing silicon silicon-carbon tapetum fibrosums, wherein trichloromethyl silane Gas: hydrogen: the molar ratio of argon gas is 1:3 ~ 5:3 ~ 5, and flow is 50 ~ 600mL/min；
(4) by above-mentioned depositing silicon silicon-carbon tapetum fibrosum be embedded to siliconising material in, under vacuum atmosphere 1500 ~ 1800 DEG C at a temperature of seep Silicon handles 3 ~ 5 hours obtained siliconising carbon fiber blankets, wherein siliconising material be silicon powder 30 ~ 50% and diameter for 0.5 ~ 3mm carbon granule 50 ~ Additional 5 ~ 15% concentration of 70% mixture is obtained after the uniform combination drying of 0.2 ~ 0.6% polyvinyl alcohol water solution；
(5) at a temperature of nitrogen treatment 10 ~ 24 hours obtained resin dispersion carbon by above-mentioned siliconising carbon fiber blanket at 1350 ~ 1700 DEG C Change hafnium silicon carbide―carbon fiber friction material.
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