CN105418118B - The preparation method of resin dispersion zirconium carbide boron carbide carbon fiber friction material - Google Patents

The preparation method of resin dispersion zirconium carbide boron carbide carbon fiber friction material Download PDF

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CN105418118B
CN105418118B CN201610014342.8A CN201610014342A CN105418118B CN 105418118 B CN105418118 B CN 105418118B CN 201610014342 A CN201610014342 A CN 201610014342A CN 105418118 B CN105418118 B CN 105418118B
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carbon fiber
boron
friction material
carbide
zirconium carbide
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CN105418118A (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 zirconium carbide boron carbide carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, resin dispersion zirconium carbide filling processing is carried out again, carry out being embedded to siliconising processing again, then resin dispersion zirconium carbide boron carbide carbon fiber friction material is made in nitrogen treatment in nitrogen atmosphere.The present invention is to realize the preparation of friction material by carburizing, depositing silicon silicon, filling zirconium carbide, the embedment step such as siliconising and nitridation using graphitized carbon fibre blanket, 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 zirconium carbide boron 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：
It by density is 0.1 ~ 1.8 g/cm that the preparation method of resin dispersion zirconium carbide boron carbide-carbon fiber friction material, which is,3 Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, then carries out at resin dispersion zirconium carbide filling Reason, then carry out being embedded to siliconising processing, then resin dispersion zirconium carbide boron carbide-carbon fiber is made in nitrogen treatment in nitrogen atmosphere 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 passed through boron chloride, methane, hydrogen and argon gas at a temperature of 900 ~ 1100 DEG C Mixed gas, boron chloride:Methane:Hydrogen:The mol ratio of argon gas is 1:1~2:3~6:4 ~ 6, flow is controlled in 50 ~ 600ml/ Min, depositing silicon boron handle 10 ~ 24 hours and obtain depositing silicon boron carbon fiber blanket；
（3）Above-mentioned depositing silicon boron carbon fiber blanket is immersed into granularity and is less than the paste resin that 0.3 μm of content is 5 ~ 20% zirconium carbides In material, it is placed in ultrasonic cleaner and fills zirconium carbide processing 30 ~ 50 minutes, takes out and filling zirconium carbide carbon fiber is made after drying Blanket, wherein resin slurry are the ethanol solution containing phenolic resin 5 ~ 20%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket 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 resins of nitrogen treatment divide at a temperature of 1350 ~ 1700 DEG C Dissipate zirconium carbide boron 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, the friction material for preparing of the present invention is by compound a kind of high-strength of carbon fiber and boron carbide, zirconium carbide, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3rd, the system of friction material is realized by carburizing, depositing silicon boron, filling zirconium carbide, the embedment step such as siliconising and nitridation It is standby, two steps of carburizing and depositing silicon boron be in order to protect carbon fiber surface not to be damaged and carbon fiber surface assign charcoal Coating and boron carbide coating, because boron carbide coating can stop the infiltration of silicon steam, boron carbide coating 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 boron may require that and be lot more time to reach Densification, manufacturing cost are very high.Will be very using the space of filling zirconium carbide 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 carbide and can further improve the anti-wear performance of friction material；
5th, the present invention produces microvesicle in the slurry using the effect of ultrasonic acoustic, when acoustic pressure or the sound intensity reach to a certain degree When, microvesicle will expand rapidly, and then closure, the moment of microvesicle closure produce shock wave, make to produce about around microvesicle suddenly again 1012Pa pressure, zirconium carbide particle is forced to be filled into the space of depositing silicon silicon-carbon tapetum fibrosum, reaches the purpose of calking；
6th, zirconium carbide filling processing is disperseed using resin slurry, zirconium carbide particle suspendability can be effectively improved, improved Charging efficiency, the activated carbon formed after resin high temperature carbonization wraps up zirconium carbide particle, anti-with silicon steam during siliconising Carborundum should be formed, zirconium carbide particle is firmly combined together by the carborundum of generation；
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 passed through to the mixing of boron chloride, methane, hydrogen and argon gas at a temperature of 900 DEG C Gas, boron chloride:Methane:Hydrogen:The mol ratio of argon gas is 1:1:3:4, flow is controlled at 50ml/min, depositing silicon boron Reason obtains depositing silicon boron carbon fiber blanket in 24 hours；
（3）Above-mentioned depositing silicon silicon-carbon tapetum fibrosum is immersed into granularity and is less than the resin slurry that 0.3 μm of content is 5% zirconium carbide In, it is placed in ultrasonic cleaner and fills zirconium carbide processing 50 minutes, takes out and filling zirconium carbide carbon fiber blanket is made after drying, set Fat slurry is the ethanol solution containing phenolic resin 5%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket 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 carbide boron carbides 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 passed through to the mixing of boron chloride, methane, hydrogen and argon gas at a temperature of 1000 DEG C Gas, boron chloride:Methane:Hydrogen:The mol ratio of argon gas is 1:1.5:4.5:5, flow control is in 350ml/min, deposition carbon Change boron and handle 17 hours acquisition depositing silicon boron carbon fiber blankets；
（3）Above-mentioned depositing silicon boron carbon fiber blanket is immersed into granularity and is less than the resin slurry that 0.3 μm of content is 12% zirconium carbide In, it is placed in ultrasonic cleaner and fills zirconium carbide processing 40 minutes, takes out and filling zirconium carbide carbon fiber blanket is made after drying, set Fat slurry is the ethanol solution containing phenolic resin 12%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket 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 carbide boron carbides 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 passed through to the mixing of boron chloride, methane, hydrogen and argon gas at a temperature of 1100 DEG C Gas, boron chloride:Methane:Hydrogen:The mol ratio of argon gas is 1:2:6:6, flow is controlled in 600ml/min, depositing silicon boron Processing obtains depositing silicon boron carbon fiber blanket in 10 hours；
（3）Above-mentioned depositing silicon boron carbon fiber blanket is immersed into granularity and is less than the resin slurry that 0.3 μm of content is 20% zirconium carbide In, it is placed in ultrasonic cleaner and fills zirconium carbide processing 30 minutes, takes out and filling zirconium carbide carbon fiber blanket is made after drying, set Fat slurry is the ethanol solution containing phenolic resin 20%；
（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 carbide boron carbides of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. the preparation method of resin dispersion zirconium carbide boron carbide-carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, then carries out resin dispersion zirconium carbide Filling is handled, then carries out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made resin dispersion zirconium carbide boron carbide- 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 passed through to the mixing of boron chloride, methane, hydrogen and argon gas at a temperature of 900 ~ 1100 DEG C Gas, boron chloride:Methane:Hydrogen:The mol ratio of argon gas is 1:1~2:3~6:4 ~ 6, flow is controlled in 50 ~ 600mL/min, is sunk Product boron carbide handles 10 ~ 24 hours and obtains depositing silicon boron carbon fiber blanket；
（3）Above-mentioned depositing silicon boron carbon fiber blanket is immersed into granularity and is less than the resin slurry that 0.3 μm of content is 5 ~ 20% zirconium carbides In, it is placed in ultrasonic cleaner and fills zirconium carbide processing 30 ~ 50 minutes, takes out and filling zirconium carbide carbon fiber is made after drying Blanket, wherein resin slurry are the ethanol solution containing phenolic resin 5 ~ 20%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket 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 at a temperature of 1350 ~ 1700 DEG C 10 ~ 24 hours obtained resin dispersion carbon of nitrogen treatment Change zirconium boron carbide-carbon fiber friction material.
CN201610014342.8A 2016-01-11 2016-01-11 The preparation method of resin dispersion zirconium carbide boron carbide carbon fiber friction material Expired - Fee Related CN105418118B (en)

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