CN105418120B - Close the preparation method that fat disperses zirconium carbide boron carbide carbon fiber friction material - Google Patents

Close the preparation method that fat disperses zirconium carbide boron carbide carbon fiber friction material Download PDF

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CN105418120B
CN105418120B CN201610014366.3A CN201610014366A CN105418120B CN 105418120 B CN105418120 B CN 105418120B CN 201610014366 A CN201610014366 A CN 201610014366A CN 105418120 B CN105418120 B CN 105418120B
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carbon fiber
fat
boron
friction material
zirconium carbide
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CN105418120A (en
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唐竹兴
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Shandong University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5622—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on zirconium or hafnium carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/591—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by reaction sintering
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase

Abstract

Close the preparation method that fat disperses 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, carry out closing the scattered zirconium carbide filling processing of fat again, carry out being embedded to siliconising processing again, then nitrogen treatment is made and closes the scattered zirconium carbide boron carbide carbon fiber friction material of fat 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 under various weather conditions.

Description

Close the preparation method that fat disperses 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：
Close fat disperse zirconium carbide boron carbide-carbon fiber friction material preparation method be by density be 0.1 ~ 1.8 g/cm3 Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, then close at the scattered zirconium carbide filling of fat Reason, then carry out being embedded to siliconising processing, then the obtained fat that closes of nitrogen treatment disperses zirconium carbide boron carbide-carbon fiber 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 conjunction fat slurry of 0.3 μm of content for 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 it is containing the ethanol solution for closing fat 5 ~ 20% to close fat slurry；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket is embedded in siliconising material, 1500 ~ 1800 DEG C of the temperature in 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, nitrogen treatment is made and closes fat point for 10 ~ 24 hours 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 is 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, using the scattered zirconium carbide filling processing of fat slurry is closed, zirconium carbide particle suspendability can be effectively improved, is improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed 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 boron carbon fiber blanket is immersed into granularity and is less than the conjunction fat 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, conjunction are made after drying Fat slurry is containing the ethanol solution for closing fat 5%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket is embedded in siliconising material, oozed in 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 18 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 conjunction fat 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, conjunction are made after drying Fat slurry is containing the ethanol solution for closing fat 12%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket is embedded in siliconising material, oozed in 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 600 ml/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 conjunction fat 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, conjunction are made after drying Fat slurry is containing the ethanol solution for closing fat 20%；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket is embedded in siliconising material, oozed in 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. close the preparation method that fat disperses 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 closing the scattered zirconium carbide of fat Filling is handled, then carries out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse 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 conjunction fat 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 it is containing the ethanol solution for closing fat 5 ~ 20% to close fat slurry；
（4）Above-mentioned filling zirconium carbide carbon fiber blanket is embedded in siliconising material, oozed in 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, nitrogen treatment is made and closes the scattered carbon of fat for 10 ~ 24 hours at a temperature of 1350 ~ 1700 DEG C Change zirconium boron carbide-carbon fiber friction material.
CN201610014366.3A 2016-01-11 2016-01-11 Close the preparation method that fat disperses zirconium carbide boron carbide carbon fiber friction material Expired - Fee Related CN105418120B (en)

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CN100371302C (en) * 2006-05-26 2008-02-27 中国科学院上海硅酸盐研究所 Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology
CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN101503305B (en) * 2009-02-03 2012-01-04 西北工业大学 Process for preparing self-sealing silicon carbide ceramic based composite material
CN103086731B (en) * 2011-10-28 2014-07-16 中国科学院上海硅酸盐研究所 Micro-region in-situ reaction preparation method for high strength fiber-reinforced ceramic matrix composite material
CN103044054A (en) * 2012-12-11 2013-04-17 中南大学 Zirconium-titanium carbide-modified anti-ablative carbon/carbon composite material and preparation method thereof
CN103724035B (en) * 2013-07-23 2016-02-03 太仓派欧技术咨询服务有限公司 A kind of density method of fibre reinforced silicon nitride-silicon carbide ceramic composite

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