CN105418103B - Close the preparation method that fat disperses vanadium carbide carborundum carbon fiber friction material - Google Patents

Close the preparation method that fat disperses vanadium carbide carborundum carbon fiber friction material Download PDF

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CN105418103B
CN105418103B CN201610014285.3A CN201610014285A CN105418103B CN 105418103 B CN105418103 B CN 105418103B CN 201610014285 A CN201610014285 A CN 201610014285A CN 105418103 B CN105418103 B CN 105418103B
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carbon fiber
silicon
vanadium carbide
fat
friction material
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CN105418103A (en
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唐竹兴
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Shandong University of Technology
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    • 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
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    • C04B35/565—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 silicon carbide
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    • 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
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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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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract

Close the preparation method that fat disperses vanadium carbide carborundum carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out closing the scattered vanadium carbide filling processing of fat after carrying out Carburization Treatment, depositing silicon silicon processing is carried out again, carry out being embedded to siliconising processing again, then nitrogen treatment is made and closes the scattered vanadium carbide carborundum carbon fiber friction material of fat in nitrogen atmosphere.The present invention is to realize the preparation of friction material by carburizing, filling vanadium carbide, depositing silicon silicon, the embedment step such as siliconising and nitridation using graphitized carbon fibre blanket, prepared friction material high intensity, high tenacity, high frictional behaviour, it is to adapt to the friction material under various weather conditions.

Description

Close the preparation method that fat disperses vanadium carbide silicon 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 vanadium carbide silicon carbide―carbon fiber friction material preparation method be by density be 0.1 ~ 1.8 g/cm3 Graphited carbon fiber blanket carries out closing the scattered vanadium carbide filling processing of fat after carrying out Carburization Treatment, then carries out at depositing silicon silicon Reason, then carry out being embedded to siliconising processing, then the obtained fat that closes of nitrogen treatment disperses vanadium carbide silicon 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 immersed into granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 5 ~ 20% vanadium carbides, It is placed in ultrasonic cleaner and fills vanadium carbide processing 30 ~ 50 minutes, takes out and filling vanadium carbide carbon fiber blanket is made after drying, its The middle fat slurry that closes is containing the ethanol solution for closing fat 5 ~ 20%；
（3）Above-mentioned filling vanadium 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 and obtains depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl Silane gas:Hydrogen:The mol 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 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 vanadium carbide silicon 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 carborundum, vanadium 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, filling vanadium carbide, depositing silicon silicon, the embedment step such as siliconising and nitridation 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 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 silicon may require that and be lot more time to reach Densification, manufacturing cost is very high, will be very using the space of filling vanadium 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 vanadium carbide and can further improve the anti-wear performance of friction material；
5th, the present invention utilizes the pliability of carburizing carbon fiber, produces microvesicle by the slurry that acts on of ultrasonic wave, works as acoustic pressure Or the sound intensity reach to a certain degree when, microvesicle will expand rapidly, then again suddenly closure, microvesicle closure moment produce impact Ripple, make the pressure that about 1012pa is produced around microvesicle, vanadium carbide particle is forced to be filled into the space of carbon fiber blanket, reaches and fills out The purpose of gap；
6th, using the scattered vanadium carbide filling processing of fat slurry is closed, vanadium carbide particle suspendability can be effectively improved, is improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed wraps up vanadium carbide particle, anti-with silicon steam during siliconising Carborundum should be formed, vanadium carbide particle is firmly combined together by generation carborundum；
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 performance and used 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 immersed into granularity and is less than 0.3 μm of content in the conjunction fat slurry of 5% vanadium carbide, to be placed in Vanadium carbide is filled in ultrasonic cleaner to handle 50 minutes, takes out and filling vanadium carbide carbon fiber blanket is made after drying, close fat slurry For containing the ethanol solution for closing fat 5%；
（3）Above-mentioned filling vanadium 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 mol 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, 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 vanadium carbide carborundum 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 immersed into granularity and is less than 0.3 μm of content in the conjunction fat slurry of 12% vanadium carbide, to put Vanadium carbide is filled in ultrasonic cleaner to handle 40 minutes, takes out and filling vanadium carbide carbon fiber blanket is made after drying, and closes fat slurry Expect for containing the ethanol solution for closing fat 12%；
（3）Above-mentioned filling vanadium 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 mol ratio of argon gas is 1:4:4, flow control is in 350ml/min, deposition Carborundum 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, 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 vanadium carbide carborundum 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 immersed into granularity and is less than 0.3 μm of content in the conjunction fat slurry of 20% vanadium carbide, to put Vanadium carbide is filled in ultrasonic cleaner to handle 30 minutes, takes out and filling vanadium carbide carbon fiber blanket is made after drying, and closes fat slurry Expect for containing the ethanol solution for closing fat 20%；
（3）Above-mentioned filling vanadium 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 mol ratio of argon gas is 1: 3:3, flow is controlled in 600ml/min, is sunk 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, 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 vanadium carbide carborundum of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. close the preparation method that fat disperses vanadium carbide silicon carbide―carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out closing the scattered vanadium carbide filling processing of fat after carrying out Carburization Treatment, then carries out deposition carbon SiClx processing, then carry out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse vanadium carbide carborundum- 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 immersed into granularity and is less than 0.3 μm of content in the conjunction fat slurry of 5 ~ 20% vanadium carbides, to be placed in Vanadium carbide is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, takes out and filling vanadium carbide carbon fiber blanket is made after drying, wherein closing Fat slurry is containing the ethanol solution for closing fat 5 ~ 20%；
（3）Above-mentioned filling vanadium 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 and obtain depositing silicon silicon-carbon tapetum fibrosum, wherein, trichloromethyl silane Gas:Hydrogen:The mol 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, 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 vanadium silicon carbide―carbon fiber friction material.
CN201610014285.3A 2016-01-11 2016-01-11 Close the preparation method that fat disperses vanadium carbide carborundum carbon fiber friction material Expired - Fee Related CN105418103B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102617178A (en) * 2012-04-16 2012-08-01 中国人民解放军国防科学技术大学 C/SiC composite material, preparation method of composite material and friction plate
CN103342570A (en) * 2013-07-11 2013-10-09 山东宝纳新材料有限公司 Method for preparing C/SiC composite material through low-cost fused silicon impregnation method
CN104150958A (en) * 2014-08-08 2014-11-19 苏州宏久航空防热材料科技有限公司 Repair method for ceramic matrix composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102617178A (en) * 2012-04-16 2012-08-01 中国人民解放军国防科学技术大学 C/SiC composite material, preparation method of composite material and friction plate
CN103342570A (en) * 2013-07-11 2013-10-09 山东宝纳新材料有限公司 Method for preparing C/SiC composite material through low-cost fused silicon impregnation method
CN104150958A (en) * 2014-08-08 2014-11-19 苏州宏久航空防热材料科技有限公司 Repair method for ceramic matrix composite material

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