CN105439592B - Close the preparation method that fat disperses tungsten boride carborundum carbon fiber friction material - Google Patents

Close the preparation method that fat disperses tungsten boride carborundum carbon fiber friction material Download PDF

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CN105439592B
CN105439592B CN201610014296.1A CN201610014296A CN105439592B CN 105439592 B CN105439592 B CN 105439592B CN 201610014296 A CN201610014296 A CN 201610014296A CN 105439592 B CN105439592 B CN 105439592B
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carbon fiber
fat
silicon
tungsten boride
friction material
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CN105439592A (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
    • C04B35/565—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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    • C04B35/00—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
    • C04B35/5805—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 borides
    • C04B35/58064—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 borides based on refractory borides
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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
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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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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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    • 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 tungsten boride carborundum carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out carrying out closing the scattered tungsten boride filling processing of fat after Carburization Treatment, depositing silicon silicon processing is carried out again, embedment siliconising processing is carried out again, and then nitrogen treatment is made and closes the scattered tungsten boride carborundum carbon fiber friction material of fat in nitrogen atmosphere.The present invention is to realize the preparation of friction material by carburizing, filling tungsten boride, 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, are to adapt to the friction material under various weather conditions.

Description

Close the preparation method that fat disperses tungsten boride silicon carbide―carbon fiber friction material
Technical field
The present invention relates to the preparation method of a kind of carbon fiber and the compound friction material of ceramic material, belong to composite system Standby technical field.
Background technology
Friction material mainly uses carbon fiber and carbon at present（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, to using bringing serious potential safety hazard.
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 tungsten boride silicon carbide―carbon fiber friction material preparation method be by density be 0.1 ~ 1.8 g/cm3 Graphited carbon fiber blanket carries out carrying out closing the scattered tungsten boride filling processing of fat after Carburization Treatment, then carries out at depositing silicon silicon Reason, then embedment siliconising processing is carried out, then the obtained fat that closes of nitrogen treatment disperses tungsten boride silicon carbide―carbon fiber in nitrogen atmosphere Friction material, is comprised 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 is controlled in 50 ~ 600ml/min, and 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% tungsten borides, It is placed in ultrasonic cleaner and fills tungsten boride processing 30 ~ 50 minutes, takes out and filling tungsten boride 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 tungsten 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 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 50 ~ 70% additional 5 ~ 15% concentration of mixture is obtained after 0.2 ~ 0.6% uniform combination drying of polyvinyl alcohol water solution；
（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 tungsten boride 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, tungsten boride, silicon nitride Degree, high frictional behaviour, the friction material adapted under various weather conditions；
3rd, the system of friction material is realized by carburizing, filling tungsten boride, depositing silicon silicon, the embedment step such as siliconising and nitridation Standby, two steps of carburizing and depositing silicon silicon are the charcoals assigned to protect carbon fiber surface not to be damaged in carbon fiber surface 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 stops silicon steam, thus protect carbon fiber surface not by Destruction；
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 tungsten boride and the method filling carbon fiber blanket of embedment siliconising It is convenient, it is time saving and energy saving, while the anti-wear performance of friction material can further be improved by filling tungsten boride；
5th, the present invention is produced microvesicle by the effect of ultrasonic wave, is worked as sound in the slurry using the pliability of carburizing carbon fiber When pressure or the sound intensity are reached to a certain degree, microvesicle will expand rapidly, then close suddenly again, and the moment of microvesicle closure produces punching Ripple is hit, makes the pressure that about 1012pa is produced around microvesicle, boronation tungsten particle is forced to be filled into the space of carbon fiber blanket, reached The purpose of calking；
6th, using the scattered tungsten boride filling processing of fat slurry is closed, boronation tungsten particle suspendability can be effectively improved, is improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed wraps up boronation tungsten particle, anti-with silicon steam during siliconising Carborundum should be formed, boronation tungsten 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 instantaneous up near 2000 DEG C, by metallic silicon nitridation 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 to be less than in the conjunction fat slurry that 0.3 μm of content is 5% tungsten boride, is placed in Tungsten boride is filled in ultrasonic cleaner to handle 50 minutes, takes out and filling tungsten boride carbon fiber blanket is made after drying, close fat slurry For containing the ethanol solution for closing fat 5%；
（3）Above-mentioned filling tungsten 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 mol ratio of argon gas is 1:5:5, flow control deposits carbon in 50ml/min 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 tungsten boride 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 to be less than in the conjunction fat slurry that 0.3 μm of content is 12% tungsten boride, put Tungsten boride is filled in ultrasonic cleaner to handle 40 minutes, takes out and filling tungsten boride 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 tungsten 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 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 tungsten boride 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 to be less than in the conjunction fat slurry that 0.3 μm of content is 20% tungsten boride, put Tungsten boride is filled in ultrasonic cleaner to handle 30 minutes, takes out and filling tungsten boride 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 tungsten 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 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 tungsten boride carborundum of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. close the preparation method that fat disperses tungsten boride silicon carbide―carbon fiber friction material, it is characterised in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out carrying out closing the scattered tungsten boride filling processing of fat after Carburization Treatment, then carries out deposition carbon SiClx processing, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse tungsten boride carborundum- Carbon fiber friction material, is comprised 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 is controlled in 50 ~ 600ml/min, and Carburization Treatment 10 ~ 24 is small When obtain carburizing carbon fiber blanket；
（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% tungsten borides, is placed in Tungsten boride is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, takes out and filling tungsten boride 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 tungsten 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 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, 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 ~ 70% additional 5 ~ 15% concentration of mixture is obtained after 0.2 ~ 0.6% uniform combination drying of polyvinyl alcohol water solution；
（5）By above-mentioned siliconising carbon fiber blanket, nitrogen treatment is made and closes the scattered boron of fat for 10 ~ 24 hours at a temperature of 1350 ~ 1700 DEG C Change tungsten silicon carbide―carbon fiber friction material.
CN201610014296.1A 2016-01-11 2016-01-11 Close the preparation method that fat disperses tungsten boride carborundum carbon fiber friction material Expired - Fee Related CN105439592B (en)

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