CN105439591B - Close the preparation method of fat dispersion ramet silicon carbide―carbon fiber friction material - Google Patents

Close the preparation method of fat dispersion ramet silicon carbide―carbon fiber friction material Download PDF

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CN105439591B
CN105439591B CN201610014294.2A CN201610014294A CN105439591B CN 105439591 B CN105439591 B CN 105439591B CN 201610014294 A CN201610014294 A CN 201610014294A CN 105439591 B CN105439591 B CN 105439591B
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carbon fiber
ramet
silicon
friction material
carbon
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CN105439591A (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
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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
    • C04B35/584—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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • 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
    • C04B35/632—Organic additives
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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
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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
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Inorganic Fibers (AREA)

Abstract

Close fat dispersion ramet carborundum carbon fiber friction material preparation method, which is characterized in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out closing fat dispersion ramet filling processing after carrying out 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 fat dispersion ramet carborundum carbon fiber friction material in nitrogen atmosphere.The present invention be using graphitized carbon fibre blanket by carburizing, filling ramet, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material preparation, prepared friction material high intensity, high tenacity, high frictional behaviour are the friction materials adapted under various weather conditions.

Description

Close the preparation method of fat dispersion ramet 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 technology
Friction material is at present mainly using carbon fiber and carbon（C/C）Composite material is wear-resisting due to C/C composite materials 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 materials exist In moist environment, its frictional behaviour can reduce, and serious security risk is brought to using.
Invention content
Drawbacks described above, realization can be overcome to prepare higher intensity, higher frictional behaviour 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 is：
Close fat dispersion ramet 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 fat dispersion ramet filling processing, then carry out at depositing silicon silicon after carrying out Carburization Treatment Reason, then embedment siliconising processing is carried out, then nitrogen treatment is made and closes fat dispersion ramet silicon carbide―carbon fiber in nitrogen atmosphere Friction material is as follows：
（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 molar 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 granularity to be less than in the conjunction fat slurry that 0.3 μm of content is 5 ~ 20% ramets, It is placed in ultrasonic cleaner and fills ramet processing 30 ~ 50 minutes, filling ramet carbon fiber blanket is made after taking out drying, The middle fat slurry that closes is containing the ethanol solution for closing fat 5 ~ 20%；
（3）Above-mentioned filling ramet 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 molar 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 of 50 ~ 70% mixture additional 5 ~ 15% a concentration of 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 ramet silicon carbide―carbon fiber friction material.
Compared with prior art, the present invention its advantage is：
1st, 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；
2nd, friction material prepared by the present invention is high-strength by the compound one kind of carbon fiber and silicon carbide, ramet, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3rd, by carburizing, filling ramet, depositing silicon silicon, embedment siliconising and nitridation and etc. realize friction material system Standby, two steps of carburizing and depositing silicon silicon are the charcoals assigned in order to which carbon fiber surface is protected 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 leaks, and carbide coatings and silicon steam reaction generation silicon carbide further stop silicon steam, so as to protect carbon fiber surface not by It destroys；
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, manufacture cost is very high, will be very using the gap of filling ramet and the method filling carbon fiber blanket for being embedded to siliconising It is convenient, it is time saving and energy saving, while fill ramet and can further improve the wear-resisting property of friction material；
5th, the present invention utilizes the flexibility of carburizing carbon fiber, generates 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 be closed, microvesicle be closed moment generate impact Wave makes to generate the pressure of about 1012pa around microvesicle, and tantalum carbide particles pressure is filled into the gap of carbon fiber blanket, reaches and fills out The purpose of gap；
6th, using the dispersion ramet filling processing of fat slurry is closed, tantalum carbide particles suspendability can be effectively improved, is improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed wraps up tantalum carbide particles, anti-with silicon steam during siliconising Silicon carbide should be formed, tantalum carbide particles are firmly combined together by generation silicon carbide；
7th, it is 1420 DEG C or so since 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.
Specific 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 molar 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% ramet, to be placed in Ramet is filled in ultrasonic cleaner to handle 50 minutes, and filling ramet carbon fiber blanket is made after taking out drying, closes fat slurry For containing the ethanol solution for closing fat 5%；
（3）Above-mentioned filling ramet 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, 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, is oozed at a temperature of 1500 DEG C in vacuum atmosphere 5 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 30% and a diameter of 0.5mm carbon granules 70% additional 5% 0.2% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1700 DEG C 10 hours obtained ramet silicon carbide 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 molar 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% ramet, to put Ramet is filled in ultrasonic cleaner to handle 40 minutes, and filling ramet carbon fiber blanket is made after taking out drying, closes fat slurry Expect for containing the ethanol solution for closing fat 12%；
（3）Above-mentioned filling ramet 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, flow control is in 350ml/min, deposition Silicon carbide 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, is oozed at a temperature of 1650 DEG C in vacuum atmosphere 4 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 40% and a diameter of 2mm carbon granules 60% additional 10% 0.4% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1550 DEG C 18 hours obtained ramet silicon carbide 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 molar 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% ramet, to put Ramet is filled in ultrasonic cleaner to handle 30 minutes, and filling ramet carbon fiber blanket is made after taking out drying, closes fat slurry Expect for containing the ethanol solution for closing fat 20%；
（3）Above-mentioned filling ramet 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, flow control is sunk in 600ml/min 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, is oozed at a temperature of 1800 DEG C in vacuum atmosphere 3 hours obtained siliconising carbon fiber blankets of silicon, wherein, siliconising material is a concentration of for silica flour 50% and a diameter of 3mm carbon granules 50% additional 15% 0.6% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket at a temperature of 1350 DEG C 24 hours obtained ramet silicon carbide of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. close the preparation method of fat dispersion ramet silicon carbide―carbon fiber friction material, which is characterized in that by density for 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out closing fat dispersion ramet filling processing, then carry out deposition carbon after carrying out Carburization Treatment SiClx processing, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat dispersion ramet silicon carbide- Carbon fiber friction material is as follows：
（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 molar ratio of nitrogen is 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 into granularity and is less than 0.3 μm of content in the conjunction fat slurry of 5 ~ 20% ramets, to be placed in Ramet is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, filling ramet carbon fiber blanket is made after taking out drying, wherein closing Fat slurry is containing the ethanol solution for closing fat 5 ~ 20%；
（3）Above-mentioned filling ramet 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 molar 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, is oozed at a temperature of 1500 ~ 1800 DEG C in vacuum atmosphere Silicon handles 3 ~ 5 hours obtained siliconising carbon fiber blankets, wherein, siliconising material for 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 of 70% mixture additional 5 ~ 15% a concentration of 0.2 ~ 0.6%；
（5）By above-mentioned siliconising carbon fiber blanket, nitrogen treatment is made and closes fat dispersion carbon for 10 ~ 24 hours at a temperature of 1350 ~ 1700 DEG C Change tantalum silicon carbide―carbon fiber friction material.
CN201610014294.2A 2016-01-11 2016-01-11 Close the preparation method of fat dispersion ramet silicon carbide―carbon fiber friction material Expired - Fee Related CN105439591B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103288468A (en) * 2013-05-14 2013-09-11 大连理工大学 Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103288468A (en) * 2013-05-14 2013-09-11 大连理工大学 Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
3D针刺C/SiC-TaC复合材料的热膨胀性能;陈杰等;《复合材料学报》;20110430;第28卷(第2期);第149-154页 *
三维针刺C/(SiC-TaC)复合材料的烧蚀性能及烧蚀机理;王毅等;《硅酸盐学报》;20091031;第37卷(第10期);第1718-1723页 *

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