CN105418121B - Close the preparation method that fat disperses titanium boride carbonization boron-carbon fiber friction material - Google Patents

Close the preparation method that fat disperses titanium boride carbonization boron-carbon fiber friction material Download PDF

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CN105418121B
CN105418121B CN201610014368.2A CN201610014368A CN105418121B CN 105418121 B CN105418121 B CN 105418121B CN 201610014368 A CN201610014368 A CN 201610014368A CN 105418121 B CN105418121 B CN 105418121B
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carbon fiber
boron
friction material
fat
titanium boride
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CN105418121A (en
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唐竹兴
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Shandong University of Technology
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    • 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
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    • C04B35/58071—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 based on titanium borides
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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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    • C04B35/626—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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    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase

Abstract

It closes fat and disperses the preparation method of titanium boride boron carbide carbon fiber friction material, which is characterized in that by density be 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, conjunction fat is carried out again disperses titanium boride filling processing, carry out again embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse titanium boride boron carbide carbon fiber friction material.The present invention be using graphitized carbon fibre blanket by carburizing, depositing silicon silicon, filling titanium boride, embedment siliconising and nitridation and etc. realize friction material preparation, prepared friction material high intensity, high tenacity, high frictional behaviour adapt to the friction material of various weather conditions.

Description

Close the preparation method that fat disperses titanium boride carbonization boron-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.
The content of the invention
It is an object of the invention to provide a kind of drawbacks described above, realization can be overcome to prepare higher intensity, higher frictional behaviour And adapt to the preparation method of the friction material of various weather conditions.Its technical solution is：
Close fat disperse titanium boride carbonization boron-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 carries out conjunction fat and disperse at titanium boride filling Reason, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse titanium boride carbonization boron-carbon fiber 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 ~ 24 obtain carburizing carbon fiber blanket when small；
（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 molar ratio of argon gas is 1:1~2:3~6:4 ~ 6, flow control is in 50 ~ 600ml/ Min, depositing silicon boron processing 10 ~ 24 obtain depositing silicon boron carbon fiber blanket when small；
（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% titanium borides It in material, is placed in ultrasonic cleaner and fills titanium boride processing 30 ~ 50 minutes, filling titanium-carbon boride fiber is made after taking out drying Blanket, wherein it is containing the ethanol solution for closing fat 5 ~ 20% to close fat slurry；
（4）Above-mentioned filling titanium-carbon boride tapetum fibrosum is embedded in siliconising material, 1500 ~ 1800 DEG C of the temperature in vacuum atmosphere Siliconising carbon fiber blanket is made when small in lower siliconising processing 3 ~ 5, 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）Above-mentioned siliconising carbon fiber blanket when nitrogen treatment 10 ~ 24 is small at a temperature of 1350 ~ 1700 DEG C is made and closes fat point Dissipate titanium boride carbonization boron-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 boron carbide, titanium boride, silicon nitride Friction material under degree, high frictional behaviour, the various weather conditions of adaptation；
3rd, by carburizing, depositing silicon boron, filling titanium boride, embedment siliconising and nitridation and etc. realize friction material system It is standby, two steps of carburizing and depositing silicon boron be in order to carbon fiber surface is protected 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 leaks, and carbide coatings and silicon steam reaction generation carborundum further stop silicon steam, so as to protect carbon fiber surface from It destroys；
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, manufacture cost is very high, will be very using the gap of filling titanium boride and the method filling carbon fiber blanket for being embedded to siliconising It is convenient, it is time saving and energy saving, while fill titanium boride and can further improve the wear-resisting property of friction material；
5th, the present invention generates microvesicle in the slurry using the effect of ultrasonic acoustic, when acoustic pressure or the sound intensity reache a certain level When, microvesicle will expand rapidly, then be closed suddenly again, and the moment that microvesicle is closed generates shock wave, makes to generate about around microvesicle Boride titanium particle pressure is filled into the gap of depositing silicon silicon-carbon tapetum fibrosum, achievees the purpose that calking by the pressure of 1012Pa；
6th, titanium boride filling processing is disperseed using conjunction fat slurry, boride titanium particle suspendability can be effectively improved, improved Charging efficiency, the activated carbon formed after fat high temperature carbonization is closed wraps up boride titanium particle, anti-with silicon steam during siliconising Carborundum should be formed, boride titanium particle is firmly combined together by the carborundum of generation；
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 service 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 is in 50ml/min, acquisition carburizing carbon when Carburization Treatment 24 is small 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 molar ratio of argon gas is 1:1:3:4, flow control is at 50ml/min, depositing silicon boron Manage 24 it is small when 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 conjunction fat slurry that 0.3 μm of content is 5% titanium boride In, it is placed in ultrasonic cleaner and fills titanium boride processing 50 minutes, filling titanium-carbon boride tapetum fibrosum, conjunction is made after taking out drying Fat slurry is containing the ethanol solution for closing fat 5%；
（4）Above-mentioned filling titanium-carbon boride tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1500 DEG C Siliconising carbon fiber blanket is made in silicon 5 when small, wherein, siliconising material is silica flour 30% and 70% additional 5% concentration of a diameter of 0.5mm carbon granules is 0.2% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 10 is small at a temperature of 1700 DEG C titanium boride boron carbide- 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 350ml/min, Carburization Treatment 18 when small 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 molar ratio of argon gas is 1:1.5:4.5:5, flow control is in 350ml/min, deposition carbon Change boron processing 18 obtains depositing silicon boron carbon fiber blanket when small；
（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% titanium boride In, it is placed in ultrasonic cleaner and fills titanium boride processing 40 minutes, filling titanium-carbon boride tapetum fibrosum, conjunction is made after taking out drying Fat slurry is containing the ethanol solution for closing fat 12%；
（4）Above-mentioned filling titanium-carbon boride tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1650 DEG C Siliconising carbon fiber blanket is made in silicon 4 when small, wherein, siliconising material is silica flour 40% and 60% additional 10% concentration of a diameter of 2mm carbon granules is 0.4% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 18 is small at a temperature of 1550 DEG C titanium boride boron carbide- 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 600ml/min, Carburization Treatment 10 when small 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 molar ratio of argon gas is 1:2:6:6, flow control is in 600 ml/min, depositing silicon boron Handle 10 it is small when 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 conjunction fat slurry that 0.3 μm of content is 20% titanium boride In, it is placed in ultrasonic cleaner and fills titanium boride processing 30 minutes, filling titanium-carbon boride tapetum fibrosum, conjunction is made after taking out drying Fat slurry is containing the ethanol solution for closing fat 20%；
（4）Above-mentioned filling titanium-carbon boride tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1800 DEG C Siliconising carbon fiber blanket is made in silicon 3 when small, wherein, siliconising material is silica flour 50% and 50% additional 15% concentration of a diameter of 3mm carbon granules is 0.6% polyvinyl alcohol water solution is dry after uniformly mixing to be made；
（5）By above-mentioned siliconising carbon fiber blanket be made when nitrogen treatment 24 is small at a temperature of 1350 DEG C titanium boride boron carbide- Carbon fiber friction material.

Claims (1)

1. close the preparation method that fat disperses titanium boride carbonization boron-carbon fiber friction material, which is characterized in that by density for 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, then carries out conjunction fat and disperse titanium boride Filling handle, then carry out embedment siliconising processing, then in nitrogen atmosphere nitrogen treatment be made close fat disperse titanium boride boron 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 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 molar ratio of argon gas is 1:1~2:3~6:4 ~ 6, flow control is sunk in 50 ~ 600mL/min Product boron carbide processing 10 ~ 24 obtains depositing silicon boron carbon fiber blanket when small；
（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% titanium borides In, it is placed in ultrasonic cleaner and fills titanium boride processing 30 ~ 50 minutes, filling titanium-carbon boride fiber is made after taking out drying Blanket, wherein it is containing the ethanol solution for closing fat 5 ~ 20% to close fat slurry；
（4）Above-mentioned filling titanium-carbon boride tapetum fibrosum is embedded in siliconising material, is oozed in vacuum atmosphere at a temperature of 1500 ~ 1800 DEG C Siliconising carbon fiber blanket is made when small in silicon processing 3 ~ 5, 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 that 70% additional 5 ~ 15% concentration of mixture is 0.2 ~ 0.6%；
（5）Conjunction fat is made when nitrogen treatment 10 ~ 24 is small at a temperature of 1350 ~ 1700 DEG C for above-mentioned siliconising carbon fiber blanket and disperses boron Change titanium carbon boron-carbon fiber friction material.
CN201610014368.2A 2016-01-11 2016-01-11 Close the preparation method that fat disperses titanium boride carbonization boron-carbon fiber friction material Expired - Fee Related CN105418121B (en)

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