CN105418127B - Ultrasonic wave disperses the preparation method of hafnium boride boron carbide carbon fiber friction material - Google Patents

Ultrasonic wave disperses the preparation method of hafnium boride boron carbide carbon fiber friction material Download PDF

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CN105418127B
CN105418127B CN201610014386.0A CN201610014386A CN105418127B CN 105418127 B CN105418127 B CN 105418127B CN 201610014386 A CN201610014386 A CN 201610014386A CN 105418127 B CN105418127 B CN 105418127B
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carbon fiber
hafnium boride
friction material
boron
fiber blanket
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CN105418127A (en
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唐竹兴
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Shandong University of Technology
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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
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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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    • C04B2235/30—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

Ultrasonic wave disperses the preparation method of hafnium boride boron carbide carbon fiber friction material, it is characterised in that by density is 0.1 ~ 1.8g/cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, ultrasonic wave is carried out again disperses hafnium boride filling processing, carry out being embedded to siliconising processing again, then the scattered hafnium boride boron carbide carbon fiber friction material of ultrasonic wave is made in nitrogen treatment in nitrogen atmosphere.The present invention is to realize the preparation of friction material by carburizing, depositing silicon silicon, filling hafnium boride, 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 of various weather conditions.

Description

Ultrasonic wave disperses the preparation method of hafnium boride 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：
It by density is 0.1 ~ 1.8 g/ that the preparation method that ultrasonic wave disperses hafnium boride boron carbide-carbon fiber friction material, which is, cm3Graphited carbon fiber blanket carries out depositing silicon boron processing after carrying out Carburization Treatment, then carries out the scattered hafnium boride of ultrasonic wave and fill out Fill processing, then carry out being embedded to siliconising processing, then in nitrogen atmosphere nitrogen treatment be made ultrasonic wave disperse hafnium boride boron carbide- Carbon fiber 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 the slurry that 0.3 μm of content is 5 ~ 20% hafnium borides In, it is placed in ultrasonic cleaner and fills hafnium boride processing 30 ~ 50 minutes, takes out and filling hafnium boride carbon fiber is made after drying Blanket, wherein, slurry is containing the aqueous solution that 0.5 ~ 1.5%pH of ammonium polyacrylate values are 9 ~ 11；
（4）Above-mentioned filling hafnium boride carbon fiber blanket is embedded in siliconising material, 1500 ~ 1800 DEG C of the temperature under 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 at a temperature of 1350 ~ 1700 DEG C 10 ~ 24 hours obtained ultrasonic waves of nitrogen treatment Scattered hafnium boride 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, friction material prepared by the present invention is rubbed by the compound a kind of high intensity of carbon fiber and hafnium boride, silicon nitride, height Wipe the friction material under performance, the various weather conditions of adaptation；
3rd, the system of friction material is realized by carburizing, depositing silicon boron, filling hafnium boride, 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 that silicon steam penetrates into during siliconising, boron carbide coating is once Seepage, carbide coatings further stop silicon steam with silicon steam reaction generation carborundum, so as to protect carbon fiber surface not by broken It is bad；
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 are very high.Will be very using the space of filling hafnium 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 hafnium boride 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, hafnium boride particle is forced to be filled into the space of depositing silicon silicon-carbon tapetum fibrosum, reaches the purpose of calking；
6th, hafnium boride filling processing is disperseed using slurry, hafnium boride particle suspendability can be effectively improved, improve filling Hafnium boride particle is firmly combined together by efficiency, the silicon nitride generated in nitridation process；
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 0.3 μm of content in the slurry of 5% hafnium boride, to put Hafnium boride is filled in ultrasonic cleaner to handle 50 minutes, takes out and filling hafnium boride carbon fiber blanket is made after drying, wherein, slurry Expect the aqueous solution for being 9 for the values of 0.5%pH containing ammonium polyacrylate；
（4）Above-mentioned filling hafnium boride carbon fiber blanket is embedded in siliconising material, oozed under 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 hafnium boride 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 350 ml/min, deposition carbon Change boron and handle 17 hours acquisition depositing silicon boron carbon fiber blankets；
（3）Above-mentioned depositing silicon boron carbon fiber blanket is immersed into granularity to be less than in the slurry that 0.3 μm of content is 12% hafnium boride, It is placed in ultrasonic cleaner and fills hafnium boride processing 40 minutes, takes out and filling hafnium boride carbon fiber blanket is made after drying, wherein, Slurry is the aqueous solution that the values of 1%pH containing ammonium polyacrylate are 10；
（4）Above-mentioned filling hafnium boride carbon fiber blanket is embedded in siliconising material, oozed under 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 hafnium boride 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 600ml/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 to be less than in the slurry that 0.3 μm of content is 20% hafnium boride, It is placed in ultrasonic cleaner and fills hafnium boride processing 30 minutes, takes out and filling hafnium boride carbon fiber blanket is made after drying, wherein, Slurry is the aqueous solution that the values of 1.5%pH containing ammonium polyacrylate are 11；
（4）Above-mentioned filling hafnium boride carbon fiber blanket is embedded in siliconising material, oozed under 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 hafnium boride boron carbides of nitrogen treatment- Carbon fiber friction material.

Claims (1)

1. ultrasonic wave disperses the preparation method of hafnium boride 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 ultrasonic wave and disperse boronation Hafnium filling is handled, then carries out being embedded to siliconising processing, and then the scattered hafnium boride carbon of ultrasonic wave is made in nitrogen treatment in nitrogen atmosphere Change boron-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, mixed gas flow control 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 0.3 μm of content in the slurry of 5 ~ 20% hafnium borides, to put Hafnium boride is filled in ultrasonic cleaner to handle 30 ~ 50 minutes, takes out and filling hafnium boride carbon fiber blanket is made after drying, its In, slurry is containing the aqueous solution that 0.5 ~ 1.5%pH of ammonium polyacrylate values are 9 ~ 11；
（4）Above-mentioned filling hafnium boride carbon fiber blanket is embedded in siliconising material, oozed under 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, 10 ~ 24 hours obtained ultrasonic waves of nitrogen treatment disperse at a temperature of 1350 ~ 1700 DEG C Hafnium boride boron carbide-carbon fiber friction material.
CN201610014386.0A 2016-01-11 2016-01-11 Ultrasonic wave disperses the preparation method of hafnium boride boron carbide carbon fiber friction material Expired - Fee Related CN105418127B (en)

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