CN105439599A - Preparation method of resin dispersed vanadium boride boron carbide-carbon fiber friction material - Google Patents

Preparation method of resin dispersed vanadium boride boron carbide-carbon fiber friction material Download PDF

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CN105439599A
CN105439599A CN201610014336.2A CN201610014336A CN105439599A CN 105439599 A CN105439599 A CN 105439599A CN 201610014336 A CN201610014336 A CN 201610014336A CN 105439599 A CN105439599 A CN 105439599A
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carbon fiber
vanadium boride
fiber blanket
siliconising
carburizing
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唐竹兴
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Shandong University of Technology
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Abstract

A preparation method of a resin dispersed vanadium boride boron carbide-carbon fiber friction material is characterized in that a graphited carbon fiber blanket with the density of 0.1-1.8g/cm<3> is subjected to carburizing treatment, and then is subjected to boron carbide deposition treatment, then resin dispersed vanadium boride filling treatment is performed, embedment siliconizing treatment is performed, and nitriding treatment is performed in a nitrogen atmosphere to obtain the resin dispersed vanadium boride boron carbide-carbon fiber friction material. The preparation of the friction material is realized by adopting the graphited carbon fiber blanket through the steps such as carburizing, boron carbide deposition, vanadium boride filling, embedment siliconizing and nitriding, and the prepared friction material has high strength, high tenacity and high friction performance, and adapts to various weather conditions.

Description

The preparation method of resin dispersion vanadium boride norbide-carbon fiber friction material
Technical field
The present invention relates to the preparation method of the friction materials of a kind of carbon fiber and stupalith compound, belong to technical field of composite preparation.
Background technology
What friction materials mainly adopted at present is carbon fiber and carbon (C/C) matrix material, and because the wear resisting property of C/C matrix material is relatively low, people are seeking the preparation method of the higher friction materials of wear resisting property.In addition, in a humid environment, its frictional behaviour can reduce C/C matrix material, brings serious potential safety hazard to use.
Summary of the invention
The object of the present invention is to provide a kind of preparation method that can overcome above-mentioned defect, realize the friction materials prepared more high strength, higher frictional behaviour and adapt to various weather condition.Its technical scheme is:
The preparation method of resin dispersion vanadium boride norbide-carbon fiber friction material is 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket carries out the process of depositing silicon boron after carrying out carburizing treatment, carry out resin dispersion vanadium boride again and fill process, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains resin dispersion vanadium boride norbide-carbon fiber friction material, and concrete steps are as follows again:
(1) be 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket passes into the mixed gas of propane flammable gas and nitrogen at 900 ~ 1100 DEG C of temperature, propane flammable gas: the mol ratio of nitrogen is 1:4 ~ 6, and flow control is at 50 ~ 600ml/min, and carburizing treatment obtains carburizing carbon fiber blanket for 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixed gas of boron trichloride, methane, hydrogen and argon gas, boron trichloride: methane: hydrogen: the mol ratio of argon gas is 1:1 ~ 2:3 ~ 6:4 ~ 6, flow control is at 50 ~ 600ml/min, and the process of depositing silicon boron obtains depositing silicon boron carbon fiber blanket for 10 ~ 24 hours;
(3) above-mentioned depositing silicon boron carbon fiber blanket immersion granularity being less than 0.3 μm of content is in the resin slurry of 5 ~ 20% vanadium borides, be placed in ultrasonic cleaner and fill vanadium boride process 30 ~ 50 minutes, take out dry rear obtained filling vanadium boride carbon fiber blanket, wherein resin slurry is the ethanolic soln containing resol 5 ~ 20%;
(4) above-mentioned filling vanadium boride carbon fiber blanket is imbedded in siliconising material, siliconising process 3 ~ 5 hours obtained siliconising carbon fiber blankets at the temperature of 1500 ~ 1800 DEG C under vacuum atmosphere, wherein, additional 5 ~ 15% concentration of mixture of siliconising material to be silica flour 30 ~ 50% and diameter be 0.5 ~ 3mm carbon granule 50 ~ 70% are obtain after the polyvinyl alcohol water solution Homogeneous phase mixing drying of 0.2 ~ 0.6%;
(5) by above-mentioned siliconising carbon fiber blanket nitriding treatment 10 ~ 24 hours obtained resin dispersion vanadium boride norbide-carbon fiber friction materials at the temperature of 1350 ~ 1700 DEG C.
Compared with prior art, its advantage is in the present invention:
1, the carbon fiber blanket that the present invention uses is graphited carbon fiber blanket, or graphited needled carbon tapetum fibrosum, or graphited weaving carbon fiber cloth, or graphited 3 D weaving carbon fiber knits block;
2, the friction materials that prepared by the present invention is by carbon fiber and norbide, vanadium boride, a kind of high strength of silicon nitride compound, high frictional behaviour, the friction materials adapted under various weather condition;
3, by carburizing, depositing silicon boron, fill vanadium boride, imbed the preparation that the step such as siliconising and nitrogenize realizes friction materials, carburizing and depositing silicon boron two steps are at the carbon coating of carbon fiber surface imparting and boron carbide coating in order to protect carbon fiber surface not to be damaged, because boron carbide coating can stop the infiltration of silicon steam in the process of siliconising, boron carbide coating is once seepage, carbide coatings and silicon steam reaction Formed SiClx stop silicon steam further, thus protection carbon fiber surface is not damaged;
4, carbon fiber blanket has very high void content, depends merely on carburizing and depositing silicon boron can need just can reach densification for a long time, and manufacturing cost is very high.Vanadium boride is filled in employing will be very convenient with the space of the method filling carbon fiber blanket imbedding siliconising, time saving and energy saving, fills the wear resisting property that vanadium boride can improve friction materials further simultaneously;
5, the present invention utilizes the effect of ultrasonic acoustic to produce microvesicle in the slurry, when acoustic pressure or the sound intensity arrive to a certain degree, microvesicle will undergoes rapid expansion, then close suddenly again, the moment that microvesicle is closed produces shockwave, make the pressure producing about 1012pa around microvesicle, vanadium boride particle is forced to be filled in the space of depositing silicon carbide carbon fiber blanket, reaches the object of calking;
6, resin slurry dispersion vanadium boride is adopted to fill process, effectively can improve vanadium boride particle suspension property, improve charging efficiency, when the gac formed after resin high temperature carbonization is by vanadium boride particle encapsulation, in siliconising process, form silicon carbide with silicon steam reaction, vanadium boride particle combines by the silicon carbide of generation securely;
7, the Pure Silicon Metal fusing point lower owing to infiltrating is about 1420 DEG C, the temperature of friction materials working face is instantaneous reaches nearly 2000 DEG C, Pure Silicon Metal nitrogenize is generated silicon nitride, form the friction materials of microvoid structure, the tolerable temperature of friction materials working face can be increased substantially, improve the work-ing life of friction materials.
Embodiment
embodiment 1
(1) be 1.8g/cm by density 3graphited carbon fiber blanket passes into the mixed gas of propane flammable gas and nitrogen at 900 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:4, flow control is at 50ml/min, and carburizing treatment 24 hours obtains carburizing carbon fiber blanket;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 DEG C of temperature the mixed gas of boron trichloride, methane, hydrogen and argon gas, boron trichloride: methane: hydrogen: the mol ratio of argon gas is 1:1:3:4, flow control is at 50ml/min, and the process of depositing silicon boron obtains depositing silicon boron carbon fiber blanket for 24 hours;
(3) above-mentioned depositing silicon carbide carbon fiber blanket immersion granularity being less than 0.3 μm of content is in the resin slurry of 5% vanadium boride, be placed in ultrasonic cleaner and fill vanadium boride process 50 minutes, take out dry rear obtained filling vanadium boride carbon fiber blanket, resin slurry is the ethanolic soln containing resol 5%;
(4) above-mentioned filling vanadium boride carbon fiber blanket is imbedded in siliconising material, siliconising 5 hours obtained siliconising carbon fiber blankets at the temperature of 1500 DEG C under vacuum atmosphere, wherein, siliconising material is silica flour 30% and diameter, and that to be additional 5% concentration of 0.5mm carbon granule 70% be is dry obtained after the polyvinyl alcohol water solution Homogeneous phase mixing of 0.2%;
(5) by above-mentioned siliconising carbon fiber blanket nitriding treatment 10 hours obtained vanadium boride norbide-carbon fiber friction materials at the temperature of 1700 DEG C.
embodiment 2
(1) be 0.8g/cm by density 3graphited carbon fiber blanket passes into the mixed gas of propane flammable gas and nitrogen at 1000 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:5, flow control is at 350ml/min, and carburizing treatment 18 hours obtains carburizing carbon fiber blanket;
(2) above-mentioned carburizing carbon fiber blanket is passed at 1000 DEG C of temperature the mixed gas of boron trichloride, methane, hydrogen and argon gas, boron trichloride: methane: hydrogen: the mol ratio of argon gas is 1:1.5:4.5:5, flow control is at 350ml/min, and the process of depositing silicon boron obtains depositing silicon boron carbon fiber blanket for 17 hours;
(3) above-mentioned depositing silicon boron carbon fiber blanket immersion granularity being less than 0.3 μm of content is in the resin slurry of 12% vanadium boride, be placed in ultrasonic cleaner and fill vanadium boride process 40 minutes, take out dry rear obtained filling vanadium boride carbon fiber blanket, resin slurry is the ethanolic soln containing resol 12%;
(4) above-mentioned filling vanadium boride carbon fiber blanket is imbedded in siliconising material, siliconising 4 hours obtained siliconising carbon fiber blankets at the temperature of 1650 DEG C under vacuum atmosphere, wherein, siliconising material is silica flour 40% and diameter, and that to be additional 10% concentration of 2mm carbon granule 60% be is dry obtained after the polyvinyl alcohol water solution Homogeneous phase mixing of 0.4%;
(5) by above-mentioned siliconising carbon fiber blanket nitriding treatment 18 hours obtained vanadium boride norbide-carbon fiber friction materials at the temperature of 1550 DEG C.
embodiment 3
(1) be 0.1g/cm by density 3graphited carbon fiber blanket passes into the mixed gas of propane flammable gas and nitrogen at 1100 DEG C of temperature, propane flammable gas: nitrogen mol ratio be 1:6, flow control is at 600ml/min, and carburizing treatment 10 hours obtains carburizing carbon fiber blanket;
(2) above-mentioned carburizing carbon fiber blanket is passed at 1100 DEG C of temperature the mixed gas of boron trichloride, methane, hydrogen and argon gas, boron trichloride: methane: hydrogen: the mol ratio of argon gas is 1:2:6:6, flow control is at 600ml/min, and the process of depositing silicon boron obtains depositing silicon boron carbon fiber blanket for 10 hours;
(3) above-mentioned depositing silicon boron carbon fiber blanket immersion granularity being less than 0.3 μm of content is in the resin slurry of 20% vanadium boride, be placed in ultrasonic cleaner and fill vanadium boride process 30 minutes, take out dry rear obtained filling vanadium boride carbon fiber blanket, resin slurry is the ethanolic soln containing resol 20%;
(4) above-mentioned depositing silicon carbide carbon fiber blanket is imbedded in siliconising material, siliconising 3 hours obtained siliconising carbon fiber blankets at the temperature of 1800 DEG C under vacuum atmosphere, wherein, siliconising material is silica flour 50% and diameter, and that to be additional 15% concentration of 3mm carbon granule 50% be is dry obtained after the polyvinyl alcohol water solution Homogeneous phase mixing of 0.6%;
(5) by above-mentioned siliconising carbon fiber blanket nitriding treatment 24 hours obtained vanadium boride norbide-carbon fiber friction materials at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of resin dispersion vanadium boride norbide-carbon fiber friction material, is characterized in that, is 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket carries out the process of depositing silicon boron after carrying out carburizing treatment, carry out resin dispersion vanadium boride again and fill process, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains resin dispersion vanadium boride norbide-carbon fiber friction material, and concrete steps are as follows again:
(1) be 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket passes into the mixed gas of propane flammable gas and nitrogen at 900 ~ 1100 DEG C of temperature, propane flammable gas: the mol ratio of nitrogen is 1:4 ~ 6, and flow control is at 50 ~ 600ml/min, and carburizing treatment obtains carburizing carbon fiber blanket for 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixed gas of boron trichloride, methane, hydrogen and argon gas, boron trichloride: methane: hydrogen: the mol ratio of argon gas is 1:1 ~ 2:3 ~ 6:4 ~ 6, flow control is at 50 ~ 600ml/min, and the process of depositing silicon boron obtains depositing silicon boron carbon fiber blanket for 10 ~ 24 hours;
(3) above-mentioned depositing silicon boron carbon fiber blanket immersion granularity being less than 0.3 μm of content is in the resin slurry of 5 ~ 20% vanadium borides, be placed in ultrasonic cleaner and fill vanadium boride process 30 ~ 50 minutes, take out dry rear obtained filling vanadium boride carbon fiber blanket, wherein resin slurry is the ethanolic soln containing resol 5 ~ 20%;
(4) above-mentioned filling vanadium boride carbon fiber blanket is imbedded in siliconising material, siliconising process 3 ~ 5 hours obtained siliconising carbon fiber blankets at the temperature of 1500 ~ 1800 DEG C under vacuum atmosphere, wherein, additional 5 ~ 15% concentration of mixture of siliconising material to be silica flour 30 ~ 50% and diameter be 0.5 ~ 3mm carbon granule 50 ~ 70% are obtain after the polyvinyl alcohol water solution Homogeneous phase mixing drying of 0.2 ~ 0.6%;
(5) by above-mentioned siliconising carbon fiber blanket nitriding treatment 10 ~ 24 hours obtained resin dispersion vanadium boride norbide-carbon fiber friction materials at the temperature of 1350 ~ 1700 DEG C.
CN201610014336.2A 2016-01-11 2016-01-11 The preparation method of resin dispersion vanadium boride boron carbide carbon fiber friction material Expired - Fee Related CN105439599B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
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

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