CN105622139A - Preparation method of ethanol dispersed hafnium boride silicon carbide-carbon fiber friction material - Google Patents

Preparation method of ethanol dispersed hafnium boride silicon carbide-carbon fiber friction material Download PDF

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CN105622139A
CN105622139A CN201610014311.2A CN201610014311A CN105622139A CN 105622139 A CN105622139 A CN 105622139A CN 201610014311 A CN201610014311 A CN 201610014311A CN 105622139 A CN105622139 A CN 105622139A
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carbon fiber
hafnium boride
fiber blanket
siliconising
friction material
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唐竹兴
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Shandong University of Technology
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Abstract

The invention provides a preparation method of an ethanol dispersed hafnium boride silicon carbide-carbon fiber friction material. The preparation method is characterized in that graphited carbon fiber blanket with the density being 0.1 to 1.8g/cm<3> is subjected to carburizing treatment; then, boron carbide deposition treatment is performed; then, ethanol dispersed hafnium boride filling treatment is performed; next, embedding siliconing treatment is performed; next, nitridation treatment is performed in nitrogen atmosphere to obtain the ethanol dispersed hafnium boride silicon carbide-carbon fiber friction material. The graphited carbon fiber blanket is used; the friction material preparation is realized through the steps of carburization, silicon carbide deposition, hafnium boride filling, embedding siliconing, nitridation and the like; the prepared friction material has high intensity, high toughness and high friction performance, and belongs to a friction material adapting to various climate conditions.

Description

The preparation method of ethanol dispersion hafnium boride boron carbide-carbon fiber friction material
Technical field
The preparation method that the present invention relates to the friction material of a kind of carbon fiber and ceramic material compound, belongs to technical field of composite preparation.
Background technology
What friction material currently mainly adopted is carbon fiber and carbon (C/C) composite, owing to the anti-wear performance of C/C composite is relatively low, and the preparation method that people are seeking the higher friction material of anti-wear performance. It addition, C/C composite is in a humid environment, its frictional behaviour can reduce, and brings serious potential safety hazard to using.
Summary of the invention
It is an object of the invention to provide and a kind of can overcome drawbacks described above, realize preparation higher intensity, higher frictional behaviour and adapt to the preparation method of friction material of various weather conditions. Its technical scheme is:
The preparation method of ethanol dispersion hafnium boride boron carbide-carbon fiber friction material is to be 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket carries out depositing silicon boron process after carrying out Carburization Treatment, carry out ethanol dispersion hafnium boride filling again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares ethanol dispersion hafnium boride boron carbide-carbon fiber friction material, specifically comprises the following steps that
(1) it is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing 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 Carburization Treatment obtains carburizing carbon fiber blanket in 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixing gas of boron chloride, methane, hydrogen and argon, boron chloride: methane: hydrogen: the mol ratio of argon is 1:1 ~ 2:3 ~ 6:4 ~ 6, flow-control is at 50 ~ 600ml/min, and depositing silicon boron processes 10 ~ 24 hours and obtains depositing silicon boron carbon fiber blanket;
(3) above-mentioned depositing silicon boron carbon fiber blanket is immersed in the ethanol slurry that granularity is 5 ~ 20% hafnium borides less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill hafnium boride process 30 ~ 50 minutes, take out dried preparing and fill hafnium boride carbon fiber blanket;
(4) above-mentioned filling hafnium boride carbon fiber blanket is imbedded in siliconising material, under vacuum atmosphere, at the temperature of 1500 ~ 1800 DEG C, siliconising processes 3 ~ 5 hours prepared siliconising carbon fiber blankets, wherein, siliconising material is silica flour 30 ~ 50% and the polyvinyl alcohol water solution Homogeneous phase mixing that additional 5 ~ 15% concentration of mixture are 0.2 ~ 0.6% that diameter is 0.5 ~ 3mm carbon granule 50 ~ 70% prepares after drying;
(5) by above-mentioned siliconising carbon fiber blanket 10 ~ 24 hours prepared ethanol dispersion hafnium boride boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1350 ~ 1700 DEG C.
Compared with prior art, its advantage is 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, friction material prepared by the present invention is by carbon fiber and hafnium boride, a kind of high intensity of silicon nitride compound, high frictional behaviour, the friction material that adapts under various weather conditions;
3, by carburizing, depositing silicon boron, fill hafnium boride, embedment siliconising and the step such as nitrogenize and realize the preparation of friction material, carburizing and two steps of depositing silicon boron be in order to protect carbon fiber surface not to be damaged and carbon fiber surface give carbon coating and boron carbide coating, because boron carbide coating can stop that silicon steam penetrates in the process of siliconising, boron carbide coating is once seepage, carbide coatings and silicon steam reaction generate carborundum and stop silicon steam further, thus protecting carbon fiber surface not to be damaged;
4, carbon fiber blanket has the significantly high porosity, depends merely on carburizing and depositing silicon boron may require that and is lot more time to reach densification, and manufacturing cost is significantly high. The space adopting the method filling carbon fiber blanket filling hafnium boride and embedment siliconising will be very convenient, time saving and energy saving, fills hafnium boride simultaneously and can improve the anti-wear performance of friction material further;
5, the present invention utilizes the effect of ultrasonic acoustic to produce microvesicle in the slurry, when acoustic pressure or the sound intensity reach to a certain degree, microvesicle will expand rapidly, then close suddenly again, the moment of microvesicle Guan Bi produces shock wave, make to produce around microvesicle the pressure of about 1012pa, force hafnium boride granule to be filled in the space of depositing silicon silicon-carbon tapetum fibrosum, reach the purpose of calking;
6, the dispersion hafnium boride filling of ethanol slurry is adopted to process, it is possible to being effectively improved hafnium boride granule suspendability, improve charging efficiency, hafnium boride granule is firmly combined together by the silicon nitride generated in nitridation process;
7, due to penetrate into metallic silicon fusing point relatively low be about 1420 DEG C, the temperature of friction material work surface is instantaneous up to nearly 2000 DEG C, metallic silicon is nitrogenized generation silicon nitride, form the friction material of microcellular structure, the tolerable temperature of friction material work surface can be increased substantially, improve the service life of friction material.
Detailed description of the invention
Embodiment 1
(1) it is 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing 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 Carburization Treatment obtains carburizing carbon fiber blanket in 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 DEG C of temperature the mixing gas of boron chloride, methane, hydrogen and argon, boron chloride: methane: hydrogen: the mol ratio of argon is 1:1:3:4, flow-control is at 50ml/min, and depositing silicon boron processes 24 hours and obtains depositing silicon boron carbon fiber blanket;
(3) above-mentioned depositing silicon boron carbon fiber blanket is immersed in the ethanol slurry that granularity is 5% hafnium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill hafnium boride process 50 minutes, take out dried preparing and fill hafnium boride carbon fiber blanket;
(4) above-mentioned filling hafnium boride carbon fiber blanket is imbedded in siliconising material, 5 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1500 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 30% and diameter to be additional 5% concentration of 0.5mm carbon granule 70% be 0.2% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 10 hours prepared hafnium boride boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1700 DEG C.
Embodiment 2
(1) it is 0.8g/cm by density3Graphited carbon fiber blanket passes into the mixing 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 Carburization Treatment obtains carburizing carbon fiber blanket in 18 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 1000 DEG C of temperature the mixing gas of boron chloride, methane, hydrogen and argon, boron chloride: methane: hydrogen: the mol ratio of argon is 1:1.5:4.5:5, flow-control is at 350ml/min, and depositing silicon boron processes 17 hours and obtains depositing silicon boron carbon fiber blanket;
(3) above-mentioned depositing silicon boron carbon fiber blanket is immersed in the ethanol slurry that granularity is 12% hafnium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill hafnium boride process 40 minutes, take out dried preparing and fill hafnium boride carbon fiber blanket;
(4) above-mentioned filling hafnium boride carbon fiber blanket is imbedded in siliconising material, 4 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1650 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 40% and diameter to be additional 10% concentration of 2mm carbon granule 60% be 0.4% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 18 hours prepared hafnium boride boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1550 DEG C.
Embodiment 3
(1) it is 0.1g/cm by density3Graphited carbon fiber blanket passes into the mixing 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 Carburization Treatment obtains carburizing carbon fiber blanket in 10 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 1100 DEG C of temperature the mixing gas of boron chloride, methane, hydrogen and argon, boron chloride: methane: hydrogen: the mol ratio of argon is 1:2:6:6, flow-control is at 600ml/min, and depositing silicon boron processes 10 hours and obtains depositing silicon boron carbon fiber blanket;
(3) above-mentioned depositing silicon boron carbon fiber blanket is immersed in the ethanol slurry that granularity is 20% hafnium boride less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill hafnium boride process 30 minutes, take out dried preparing and fill hafnium boride carbon fiber blanket;
(4) above-mentioned filling hafnium boride carbon fiber blanket is imbedded in siliconising material, 3 hours prepared siliconising carbon fiber blankets of siliconising at the temperature of 1800 DEG C under vacuum atmosphere, wherein, siliconising material be silica flour 50% and diameter to be additional 15% concentration of 3mm carbon granule 50% be 0.6% polyvinyl alcohol water solution Homogeneous phase mixing after dry prepare;
(5) by above-mentioned siliconising carbon fiber blanket 24 hours prepared hafnium boride boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of ethanol dispersion hafnium boride boron carbide-carbon fiber friction material, it is characterised in that be 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket carries out depositing silicon boron process after carrying out Carburization Treatment, carry out ethanol dispersion hafnium boride filling again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares ethanol dispersion hafnium boride boron carbide-carbon fiber friction material, specifically comprises the following steps that
(1) it is 0.1 ~ 1.8g/cm by density3Graphited carbon fiber blanket passes into the mixing 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 Carburization Treatment obtains carburizing carbon fiber blanket in 10 ~ 24 hours;
(2) above-mentioned carburizing carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixing gas of boron chloride, methane, hydrogen and argon, boron chloride: methane: hydrogen: the mol ratio of argon is 1:1 ~ 2:3 ~ 6:4 ~ 6, mixed gas flow controls at 50 ~ 600ml/min, and depositing silicon boron processes 10 ~ 24 hours and obtains depositing silicon boron carbon fiber blanket;
(3) above-mentioned depositing silicon boron carbon fiber blanket is immersed in the ethanol slurry that granularity is 5 ~ 20% hafnium borides less than 0.3 ��m of content, be placed in ultrasonic cleaner and fill hafnium boride process 30 ~ 50 minutes, take out dried preparing and fill hafnium boride carbon fiber blanket;
(4) above-mentioned filling hafnium boride carbon fiber blanket is imbedded in siliconising material, under vacuum atmosphere, at the temperature of 1500 ~ 1800 DEG C, siliconising processes 3 ~ 5 hours prepared siliconising carbon fiber blankets, wherein, siliconising material is silica flour 30 ~ 50% and the polyvinyl alcohol water solution Homogeneous phase mixing that additional 5 ~ 15% concentration of mixture are 0.2 ~ 0.6% that diameter is 0.5 ~ 3mm carbon granule 50 ~ 70% prepares after drying;
(5) by above-mentioned siliconising carbon fiber blanket 10 ~ 24 hours prepared ethanol dispersion hafnium boride boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1350 ~ 1700 DEG C.
CN201610014311.2A 2016-01-11 2016-01-11 Ethanol disperses the preparation method of hafnium boride boron carbide carbon fiber friction material Expired - Fee Related CN105622139B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110453495A (en) * 2019-09-24 2019-11-15 吉林大学 A kind of method of carbon fiber surface plating boron carbide

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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
CN104909790A (en) * 2015-05-26 2015-09-16 中国科学院上海硅酸盐研究所 Two-dimensional fiber/boron nitride nanotube multistage reinforcement and preparation method thereof

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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
CN104909790A (en) * 2015-05-26 2015-09-16 中国科学院上海硅酸盐研究所 Two-dimensional fiber/boron nitride nanotube multistage reinforcement and preparation method thereof

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