CN105622147A - Method for preparing resin-dispersed hafnium carbide, boron carbide and carbon fiber friction material - Google Patents

Method for preparing resin-dispersed hafnium carbide, boron carbide and carbon fiber friction material Download PDF

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CN105622147A
CN105622147A CN201610014346.6A CN201610014346A CN105622147A CN 105622147 A CN105622147 A CN 105622147A CN 201610014346 A CN201610014346 A CN 201610014346A CN 105622147 A CN105622147 A CN 105622147A
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carbon fiber
carbide
fiber blanket
boron
hafnium carbide
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唐竹兴
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Shandong University of Technology
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Abstract

The invention discloses a method for preparing a resin-dispersed hafnium carbide, boron carbide and carbon fiber friction material. The method is characterized by comprising the following steps: carbonizing a graphitized carbon fiber blanket with a density of 0.1-1.8g/cm<3>, then depositing boron carbide, filling resin-dispersed tungsten boride, embedding and siliconizing, then nitriding in nitrogen atmosphere to prepare the resin-dispersed hafnium carbide, boron carbide and carbon fiber friction material. The method is characterized by preparing the friction material via the steps of carbonizing the graphitized carbon fiber blanket, depositing boron carbide, filling resin-dispersed hafnium carbide, embedding and siliconizing, and nitriding and the like; the prepared friction material has high strength, high toughness and high friction performance, and can be adapted to various climate conditions.

Description

The preparation method of resin dispersion hafnium carbide 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 resin dispersion hafnium carbide 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 resin dispersion hafnium carbide filling again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares resin dispersion hafnium carbide 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 resin slurry that granularity is 5 ~ 20% hafnium carbides less than 0.3 ��m of content, it is placed in ultrasonic cleaner and fills hafnium carbide process 30 ~ 50 minutes, taking out dried preparing and fill hafnium carbide carbon fiber blanket, wherein resin slurry is the alcoholic solution containing phenolic resin 5 ~ 20%;
(4) above-mentioned filling hafnium carbide 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 resin dispersion hafnium carbide 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 boron carbide, hafnium carbide, 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 carbide, 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 the infiltration of silicon steam 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 carbide and embedment siliconising will be very convenient, time saving and energy saving, fills hafnium carbide 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 arrive 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 carbide granule to be filled in the space of depositing silicon silicon-carbon tapetum fibrosum, reach the purpose of calking;
6, resin slurry dispersion hafnium carbide filling is adopted to process, hafnium carbide granule suspendability can be effectively improved, improve charging efficiency, when the activated carbon formed after resin high temperature carbonization is by hafnium carbide particle encapsulation, forming carborundum with silicon steam reaction in siliconising process, hafnium carbide granule is firmly combined together by the carborundum of generation;
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 silicon-carbon tapetum fibrosum is immersed in the resin slurry that granularity is 5% hafnium carbide less than 0.3 ��m of content, it is placed in ultrasonic cleaner and fills hafnium carbide process 50 minutes, taking out dried preparing and fill hafnium carbide carbon fiber blanket, resin slurry is the alcoholic solution containing phenolic resin 5%;
(4) above-mentioned filling hafnium carbide 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 carbide 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 resin slurry that granularity is 12% hafnium carbide less than 0.3 ��m of content, it is placed in ultrasonic cleaner and fills hafnium carbide process 40 minutes, taking out dried preparing and fill hafnium carbide carbon fiber blanket, resin slurry is the alcoholic solution containing phenolic resin 12%;
(4) above-mentioned filling hafnium carbide 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 carbide 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 resin slurry that granularity is 20% hafnium carbide less than 0.3 ��m of content, it is placed in ultrasonic cleaner and fills hafnium carbide process 30 minutes, taking out dried preparing and fill hafnium carbide carbon fiber blanket, resin slurry is the alcoholic solution containing phenolic resin 20%;
(4) above-mentioned depositing silicon silicon-carbon tapetum fibrosum 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 carbide boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of resin dispersion hafnium carbide 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 resin dispersion hafnium carbide filling again to process, carrying out embedment siliconising again to process, then in nitrogen atmosphere, nitrogen treatment prepares resin dispersion hafnium carbide 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 resin slurry that granularity is 5 ~ 20% hafnium carbides less than 0.3 ��m of content, it is placed in ultrasonic cleaner and fills hafnium carbide process 30 ~ 50 minutes, taking out dried preparing and fill hafnium carbide carbon fiber blanket, wherein resin slurry is the alcoholic solution containing phenolic resin 5 ~ 20%;
(4) above-mentioned filling hafnium carbide 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 resin dispersion hafnium carbide boron carbide-carbon fiber friction materials of nitrogen treatment at the temperature of 1350 ~ 1700 DEG C.
CN201610014346.6A 2016-01-11 2016-01-11 The preparation method of resin dispersion hafnium carbide boron carbide carbon fiber friction material Expired - Fee Related CN105622147B (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
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

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
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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