CN105439594A - Preparation method for ethanol dispersed niobium boride boron carbide-carbon fiber friction material - Google Patents

Preparation method for ethanol dispersed niobium boride boron carbide-carbon fiber friction material Download PDF

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CN105439594A
CN105439594A CN201610014301.9A CN201610014301A CN105439594A CN 105439594 A CN105439594 A CN 105439594A CN 201610014301 A CN201610014301 A CN 201610014301A CN 105439594 A CN105439594 A CN 105439594A
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carbon fiber
boride
niobium
fiber blanket
siliconising
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唐竹兴
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Shandong University of Technology
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Abstract

The invention relates to a preparation method for an ethanol dispersed niobium boride boron carbide-carbon fiber friction material. The preparation method is characterized by comprising the following steps: carrying out carburizing treatment on a graphited carbon fiber blanket having a density of 0.1 to 1.8g/cm<3>, then carrying out boron carbide deposition treatment, and then carrying out filling treatment with ethanol dispersed niobium boride; then carrying out buried siliconing treatment and then carrying out nitrogen treatment in a nitrogen atmosphere to prepare the ethanol dispersed niobium boride boron carbide-carbon fiber friction material. According to the preparation method disclosed by the invention, the friction material is prepared from the graphited carbon fiber blanket through the steps, such as carburizing, boron carbide deposition, niobium boride filling, buried boronizing and nitriding; the prepared friction material is high in strength, tenacity and friction performance and capable of adapting to various climatic conditions.

Description

The preparation method of ethanol dispersion niobium (Nb) 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 ethanol dispersion niobium (Nb) 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 ethanol dispersion niobium (Nb) boride again and fill process, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains ethanol dispersion niobium (Nb) 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 is immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 5 ~ 20% niobium (Nb) borides, be placed in ultrasonic cleaner and fill niobium (Nb) boride process 30 ~ 50 minutes, take out dry rear obtaining and fill niobium (Nb) boride carbon fiber blanket;
(4) above-mentioned filling niobium (Nb) 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 ethanol dispersion niobium (Nb) 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 niobium (Nb) 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 niobium (Nb) 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 that silicon steam infiltrates 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.Niobium (Nb) 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 niobium (Nb) 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 acquire 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, niobium (Nb) boride particle is forced to be filled in the space of depositing silicon carbide carbon fiber blanket, reaches the object of calking;
6, adopt ethanol slurry dispersion niobium (Nb) boride to fill process, effectively can improve niobium (Nb) boride particle suspension property, improve charging efficiency, niobium (Nb) boride particle combines by silicon nitride securely that generate in nitridation process;
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 boron carbon fiber blanket is immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 5% niobium (Nb) boride, be placed in ultrasonic cleaner and fill niobium (Nb) boride process 50 minutes, take out dry rear obtaining and fill niobium (Nb) boride carbon fiber blanket;
(4) above-mentioned filling niobium (Nb) 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 niobium (Nb) 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 is immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 12% niobium (Nb) boride, be placed in ultrasonic cleaner and fill niobium (Nb) boride process 40 minutes, take out dry rear obtaining and fill niobium (Nb) boride carbon fiber blanket;
(4) above-mentioned filling niobium (Nb) 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 niobium (Nb) 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 is immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 20% niobium (Nb) boride, be placed in ultrasonic cleaner and fill niobium (Nb) boride process 30 minutes, take out dry rear obtaining and fill niobium (Nb) boride carbon fiber blanket;
(4) above-mentioned filling niobium (Nb) boride 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 niobium (Nb) boride norbide-carbon fiber friction materials at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of ethanol dispersion niobium (Nb) boride norbide-carbon fiber friction material, it is characterized in that, be 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 ethanol dispersion niobium (Nb) boride again and fill process, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains ethanol dispersion niobium (Nb) 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, mixed gas flow controls 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 is immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 5 ~ 20% niobium (Nb) borides, be placed in ultrasonic cleaner and fill niobium (Nb) boride process 30 ~ 50 minutes, take out dry rear obtaining and fill niobium (Nb) boride carbon fiber blanket;
(4) above-mentioned filling niobium (Nb) 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 ethanol dispersion niobium (Nb) boride norbide-carbon fiber friction materials at the temperature of 1350 ~ 1700 DEG C.
CN201610014301.9A 2016-01-11 2016-01-11 Ethyl alcohol disperses the preparation method of niobium (Nb) boride boron carbide-carbon fiber friction material Expired - Fee Related CN105439594B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
CN102617178A (en) * 2012-04-16 2012-08-01 中国人民解放军国防科学技术大学 C/SiC composite material, preparation method of composite material and friction plate
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
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
CN102617178A (en) * 2012-04-16 2012-08-01 中国人民解放军国防科学技术大学 C/SiC composite material, preparation method of composite material and friction plate
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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