CN105481432A - Preparing method for ethanol-dispersed zirconium carbide silicon carbide and carbon fiber friction material - Google Patents

Preparing method for ethanol-dispersed zirconium carbide silicon carbide and carbon fiber friction material Download PDF

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CN105481432A
CN105481432A CN201610014319.9A CN201610014319A CN105481432A CN 105481432 A CN105481432 A CN 105481432A CN 201610014319 A CN201610014319 A CN 201610014319A CN 105481432 A CN105481432 A CN 105481432A
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carbon fiber
silicon carbide
fiber blanket
carbide
zirconium carbide
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CN105481432B (en
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唐竹兴
田帅
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Shandong University of Technology
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Abstract

The invention relates to a preparing method for an ethanol-dispersed zirconium carbide silicon carbide and carbon fiber friction material. The preparing method is characterized in that a graphited carbon fiber blanket with the density being 0.1-1.8 g/cm<3> is subjected to carburizing treatment and then subjected to ethanol-dispersed zirconium carbide filling treatment, then silicon carbide deposition treatment and embedding siliconizing treatment are carried out in sequence, then nitriding treatment is carried out in a nitrogen atmosphere, and the ethanol-dispersed zirconium carbide silicon carbide and carbon fiber friction material is obtained. According to the preparing method, the friction material is prepared by carrying out the steps of carburizing, zirconium carbide filling, silicon carbide deposition, embedding siliconizing, nitriding and the like on the graphited carbon fiber blanket, and the prepared friction material is high in strength, toughness and friction performance and adaptive to various weather conditions.

Description

The preparation method of ethanol dispersion zirconium carbide silicon carbide―carbon fiber friction materials
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 zirconium carbide silicon carbide―carbon fiber friction materials, it is characterized in that, be 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket carries out ethanol dispersion zirconium carbide and fills process after carrying out carburizing treatment, carry out depositing silicon carbide process again, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains ethanol dispersion zirconium carbide silicon carbide―carbon fiber friction materials, 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 immersion granularity is less than in the ethanol slurry that 0.3 μm of content is 5 ~ 20% zirconium carbides, is placed in ultrasonic cleaner and fills the dry rear obtained filling zirconium carbide carbon fiber blanket of zirconium carbide process taking-up in 30 ~ 50 minutes;
(3) above-mentioned filling zirconium carbide carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixed gas of trichloromethyl silane gas, hydrogen and argon gas, depositing silicon carbide process obtains depositing silicon carbide carbon fiber blanket for 10 ~ 24 hours, wherein, trichloromethyl silane gas: hydrogen: the mol ratio of argon gas is 1:3 ~ 5:3 ~ 5, and flow is 50 ~ 600ml/min;
(4) above-mentioned depositing silicon carbide 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 zirconium carbide silicon carbide―carbon fiber friction materialss 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 graphited carbon fiber and silicon carbide, zirconium carbide, a kind of high strength of silicon nitride compound, high frictional behaviour, the friction materials adapted under various weather condition;
3, by carburizing, fill zirconium carbide, depositing silicon carbide, imbed the preparation that the step such as siliconising and nitrogenize realizes friction materials, carburizing and depositing silicon carbide two steps are at the carbon coating of carbon fiber surface imparting and coat of silicon carbide in order to protect carbon fiber surface not to be damaged, because coat of silicon carbide can stop the infiltration of silicon steam in the process of siliconising, coat of silicon carbide 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, depend merely on carburizing and depositing silicon carbide can need just can reach densification for a long time, manufacturing cost is very high, zirconium carbide 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, fill the wear resisting property that zirconium carbide can improve friction materials further simultaneously;
5, the present invention utilizes the snappiness of carburizing carbon fiber, microvesicle is produced by hyperacoustic ethanol slurry that acts on, 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, makes the pressure producing about 1012pa around microvesicle, zirconium carbide particle is forced to be filled in the space of carbon fiber blanket, reaches the object of calking;
6, adopt ethanol slurry dispersed carbon zirconium to fill process, can effectively improve zirconium carbide particle suspension property, improve charging efficiency, zirconium carbide particle combines by silicon nitride securely that formed in nitriding treatment 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 immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 5% zirconium carbide, be placed in ultrasonic cleaner and fill zirconium carbide process 50 minutes, take out dry rear obtaining and fill zirconium carbide carbon fiber blanket;
(3) above-mentioned filling zirconium carbide carbon fiber blanket is passed at 900 DEG C of temperature the mixed gas of trichloromethyl silane gas, hydrogen and argon gas, trichloromethyl silane gas: hydrogen: the mol ratio of argon gas is 1:5:5, flow control is at 50ml/min, and depositing silicon carbide process obtains depositing silicon carbide carbon fiber blanket for 24 hours;
(4) above-mentioned depositing silicon carbide 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 zirconium carbide silicon carbide―carbon fiber friction materialss 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 immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 12% zirconium carbide, be placed in ultrasonic cleaner and fill zirconium carbide process 40 minutes, take out dry rear obtaining and fill zirconium carbide carbon fiber blanket;
(3) above-mentioned filling zirconium carbide carbon fiber blanket is passed at 1000 DEG C of temperature the mixed gas of trichloromethyl silane gas, hydrogen and argon gas, trichloromethyl silane gas: hydrogen: the mol ratio of argon gas is 1:4:4, flow control is at 350ml/min, and depositing silicon carbide process obtains depositing silicon carbide carbon fiber blanket for 18 hours;
(4) above-mentioned depositing silicon carbide 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 zirconium carbide silicon carbide―carbon fiber friction materialss 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 immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 20% zirconium carbide, be placed in ultrasonic cleaner and fill zirconium carbide process 30 minutes, take out dry rear obtaining and fill zirconium carbide carbon fiber blanket;
(3) above-mentioned filling zirconium carbide carbon fiber blanket is passed at 1100 DEG C of temperature the mixed gas of trichloromethyl silane gas, hydrogen and argon gas, trichloromethyl silane gas: hydrogen: the mol ratio of argon gas is 1:3:3, flow control is at 600ml/min, and depositing silicon carbide process obtains depositing silicon carbide carbon fiber blanket for 10 hours;
(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 zirconium carbide silicon carbide―carbon fiber friction materialss at the temperature of 1350 DEG C.

Claims (1)

1. the preparation method of ethanol dispersion zirconium carbide silicon carbide―carbon fiber friction materials, it is characterized in that, be 0.1 ~ 1.8g/cm by density 3graphited carbon fiber blanket carries out ethanol dispersion zirconium carbide and fills process after carrying out carburizing treatment, carry out depositing silicon carbide process again, carry out imbedding siliconising process, then in nitrogen atmosphere, nitriding treatment obtains ethanol dispersion zirconium carbide silicon carbide―carbon fiber friction materials, 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 immersed granularity to be less than in the ethanol slurry that 0.3 μm of content is 5 ~ 20% zirconium carbides, be placed in ultrasonic cleaner and fill zirconium carbide process 30 ~ 50 minutes, take out dry rear obtaining and fill zirconium carbide carbon fiber blanket;
(3) above-mentioned filling zirconium carbide carbon fiber blanket is passed at 900 ~ 1100 DEG C of temperature the mixed gas of trichloromethyl silane gas, hydrogen and argon gas, depositing silicon carbide process obtains depositing silicon carbide carbon fiber blanket for 10 ~ 24 hours, wherein, trichloromethyl silane gas: hydrogen: the mol ratio of argon gas is 1:3 ~ 5:3 ~ 5, and flow is 50 ~ 600ml/min;
(4) above-mentioned depositing silicon carbide 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 zirconium carbide silicon carbide―carbon fiber friction materialss at the temperature of 1350 ~ 1700 DEG C.
CN201610014319.9A 2016-01-11 2016-01-11 Ethyl alcohol disperses the preparation method of zirconium carbide silicon carbide―carbon fiber friction material Expired - Fee Related CN105481432B (en)

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