CN115368140A - Low-wear carbon-ceramic brake material and preparation method thereof - Google Patents
Low-wear carbon-ceramic brake material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 312
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 309
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 97
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 92
- 238000001764 infiltration Methods 0.000 claims abstract description 84
- 230000008595 infiltration Effects 0.000 claims abstract description 84
- 239000010703 silicon Substances 0.000 claims abstract description 53
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 53
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 42
- 238000005470 impregnation Methods 0.000 claims abstract description 32
- 238000005299 abrasion Methods 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 154
- 229910052757 nitrogen Inorganic materials 0.000 claims description 77
- 238000010438 heat treatment Methods 0.000 claims description 76
- 238000000034 method Methods 0.000 claims description 52
- 238000005475 siliconizing Methods 0.000 claims description 52
- 239000004744 fabric Substances 0.000 claims description 47
- 238000000151 deposition Methods 0.000 claims description 45
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 28
- 239000003085 diluting agent Substances 0.000 claims description 25
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- 239000004743 Polypropylene Substances 0.000 description 26
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
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- GUWKQWHKSFBVAC-UHFFFAOYSA-N [C].[Au] Chemical compound [C].[Au] GUWKQWHKSFBVAC-UHFFFAOYSA-N 0.000 description 1
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- 238000009827 uniform distribution Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
- F16D69/02—Composition of linings ; Methods of manufacturing
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- C04B2235/428—Silicon
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- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0034—Materials; Production methods therefor non-metallic
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Abstract
The invention discloses a preparation method of a low-abrasion carbon-ceramic brake material, which comprises the steps of carrying out chemical vapor deposition and resin impregnation on a carbon fiber preform to obtain a carbon matrix, and then carrying out reaction infiltration on silicon to obtain the carbon-ceramic brake material.
Description
Technical Field
The invention relates to a low-abrasion carbon-ceramic brake material and a preparation method thereof, belonging to the technical field of brake disc preparation.
Background
The carbon-ceramic brake material is a high-performance friction material developed on the basis of a C/C material, compared with the C/C friction material, the carbon-ceramic brake material has the advantages that the wet friction performance attenuation is reduced, the static friction coefficient is large, and the C/C friction material can obtain stable braking capability at high temperature but cannot obtain stable braking capability at low temperature. The C/SiC friction material has stable braking capability at high temperature and very stable braking capability at low temperature.
At present, a plurality of methods for preparing the carbon/silicon carbide ceramic brake material comprise a precursor impregnation cracking method, a plasma spraying method, a vapor deposition method, a reaction infiltration method and the like. The carbon-ceramic brake material prepared by the method can basically solve the brake problems of most airplanes, high-speed trains, automobiles and the like. But the wear of carbon-ceramic brake materials is still high compared to carbon/carbon brake materials. The wear of the brake material is mainly abrasive wear and fatigue wear. The carbon/carbon brake material can form a self-lubricating layer which takes graphite as a main component on a friction surface, abrasive wear can be effectively reduced, and the high heat conduction of the graphite can effectively reduce the friction surface temperature, so that fatigue wear is reduced. The abrasive dust of the carbon ceramic brake material takes silicon carbide particles as main components, and a lubricating layer cannot be formed on a friction surface. The carbon-ceramic brake material has poor heat conduction compared with a carbon/carbon brake material, high friction surface temperature and increased fatigue wear.
Disclosure of Invention
In view of the defects of the prior art, the first object of the invention is to provide a preparation method of a low-abrasion carbon-ceramic brake material.
The second purpose of the invention is to provide the carbon-ceramic brake material with low abrasion prepared by the preparation method. The carbon-ceramic brake material is low in abrasion, low in brake curve peak-to-valley ratio and free of tail warping.
In order to realize the problems, the invention adopts the following technical scheme:
the invention relates to a preparation method of a low-abrasion carbon ceramic brake material, which comprises the following steps:
step one preparation of carbon fiber preform
Alternately laying a non-woven fabric and a thin net felt, continuously needling in X and Y directions, and then performing bidirectional puncture on asphalt-based carbon fibers in Z direction to obtain a carbon fiber preform, wherein the weight percentage of the non-woven fabric to the thin net felt in the carbon fiber preform is 58-62: 38 to 42;
step two, preparation of carbon/carbon prefabricated body
Carrying out chemical vapor deposition and heat treatment on the carbon fiber preform obtained in the step one by taking propylene as a carbon source and nitrogen as a diluent gas to obtain a carbon/carbon preform, wherein the deposition pressure is 1.4-1.8 kPa during the chemical vapor deposition, and the deposition temperature is 920-970 ℃;
step three, preparation of carbon/carbon porous body
Adding the carbon/carbon preform obtained in the second step into an impregnant for impregnation, then curing to obtain a cured preform, and then carbonizing and cracking to obtain a carbon/carbon porous body, wherein the impregnant consists of bisphenol A epoxy resin, epoxypropane benzyl ether and a boron nitride ethylamine complex, the mass fraction of the epoxypropane benzyl ether is 28-32%, and the mass fraction of the boron nitride ethylamine complex is 22-26%;
step four, preparing carbon-ceramic brake material
And (4) carrying out reaction, melting and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material.
According to the preparation method, in the preparation process of the preform, the weftless fabric lower than the prior art is adopted, so that the content of the thin net felt is increased, and in the chemical vapor deposition process, carbon is enriched in the thin net felt layer, so that the content of pyrolytic carbon can be increased during chemical vapor deposition, the content of SiC is increased finally, and the hardness and strength of the matrix can be greatly increased due to the increase of the content of SiC, so that the abrasion is effectively reduced; in addition, after 2D layering and needling are completed, the Z-direction steel needle introduces the asphalt carbon fibers with high heat conductivity into the 2D preform to form a 3D preform, so that the interlaminar shear strength and heat conductivity of the material are improved, and fatigue wear and oxidation wear are reduced.
In the chemical vapor deposition process, the pyrolytic carbon is controlled to be of a smooth layer structure through the control of temperature and pressure during chemical vapor deposition, the smooth layer structure has high carbon hardness and high strength, can effectively support silicon carbide, is not easy to break, has good lubricity and can greatly reduce the material abrasion.
After the chemical vapor deposition, the resin carbon matrix is further introduced, the viscosity of the obtained impregnant cannot change along with the increase of the impregnation times by adjusting the formula of the impregnant, the volume of the impregnant shrinks after carbonization and cracking, gaps of a blank cannot be blocked, and the formed pyrolytic carbon has a porous structure and is favorable for infiltration of subsequent reaction infiltration silicon liquid. In addition, in the formula of the impregnant, the boron nitride ethylamine complex is used as a curing agent, a small amount of nitrogen and boron elements can be introduced into a carbon matrix, and the growth of silicon carbide crystal grains in the reaction infiltration process can be effectively inhibited under the synergistic action of nitrogen and boron, so that the size distribution of the silicon carbide crystal grains is uniform. The uniform silicon carbide grains in the friction process can reduce vibration and reduce abrasion. Finally, the low-abrasion carbon-ceramic brake material is obtained by reaction, melting and siliconizing.
Certainly, in the preparation process of the preform, the weight percentage of the non-woven cloth and the thin net felt needs to be effectively controlled, if the proportion of the non-woven cloth is too low, the brittleness and the toughness of the subsequently prepared material are reduced, the brittle fracture or the collapse of the tooth part is easily caused by impact in the braking process, and if the proportion of the non-woven cloth is too high, a larger gap cannot be formed, the content of the CVD carbon is reduced, so that the content of the SiC is reduced, and the effect of reducing the abrasion cannot be achieved.
In chemical vapor deposition, the pressure and temperature are not controlled properly, and 100% smooth layer structure, such as rough layer structure or carbon black formation, cannot be obtained.
Preferably, in the first step, the weftless fabric and the thin net felt are alternately layered, the density between layers is controlled to be 11-15 layers/cm, then the fabric is continuously needled in the X and Y directions, the row spacing and the spacing of needling are both controlled to be 2.0-2.4 multiplied by 2.0-2.4 mm, and the needling density is 20-25 needles/cm 2 And then, performing bidirectional puncture by using pitch-based carbon fibers in the Z direction, wherein the row spacing and the interval of the puncture are controlled to be 4.8-5.2 multiplied by 4.8-5.2 mm, and thus obtaining the carbon fiber preform.
Preferably, in the first step, the weftless fabric is polypropylene-based carbon fiber (PANCF) weftless fabric, and the thin net felt is polypropylene-based carbon fiber (PANCF) weftless fabric.
Preferably, in the first step, the density of the carbon fiber preform is 0.50-0.60 g/cm 3 。
Preferably, in the second step, the volume ratio of the propylene to the nitrogen is 0.8-1.2: 0.8 to 1.2.
Preferably, in the second step, the deposition temperature is 930-960 ℃ and the deposition time is 180-220 h during the chemical vapor deposition.
The inventors have found that by controlling the deposition temperature within the above range, the resulting smooth layer structure is optimized.
Preferably, in the second step, the temperature of the heat treatment is 1500-1800 ℃, preferably 1550-1650 ℃, and the time of the heat treatment is 1-3 h, preferably 1.5h.
After chemical vapor deposition, through thermal treatment, open the hole, promote follow-up charcoal/charcoal porous body preparation in-process, the efficiency of flooding, in thermal treatment, avoid the high temperature to make smooth layer structure charcoal stress graphitization appear, the microcrack appears in the interface of carbon fiber and pyrolytic carbon, interface strength reduces, and material fatigue wearing increases.
Preferably, in the second step, the density of the carbon/carbon preform is 1.30-1.33 g/cm 3 。
Hair brushIn the light of the above, the inventors have found that the abrasion of the material can be reduced by controlling the density within the above range by chemical vapor deposition, then obtaining a carbon-carbon porous body by resin impregnation and densification, and then melt siliconizing, while obtaining a density of 1.38 to 1.45g/cm by direct chemical vapor deposition 3 The carbon/carbon porous body has different pore sizes, so that the simple substance silicon can remain in the macropores in the reaction infiltration process. In the braking process, the simple substance silicon can be softened along with the rise of the temperature of the friction surface, the friction coefficient is rapidly reduced, and the micro silicon powder in the abrasive dust has strong water absorption, so that the wet braking performance is attenuated. The process for impregnating the porous carbon by the resin not only increases the specific surface area of pores, but also effectively fills the macropores with the resin carbon, silicon liquid enters the pores to react with the resin carbon to generate silicon carbide, so that the content of the silicon carbide is increased, the amount of simple substance silicon is reduced, the silicon carbide generated by the reaction of the porous carbon and the silicon has a more stable structure, and the material abrasion can be effectively reduced.
Preferably, in the third step, the impregnant is obtained by the following method: firstly, the bisphenol A type epoxy resin is kept at the temperature of 35-45 ℃ for 0.5-1 h, then the epoxypropane benzyl ether is added, after even stirring, the boron nitride ethylamine complex is added, and even stirring is carried out, thus obtaining the bisphenol A type epoxy resin.
Preferably, in the third step, before dipping, the carbon/carbon preform is washed by distilled water, then washed by distilled water for 0.5-1 h, and finally dried at 110-130 ℃ for 4-10 h.
Preferably, in the third step, the impregnation process comprises the steps of putting the carbon/carbon preform into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 1-2 h, pressurizing to 3-5 MPa by using nitrogen, and impregnating for 1-2 h.
Preferably, in the third step, the curing temperature is 120-180 ℃, and the curing time is 4-6 h.
Further preferably, the curing is performed under normal pressure. The inventor finds that the porous carbon structure can be better formed by adopting normal pressure solidification, and is beneficial to silicon liquid infiltration in the reaction infiltration process.
In the actual operation process, the curing agent can be directly cured in an impregnation tank, namely after the impregnation is finished, the impregnating agent is discharged, and the curing agent is cured after the temperature is directly raised.
In the preferred scheme, in the third step, the carbonization and pyrolysis temperature is 1100-1200 ℃, the heat preservation time is 2-3 h, the temperature rise rate is 3-5 ℃/min, and the pressure is 0-0.005 MPa.
In the actual operation process, the solidified blank is put into a carbonization furnace, the vacuum-pumping nitrogen is used for replacing for two times, then the nitrogen is filled to the micro-positive pressure (0-0.005) MPa, and then the temperature is raised.
Preferably, in the third step, the density of the carbon/carbon porous body is 1.38-1.45 g/cm 3 。
In the actual operation process, the obtained carbon/carbon porous body is machined according to the size of the brake disc, and machining allowance of 0.2mm is reserved on the friction surface in two directions.
In the preferred scheme, in the fourth step, the purity of the silicon used for the reaction infiltration is more than or equal to 99.0 percent, and the particle size is less than or equal to 400 meshes.
Preferably, in the fourth step, the reaction infiltration silicon is carried out in nitrogen atmosphere, the temperature of the reaction infiltration silicon is 1850-2100 ℃, preferably 1850-1950 ℃, the time of the reaction infiltration silicon is 2-3 h, preferably 2h, and the pressure is 6000-8000 Pa.
The invention adopts micro negative pressure reaction infiltration during reaction infiltration silicon, and simultaneously vacuumizes and directly introduces nitrogen into the reaction chamber, thereby not only ensuring uniform distribution of nitrogen in the reaction chamber, but also improving the vapor saturation pressure of silicon, leading silicon and carbon to react fully, simultaneously fully utilizing nitrogen, leading nitrogen atoms to enter silicon carbide crystal cells and inhibiting the rapid growth of silicon carbide crystal grains, thus not only ensuring uniform reaction infiltration, but also refining the silicon carbide crystal grains.
The invention also provides the carbon-ceramic brake material prepared by the preparation method.
Principles and advantages
According to the preparation method, in the preparation process of the preform, the weftless fabric lower than the prior art is adopted, so that the content of the thin net felt is increased, and in the chemical vapor deposition process, carbon is enriched in the thin net felt layer, so that the content of pyrolytic carbon can be increased during chemical vapor deposition, the content of SiC is increased finally, and the hardness and strength of the matrix can be greatly increased due to the increase of the content of SiC, so that the abrasion is effectively reduced; in addition, after 2D layering and needling are completed, the pitch carbon fibers with high heat conductivity are introduced into the 2D preform by the Z-direction steel needle to form a 3D preform, so that the interlaminar shear strength and the heat conductivity of the material are improved, and the fatigue wear and the oxidation wear are reduced.
In the chemical vapor deposition process, the pyrolytic carbon is controlled to be of a smooth layer structure through the control of temperature and pressure during chemical vapor deposition, the smooth layer structure has high carbon hardness and high strength, can effectively support silicon carbide, is not easy to break, has good lubricity and can greatly reduce the material abrasion.
After the chemical vapor deposition, the resin carbon matrix is further introduced, the viscosity of the obtained impregnant cannot change along with the increase of the impregnation times by adjusting the formula of the impregnant, the volume of the impregnant shrinks after carbonization and cracking, gaps of a blank cannot be blocked, and the formed pyrolytic carbon has a porous structure and is favorable for infiltration of subsequent reaction infiltration silicon liquid. In addition, in the formula of the impregnant, a boron nitride ethylamine complex compound is used as a curing agent, a small amount of nitrogen and boron elements can be introduced into a carbon matrix, and the growth of silicon carbide crystal grains in the reaction infiltration process can be effectively inhibited under the synergistic action of nitrogen and boron, so that the size distribution of the silicon carbide crystal grains is uniform. The uniform carborundum grains can reduce vibration and abrasion in the friction process.
Finally, silicon is melted and infiltrated through reaction, micro negative pressure reaction infiltration is adopted during the silicon melting and infiltration reaction, vacuum pumping is carried out, nitrogen is directly introduced into the reaction chamber, the nitrogen in the reaction chamber can be ensured to be uniformly distributed, the steam saturation pressure of silicon can be improved, the silicon-carbon reaction is sufficient, nitrogen is fully utilized, nitrogen atoms can enter silicon carbide crystal cells, the rapid growth of silicon carbide crystal grains is inhibited, the uniform reaction infiltration can be ensured, the silicon carbide crystal grains can be refined, and finally the low-wear carbon ceramic brake material is obtained.
The advantages of the invention are as follows:
1. the invention increases the content of the thin net felt and increases the fiber puncture in the Z direction, so that the interlaminar shear strength of the brake material is improved from (30 +/-10) MPa to (95 +/-10) MPa. The problem of the monoblock condition of droing that causes because of fatigue wear is solved.
2. The CVD pyrolytic carbon prepared by the invention is of a smooth layer structure, has high hardness, high strength and good wear resistance, is strongly bonded with the interface of carbon fiber and silicon carbide, enhances the supporting effect on the silicon carbide and reduces the wear of silicon carbide particles.
3. The content of simple substance silicon formed in the reaction infiltration process is generally (5-15)%, the simple substance silicon can increase the attenuation rate of high-energy braking, and the micro silicon powder formed in the abrasive dust has strong water absorption and can increase the attenuation rate of wet braking performance. The invention uses resin dipping technique to fill the macropores in the carbon/carbon prefabricated body, so that the gap distribution of the matrix is more uniform, and the content of the simple substance silicon after the reaction infiltration is low, which is only (1.5 +/-0.1)%.
4. The invention adopts the boron nitride ethylamine complex containing nitrogen and boron as the curing agent, can introduce a small amount of nitrogen and boron elements into the carbon matrix, and can effectively inhibit the growth of silicon carbide crystal grains in the reaction infiltration process under the synergistic action of nitrogen and boron. However, the size of the silicon carbide crystal grains is increased at high temperature, the large silicon carbide crystal grains can vibrate at low speed due to the enhanced meshing effect in the braking process, and the braking curve has tail warping and large peak-to-valley ratio. The invention carries out reaction infiltration in nitrogen atmosphere, nitrogen atoms can enter the silicon carbide unit cell to inhibit the rapid growth of silicon carbide crystal grains, thus not only ensuring the uniform reaction infiltration, but also ensuring that the silicon carbide crystal grains cannot grow too large. In the carbon-ceramic brake material prepared by the invention, the content of silicon carbide (40 +/-1.5)%, and the grain size
Surface hardness 94HD.
The carbon-ceramic brake material prepared by the invention has the wear rate of less than 0.62 mu m/surface/time, is basically consistent with that of a carbon/carbon brake material, has low peak-to-valley ratio of a brake curve, does not have tail warping, has stable brake performance, and can realize the application of the carbon-ceramic brake material in civil aviation.
Drawings
FIG. 1 is a carbon-ceramic brake disc test sample prepared in example 1 of the present invention.
Fig. 2 is a phase diagram of CVD pyrolytic carbon gold in the structure of a carbon-ceramic brake material prepared in example 1 of the present invention. The metallographic structure showed full-gloss sliding-layer structure carbon.
FIG. 3 shows the structural XRD detection of the carbon ceramic brake material prepared in the embodiment 1 of the present invention. The test results show that the CVD pyrolytic carbon content is 42.7%, the silicon carbide content is 40.0%, the resin carbon content is 15.9%, and the elemental silicon content is 1.5%.
Detailed Description
Example 1
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling after layering is completed in the X direction and the Y direction, controlling the row spacing and the space between needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The carbon/carbon preform of (1), wherein the deposition pressure is 1.5kPa and the deposition temperature is 930 ℃; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing carbon-ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40 percent of silicon carbide, 1.5 percent of silicon, 310MPa of compressive strength, 240MPa of bending strength and 90MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.62 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 13%.
Example 2
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The carbon/carbon preform, wherein during the chemical vapor deposition, the deposition pressure is 1.5kPa, and the deposition temperature is 945 ℃; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonization and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 More carbon/carbonA porous body.
Step four, preparing the carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40.2 percent of silicon carbide, 1.4 percent of silicon, 312MPa of compressive strength, 241MPa of bending strength and 94MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.62 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 13%.
Example 3
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the first step, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The deposition pressure is 1.5kPa and the deposition temperature is 960 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and preserving heat for 1h. Then 30 percent of epoxy propane benzyl ether serving as a diluent is added and stirred evenly, and finally 24 percent of boron nitride ethylamine complex serving as a curing agent is added and stirred evenly.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ for curing for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing carbon-ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40 percent of silicon carbide, 1.6 percent of silicon, 315MPa of compressive strength, 239MPa of bending strength and 92MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.60 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet brake performance attenuation rate is 14%.
Example 4
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid fabric and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid fabric 0) 0 /90 0 /270 0 Layering), wherein the weight percentage of the non-woven cloth to the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 After the two-way puncture is carried out on the high-heat-conductivity pitch carbon fiber (TYG) in the Z direction to prepare a carbon fiber preform, the row spacing and the spacing of the Z-direction fiber are 5.0mmx5.0mm during the puncture, and the density of the obtained carbon fiber preform is 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the first step, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The carbon/carbon preform of (1), wherein the deposition pressure is 1.5kPa and the deposition temperature is 930 ℃; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and preserving heat for 1h. Then adding 28 percent of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 22 percent of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonization and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 Carbon/carbon porousAnd (3) a body.
Step four, preparing the carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 The silicon carbide content is 39.9 percent, the silicon content is 1.4 percent, the compressive strength is 309MPa, the bending strength is 241MPa, and the shearing strength is 94MPa. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.62 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 13%.
Example 5
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid fabric and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid fabric 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 After the two-way puncture is carried out on the high-heat-conductivity pitch carbon fiber (TYG) in the Z direction to prepare a carbon fiber preform, the row spacing and the spacing of the Z-direction fiber are 5.0mmx5.0mm during the puncture, and the density of the obtained carbon fiber preform is 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The deposition pressure is 1.5kPa, and the deposition temperature is 930 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 32% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 26% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix by using distilled water, then putting the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix by using a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ for curing for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing the carbon ceramic brake material
And (3) performing reaction infiltration siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction siliconizing is performed in a nitrogen atmosphere, the temperature of the reaction siliconizing is 1900 ℃, the time of the reaction siliconizing is 2h, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 The silicon carbide content is 40 percent, the silicon content is 1.5 percent, the compressive strength is 315MPa, the bending strength is 243MPa, and the shearing strength is 95MPa. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.62 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 12%.
Example 6
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Layering), the weight percentage of the non-woven cloth to the thin net felt is 58:42, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 After the two-way puncture is carried out on the high-heat-conductivity pitch carbon fiber (TYG) in the Z direction to prepare a carbon fiber preform, the row spacing and the spacing of the Z-direction fiber are 5.0mmx5.0mm during the puncture, and the density of the obtained carbon fiber preform is 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The deposition pressure is 1.5kPa, and the deposition temperature is 930 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and preserving heat for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix by using distilled water, then putting the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix by using a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: putting the dried and cooled carbon/carbon blank into a dipping kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the dipping kettle, dipping for 2 hours, pressurizing to 4MPa by using nitrogen, dipping for 2 hours, then decompressing, and discharging the impregnant. Then the temperature is increased to 150 ℃ for curing for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 Carbon/carbon porous body of。
Step four, preparing carbon-ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40.2 percent of silicon carbide, 1.7 percent of silicon, 312MPa of compressive strength, 240MPa of bending strength and 93MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.63 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 14%.
Example 7
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid fabric and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid fabric 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 62:38, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The deposition pressure is 1.5kPa, and the deposition temperature is 930 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix by using distilled water, then putting the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix by using a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonization and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing carbon-ceramic brake material
And (3) performing reaction infiltration siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction siliconizing is performed in a nitrogen atmosphere, the temperature of the reaction siliconizing is 1900 ℃, the time of the reaction siliconizing is 2h, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40.3 percent of silicon carbide, 1.3 percent of silicon, 308MPa of compressive strength, 293MPa of bending strength and 89MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.35, the wear rate is 0.61 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.48, and the wet braking performance attenuation rate is 12%.
TABLE 1 Performance results of the carbon-ceramic brake materials obtained in examples 1 to 7
Comparative example 1 (preform non-piercing structure)
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is (60): (40) Controlling the interlayer density to be 15 layers/cm, continuously needling in X and Y directions after layering, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 The density of the obtained carbon fiber preform was 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the first step, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.32g/cm 3 The deposition pressure is 1.5kPa, and the deposition temperature is 930 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix by using distilled water, then putting the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix by using a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: putting the dried and cooled carbon/carbon blank into a dipping kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the dipping kettle, dipping for 2 hours, pressurizing to 4MPa by using nitrogen, dipping for 2 hours, then decompressing, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, and vacuumizing nitrogenReplacing twice, then filling nitrogen to micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating rate 5 ℃/min, and keeping the temperature for 3h to obtain the product with density of 1.47g/cm 3 The carbon/carbon porous body of (3).
Step four, preparing the carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.22g/cm 3 38 percent of silicon carbide, 3.5 percent of silicon, 240MPa of compressive strength, 201MPa of bending strength and 23MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.33, the wear rate is 1.22 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.52, and the wet brake performance attenuation rate is 28%.
Comparative example 2 (No impregnation procedure, no porous carbon in the green body)
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 12 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 After the two-way puncture is carried out on the high-heat-conductivity pitch carbon fiber (TYG) in the Z direction to prepare a carbon fiber preform, the row spacing and the spacing of the Z-direction fiber are 5.0mmx5.0mm during the puncture, and the density of the obtained carbon fiber preform is 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain a density of 1.45g/cm 3 The deposition pressure during the chemical vapor deposition is 1.5kPa, deposition temperature 930 ℃; the deposition time is 300h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparing carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.17g/cm 3 26 percent of silicon carbide, 7 percent of silicon, 278MPa of compressive strength, 217MPa of bending strength and 70MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.30, the wear rate is 0.89 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.53, and the wet brake performance attenuation rate is 40%.
Comparative example 3 (CVD pyrolytic carbon coarse layer ratio > 50%, non-full smooth layer structure carbon)
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), weight percentage of the non-woven cloth and the thin net felt is 60:40, controlling the interlayer density to be 11 layers/cm, continuously needling in X and Y directions after layering is finished, controlling the row spacing and the interval of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.55g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 At a deposition pressure of 1.2kPa and at a deposition temperature of 990 in the chemical vapor depositionDEG C; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonization and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing twice by nitrogen, then filling nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.48g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing the carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon-ceramic brake material is 2.20g/cm 3 40 percent of silicon carbide, 1.5 percent of silicon, 290MPa of compressive strength, 232MPa of bending strength and 53MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.36, the wear rate is 1.53 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.42, and the wet braking performance attenuation rate is 18%.
Comparative example 4 (high content thin net felt prefabricated body structure)
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Ply), the weight percentage of the non-woven cloth and the thin net felt is 50:50, controlling the interlayer density to be 11 layers/cm, continuously needling after layering is completed in the X direction and the Y direction, controlling the row spacing and the space of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.45g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain the product with the density of 1.30g/cm 3 The deposition pressure is 1.5kPa, and the deposition temperature is 930 ℃ during the chemical vapor deposition; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix by using distilled water, then putting the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix by using a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: putting the dried and cooled carbon/carbon blank into a dipping kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the dipping kettle, dipping for 2 hours, pressurizing to 4MPa by using nitrogen, dipping for 2 hours, then decompressing, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonization and cracking: will be fixedPutting the blank after the carbonization into a carbonization furnace, vacuumizing and replacing the blank twice by nitrogen, then filling the nitrogen to the micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at the speed of 5 ℃/min, keeping the temperature for 3h to obtain the blank with the density of 1.53g/cm 3 The carbon/carbon porous body of (2).
Step four, preparing the carbon ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon ceramic brake material is 2.30g/cm 3 55% of silicon carbide, 2.6% of silicon, 298MPa of compressive strength, 237MPa of bending strength and 93MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.53, the wear rate is 0.83 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.79, and the wet braking performance attenuation rate is 19%.
COMPARATIVE EXAMPLE 5 (Low content thin row net felt precast body structure)
The method comprises the following steps: preparation of carbon fiber preform
Alternately laminating a layer of polypropylene-based carbon fiber (PANCF) laid cloth and a layer of polypropylene-based carbon fiber (PANCF) thin net felt (laid cloth 0) 0 /90 0 /270 0 Layering), wherein the weight percentage of the non-woven cloth to the thin net felt is 70:30, controlling the interlayer density to be 11 layers/cm, continuously needling after layering is completed in the X direction and the Y direction, controlling the row spacing and the space of needling to be 2.2 multiplied by 2.2mm, and controlling the needling density to be 25 needles/cm 2 Performing bidirectional puncture in Z direction with high thermal conductivity pitch carbon fiber (TYG) to obtain carbon fiber preform with Z-direction fiber row spacing and pitch of 5.0mmx5.0mm, and density of 0.75g/cm 3 。
Step two, preparation of carbon/carbon prefabricated body
Taking propylene as a carbon source and nitrogen as a diluent gas for the carbon fiber preform obtained in the step one, wherein the volume ratio of the propylene to the nitrogen is 1:1, carrying out chemical vapor deposition and heat treatment to obtain a density of 1.30g/cm 3 Carbon/carbon preform ofThe chemical vapor deposition is carried out under the deposition pressure of 1.5kPa and the deposition temperature of 930 ℃; the deposition time is 200h, the heat treatment temperature is 1600 ℃, and the heat treatment time is 2h.
Step three, preparation of carbon/carbon porous body
Preparation of the impregnant: adding bisphenol A epoxy resin into a preheating tank, heating to 40 ℃ in a water bath, and keeping the temperature for 1h. Then adding 30% of epoxy propane benzyl ether serving as a diluent, uniformly stirring, finally adding 24% of boron nitride ethylamine complex serving as a curing agent, and uniformly stirring.
Cleaning a carbon/carbon matrix: cleaning the carbon/carbon matrix with distilled water, then placing the carbon/carbon matrix into an ultrasonic cleaning machine for ultrasonic cleaning for 1h, and finally drying the carbon/carbon matrix with a hot air circulation drying box at the temperature of 120 ℃ for 6h.
Dipping and curing: and putting the dried and cooled carbon/carbon blank into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking the impregnant into the impregnation kettle, impregnating for 2 hours, pressurizing to 4MPa by using nitrogen, impregnating for 2 hours, relieving pressure, and discharging the impregnant. Then the temperature is increased to 150 ℃ to be cured for 6h.
Carbonizing and cracking: putting the solidified blank into a carbonization furnace, vacuumizing and replacing with nitrogen twice, then filling nitrogen to micro positive pressure (0-0.005) MPa, heating to 1200 ℃, heating at a rate of 5 ℃/min, keeping the temperature for 3h to obtain the product with the density of 1.45g/cm 3 The carbon/carbon porous body of (3).
Step four, preparing carbon-ceramic brake material
And (3) carrying out reaction infiltration and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material, wherein the purity of silicon used for the reaction infiltration is more than or equal to 99.0%, the particle size is less than or equal to 400 meshes, the reaction infiltration and siliconizing is carried out in a nitrogen atmosphere, the temperature of the reaction infiltration and siliconizing is 1900 ℃, the time of the reaction infiltration and siliconizing is 2 hours, and the pressure is 6000Pa.
The density of the prepared carbon ceramic brake material is 2.07g/cm 3 27% of silicon carbide, 0.8% of silicon, 261MPa of compressive strength, 228MPa of bending strength and 81MPa of shearing strength. The friction coefficient of the carbon-ceramic brake disc is 0.25, the wear rate is 1.14 mu m/surface/time, the peak-to-valley ratio of a friction curve is 1.41, and the wet brake performance attenuation rate is 11%.
TABLE 2 Performance results of the carbon-ceramic brake materials obtained in comparative examples 1 to 5
Note: in comparative example 5, the content of the simple substance silicon is only 0.8 percent and is lower than that of the embodiment, so the wet braking performance attenuation rate is lower than that of the embodiment, and the main reason of the wet braking performance attenuation of the simple substance silicon is fully explained.
Claims (10)
1. A preparation method of a low-abrasion carbon ceramic brake material is characterized by comprising the following steps: the method comprises the following steps:
step one preparation of a carbon fiber preform
Alternately laying a non-woven fabric and a thin net felt, continuously needling in X and Y directions, and then performing bidirectional puncture on asphalt-based carbon fibers in Z direction to obtain a carbon fiber preform, wherein the weight percentage of the non-woven fabric to the thin net felt in the carbon fiber preform is 58-62: 38 to 42;
step two, preparation of carbon/carbon prefabricated body
Carrying out chemical vapor deposition and heat treatment on the carbon fiber preform obtained in the step one by taking propylene as a carbon source and nitrogen as a diluent gas to obtain a carbon/carbon preform, wherein the deposition pressure is 1.4-1.8 kPa during the chemical vapor deposition, and the deposition temperature is 920-970 ℃;
step three, preparation of carbon/carbon porous body
Adding the carbon/carbon prefabricated body obtained in the second step into an impregnant for impregnation, then curing to obtain a cured prefabricated body, and then carbonizing and cracking to obtain a carbon/carbon porous body, wherein the impregnant consists of bisphenol A epoxy resin, epoxypropane benzyl ether and a boron nitride ethylamine complex compound, the mass fraction of the epoxypropane benzyl ether is 28-32%, and the mass fraction of the boron nitride ethylamine complex compound is 22-26%;
step four, preparing the carbon ceramic brake material
And (4) carrying out reaction, melting and siliconizing on the carbon/carbon porous body obtained in the step three to obtain the carbon-ceramic brake material.
2. The method for preparing a low-wear carbon-ceramic brake material as claimed in claim 1, wherein the method comprises the following steps: in the first step, the non-woven cloth and the thin net felt are alternately layered, the density between layers is controlled to be 11-15 layers/cm, then continuous needling is carried out in the X and Y directions, the row spacing and the interval of the needling are controlled to be 2.0-2.4 multiplied by 2.0-2.4 mm, and the needling density is 20-25 needles/cm 2 And then, performing bidirectional puncture by using pitch-based carbon fibers in the Z direction, wherein the row spacing and the interval of the puncture are controlled to be 4.8-5.2 multiplied by 4.8-5.2 mm, and thus obtaining the carbon fiber preform.
3. The method for preparing a low-wear carbon-ceramic brake material as claimed in claim 1, wherein the method comprises the following steps: in the first step, the density of the carbon fiber preform is 0.50-0.60 g/cm 3 。
4. The preparation method of the low-wear carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: in the second step, the volume ratio of the propylene to the nitrogen is 0.8-1.2: 0.8 to 1.2;
in the second step, the deposition temperature is 930-960 ℃ and the deposition time is 180-220 h during the chemical vapor deposition.
5. The preparation method of the low-wear carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: in the second step, the temperature of the heat treatment is 1500-1800 ℃, and the time of the heat treatment is 1-3 h;
in the second step, the density of the carbon/carbon preform is 1.30-1.33 g/cm 3 。
6. The method for preparing a low-wear carbon-ceramic brake material as claimed in claim 1, wherein the method comprises the following steps: in the third step, the impregnant is obtained by the following steps: firstly, keeping the temperature of bisphenol A epoxy resin at 35-45 ℃ for 0.5-1 h, then adding epoxypropane benzyl ether, stirring uniformly, and finally adding boron nitride ethylamine complex and stirring uniformly to obtain the bisphenol A epoxy resin;
and in the third step, the impregnation process comprises the steps of putting the carbon/carbon prefabricated body into an impregnation kettle, vacuumizing until the pressure is less than 100Pa, then sucking an impregnant into the impregnation kettle, impregnating for 1-2 h, pressurizing to 3-5 MPa by using nitrogen, and impregnating for 1-2 h.
7. The method for preparing a low-wear carbon-ceramic brake material as claimed in claim 1, wherein the method comprises the following steps: in the third step, the curing temperature is 120-180 ℃, and the curing time is 4-6 h; the curing is carried out at atmospheric pressure.
8. The preparation method of the low-wear carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: in the third step, the carbonization cracking temperature is 1100-1200 ℃, the heat preservation time is 2-3 h, the heating rate is 3-5 ℃/min, and the pressure is 0-0.005 MPa.
9. The preparation method of the low-wear carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: in the fourth step, the purity of the silicon used for reaction infiltration is more than or equal to 99.0 percent, and the grain diameter is less than or equal to 400 meshes;
in the fourth step, the reaction infiltration silicon is carried out in nitrogen atmosphere, the temperature of the reaction infiltration silicon is 1850-2100 ℃, the time of the reaction infiltration silicon is 2-3 h, preferably 2h, and the pressure is 6000-8000 Pa.
10. The carbon-ceramic brake material prepared by the preparation method according to any one of claims 1 to 9.
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| WO2018222569A1 (en) * | 2017-05-31 | 2018-12-06 | Brilliant Light Power, Inc. | Magnetohydrodynamic electric power generator |
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| CN113248272A (en) * | 2021-05-11 | 2021-08-13 | 广州三的投资管理企业（有限合伙） | Preparation method and application of carbon-ceramic friction material |
| CN113915021A (en) * | 2021-09-29 | 2022-01-11 | 湖北瑞宇空天高新技术有限公司 | Cylindrical prefabricated body, light high-temperature-resistant composite piston and preparation method thereof |
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| CN115724677A (en) * | 2022-11-25 | 2023-03-03 | 贵州省紫安新材料科技有限公司 | Preparation method of carbon-metal fiber mixed carbon-ceramic brake disc |
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