CN108530096B - Preparation method of carbon-based automobile brake pair - Google Patents
Preparation method of carbon-based automobile brake pair Download PDFInfo
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- CN108530096B CN108530096B CN201810426828.1A CN201810426828A CN108530096B CN 108530096 B CN108530096 B CN 108530096B CN 201810426828 A CN201810426828 A CN 201810426828A CN 108530096 B CN108530096 B CN 108530096B
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- C04B35/806—
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- 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—Compositions of linings; Methods of manufacturing
- F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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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
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0034—Materials; Production methods therefor non-metallic
- F16D2200/0052—Carbon
Abstract
The invention belongs to the field of manufacturing of carbon-based composite materials, and relates to a preparation method of a carbon-based automobile brake pair. The invention comprises the following steps: step 1, performing high-temperature heat treatment on a carbon fiber preform; step 2, CVD deposition; step 3, intermediate high-temperature heat treatment; step 4, fine machining; step 5, RMI densification process; and 6, finally carrying out high-temperature heat treatment. The invention adopts the long fiber integral needled felt as a prefabricated body, and prepares the high-performance carbon-based automobile brake pair through CVD densification and reactive melt impregnation densification, and the brake pair has stable brake performance and high safety and reliability.
Description
Technical Field
The invention belongs to the field of manufacturing of carbon-based composite materials, and relates to a preparation method of a carbon-based automobile brake pair.
Background
At present, the brake materials widely applied to high-speed trains, racing cars and airplanes mainly adopt powder metallurgy materials and carbon-carbon composite materials. However, the powder metallurgy brake material is easy to generate the phenomena of high-temperature bonding, friction performance recession, high-temperature mechanical performance attenuation, short service life and the like in the high-temperature use process; the carbon-carbon composite material has the problems of low wet friction coefficient, morning sickness, long production period and high production cost, and the development of the carbon-carbon composite material is restricted. Therefore, a new generation of carbon/ceramic brake materials developed in recent years is a multiphase composite brake material using high strength carbon fibers as a reinforcement and pyrolytic carbon, modified powder, etc. as a matrix, and having a low density (about 2.0 g/cm)3) High friction factor, stable braking, corrosion resistance, oxidation resistance, high temperature resistance, long service life and the like, and the material also has higher static friction coefficient and has the advantages of severe environment (moisture, mould, oil stain and the like)) The braking performance has better stability. Researchers at units such as German Stuttgart university and German aerospace research institute developed a carbon fiber reinforced carbon-ceramic based composite brake pair applied to a Porsche car; carbon fiber reinforced ceramic matrix composite brake shoes have been tried in japan newstem.
The automobile brake pair is a structure/function integrated material, and has good frictional wear performance and thermal performance and sufficiently high mechanical performance. Compared with an airplane brake pair, the material prepared by the automobile brake pair is consistent with the airplane brake pair. However, the braking mode, the frictional wear performance and the opposite-grinding material of the automobile brake pair are different, namely the automobile brake pair is a caliper brake, namely the brake pair and a brake pad are opposite-ground, and the friction area of the brake pad is only about 20% of the area of the brake pair; the carbon-based automobile brake pair is a carbon-based brake pair and is opposite to the brake pad made of other materials, and the abrasion of the brake pair is required to be far less than that of the brake pad. Therefore, compared with the severe requirement of the airplane brake pair, the automobile brake pair has lower cost and performance requirements under the condition of ensuring safety.
At present, the mainstream methods for preparing carbon brake pairs at home and abroad are a Chemical Vapor Infiltration (CVI) process and a resin impregnation-carbonization process. The two processes have the defects of low carbon deposition efficiency, easy surface incrustation, overlong production period, high process cost and the like. A master academic paper of the university of China & south China, namely preparation and performance research of a C/C-SiC composite material for automobile braking, researches a preparation method of an automobile brake pad, and the method takes short fibers as raw materials to prepare the C/C-SiC composite material brake pad by a compression molding-reaction sintering method, and has the advantages of short preparation period, good decay resistance, low mechanical property and high material wear rate. Secondly, a paper "rapidly preparing different prefabricated C/C composite material tribology performance research" of the solid rocket technology, 2008 4 th 31 th curling chart describes a method for preparing a C/C composite material by using a rapid CVI process and using a short fiber molded felt as a prefabricated body. Compared with a carbon cloth laminated prefabricated body structure, the method improves the frictional wear performance of the material. But compared with the invention, the finished product of the C/C composite material has low density, long production period, poor mechanical property and low friction property.
Disclosure of Invention
In order to overcome the defects of the traditional CVI process and the technology for preparing the carbon brake pair by the resin impregnation-carbonization process, the CVI process comprises the steps of firstly carrying out high-temperature thermal treatment on a porous prefabricated body such as carbon fiber and the like, then putting the porous prefabricated body into a chemical vapor deposition furnace, introducing carbon source gas for cracking at a certain temperature and pressure, and continuously depositing the generated carbon into pores of the prefabricated body to gradually densify the prefabricated body, but has the defects of low carbon deposition efficiency, easy surface crusting and overlong production period. In order to further increase the bulk density of the green body, the resin impregnation-carbonization process needs to be repeatedly densified, which results in a significant increase in the cost of the subsequent process. The invention provides a preparation method of a carbon brake pair, which has a short production period and more excellent mechanical properties.
The technical scheme of the invention is as follows: a preparation method of a carbon-based automobile brake pair comprises the following steps:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Putting the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, heating to the deposition temperature of 950-1020 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 120 SLM-180 SLM, the propane flow is 25 SLM-55 SLM, the hearth pressure is 1 KPa-5 KPa, the deposition time is 450 h-550 h, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
And putting the semi-finished automobile brake pair into a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace. The adding amount of the silicon powder is calculated as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained in the step 4. And flatly paving the semi-finished automobile brake pair on the silicon powder and lightly pressing, and stacking a plurality of graphite crucibles filled with the silicon powder and the semi-finished automobile brake pair in a high-temperature vacuum furnace. Vacuumizing to less than or equal to 1KPa, keeping the vacuum for 12h, heating to the deposition temperature of 1600-1800 ℃ and keeping the temperature for 2-3 h, wherein the vacuum degree is less than or equal to 2 KPa. And discharging the product after the dipping is finished, performing surface processing by adopting a mechanical processing method, and weighing and measuring density. Continuously densifying the workpiece with low density according to the process in the step 5 to finally obtain the workpiece with the density of 1.80g/cm3～2.10g/cm3The semi-finished product of the automobile brake pair.
Step 6, final high temperature heat treatment
Placing the semi-finished product of the automobile brake pair into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; continuously heating to 1600-2000 ℃, and preserving heat for 1-4 h for high-temperature heat treatment.
The invention adopts long fiber integral needled felt as a prefabricated body, and prepares the high-performance carbon-based automobile brake pair through CVD densification and densification of a reaction melting impregnation process. Compared with the traditional CVI process and the resin impregnation-carbonization process, the long fiber integrally needled felt plus the CVD process plus the melt impregnation process has the initial porosity of 60-70 percent, belongs to a porous carbon-based composite material, and can be quickly compacted to the density of more than or equal to 1.42g/cm through the CVD process3The semi-finished product with the porosity of 25-35 percent finally permeates into the C/C composite material by utilizing the molten silicon under the action of capillary force to generate a SiC ceramic matrix, and finally the density is more than or equal to 1.80g/cm3And (4) obtaining a finished product. Not only the preparation period is greatly shortened (Table 1), but also the composite material has excellent performanceThe toughness and strength of (D) are shown in Table 2.
TABLE 1 preparation periods of the different processes
TABLE 2 Properties of samples of different preparation methods
When the sample is subjected to a friction wear test on an MM1000-II type friction wear testing machine, when the brake pressure is 0.8MPa, the rotating speed is 8579r/min, and the inertia is 0.210Kgm2The radius of the sample is 33mm, and the friction area is 2220mm2And the braking times are 30 times, the braking curve is stable, and the friction surface of the sample is smooth. The simulated brake test results are shown in table 3, and the test results show that the average friction coefficient range of the 5 batches of samples is 0.314-0.425, the wear rate is 0.0022-0.0026 mm per time surface, the fluctuation range of the friction coefficient and the wear rate among different batches is small, and the friction and wear performance is stable.
Average coefficient of friction and wear rate for the samples in Table 35
In addition, referring to fig. 3, the bench test for carbon-based automobile brake pair product of the present invention is performed on a LINK3000 heavy-duty automobile brake test bench manufactured by LINK engineering technology corporation in the united states of america, and the test is performed according to the automobile brake performance test method (GB 12676 + 1999) with reference to the technical conditions of the model of SUBARU WRX STI FRONT 150111. The test result shows that the friction coefficient of the brake pair is in a slow rising trend along with the increase of the brake pressure in the whole brake speed interval, the fluctuation range of the average friction coefficient in different brake speed intervals is small, the brake surface is smooth, and the carbon-based automobile brake pair is stable in brake performance and high in safety and reliability.
Drawings
FIG. 1 is a schematic diagram of the preparation of RMI in step 5 of the present invention, wherein: 1. graphite paper; 2. a green body; 3. a crucible; 4. silicon powder; 5. a graphite paper gasket;
FIG. 2 is a flow chart of the present invention;
FIG. 3 is a trend chart of test data of a large sample rack of a carbon-based automobile brake pair.
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings.
Example 1
The embodiment is a preparation method of a carbon-based automobile brake pair, and referring to fig. 2, the specific process is as follows:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Placing the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, heating to the deposition temperature of 950 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 120SLM, the propane flow is 25SLM, the hearth pressure is 1KPa, the deposition time is 450 hours, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
Adding the fine powderThe semi-finished product of the automobile brake pair is placed in a graphite crucible filled with silicon powder, and silicon melting infiltration is carried out in a high-temperature vacuum furnace, wherein the granularity of the silicon powder is 320 meshes. The adding amount of the silicon powder is as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained after the treatment in the step 4.
And flatly paving the semi-finished product of the automobile brake pair on the silicon powder and lightly pressing.
And stacking a plurality of graphite crucibles filled with silicon powder and semi-finished automobile brake pair products in a high-temperature vacuum furnace.
And vacuumizing the high-temperature vacuum furnace to be less than or equal to 1KPa, and keeping the vacuum for 12 hours, wherein the vacuum degree of the high-temperature vacuum furnace is less than or equal to 2 KPa. And heating the high-temperature vacuum furnace to the deposition temperature of 1600 ℃, and preserving the heat for 2.5 hours. And finishing the impregnation of the semi-finished product of the automobile brake pair after the heat preservation is finished.
And discharging the product after the dipping is finished, performing surface processing by adopting a conventional mechanical processing method, weighing and measuring density. Continuing to dip the workpiece with low density according to the process to obtain the workpiece with the density of more than or equal to 1.80g/cm3The semi-finished product of the automobile brake pair.
And 6, performing high-temperature heat treatment.
And putting the semi-finished product of the automobile brake pair into a heat treatment furnace. Vacuumizing the heat treatment furnace to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; and continuously heating to 1600 ℃, and preserving the heat for 2h for high-temperature heat treatment.
Example 2
The embodiment is a preparation method of a carbon-based automobile brake pair, which comprises the following specific processes:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Placing the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, and heating to the deposition temperature of 9 DEG CIntroducing natural gas and propane at 70 ℃ for deposition, wherein the natural gas flow rate is 135SLM, the propane flow rate is 32SLM, the hearth pressure is 2KPa, the deposition time is 480h, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
And (3) placing the finely processed semi-finished automobile brake pair into a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace, wherein the granularity of the silicon powder is 320 meshes. The adding amount of the silicon powder is as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained after the treatment in the step 4.
And flatly paving the semi-finished product of the automobile brake pair on the silicon powder and lightly pressing.
And stacking a plurality of graphite crucibles filled with silicon powder and semi-finished automobile brake pair products in a high-temperature vacuum furnace.
And vacuumizing the high-temperature vacuum furnace to be less than or equal to 1KPa, and keeping the vacuum for 12 hours, wherein the vacuum degree of the high-temperature vacuum furnace is less than or equal to 2 KPa. And the high-temperature vacuum furnace is heated to the deposition temperature of 1650 ℃, and the temperature is kept for 2.5 h. And finishing the impregnation of the semi-finished product of the automobile brake pair after the heat preservation is finished.
And discharging the product after the dipping is finished, performing surface processing by adopting a conventional mechanical processing method, weighing and measuring density. Continuing to dip the workpiece with low density according to the process to obtain the workpiece with the density of more than or equal to 1.80g/cm3The semi-finished product of the automobile brake pair.
And 6, performing high-temperature heat treatment.
And putting the semi-finished product of the automobile brake pair into a heat treatment furnace. Vacuumizing the heat treatment furnace to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; and continuously heating to 1600 ℃, and preserving the heat for 2h for high-temperature heat treatment.
Example 3
The embodiment is a preparation method of a carbon-based automobile brake pair, which comprises the following specific processes:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Placing the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, heating to the deposition temperature of 990 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 150SLM, the propane flow is 39SLM, the hearth pressure is 3KPa, the deposition time is 510 hours, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
And (3) placing the finely processed semi-finished automobile brake pair into a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace, wherein the granularity of the silicon powder is 320 meshes. The adding amount of the silicon powder is as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained after the treatment in the step 4.
And flatly paving the semi-finished product of the automobile brake pair on the silicon powder and lightly pressing.
And stacking a plurality of graphite crucibles filled with silicon powder and semi-finished automobile brake pair products in a high-temperature vacuum furnace.
And vacuumizing the high-temperature vacuum furnace to be less than or equal to 1KPa, and keeping the vacuum for 12 hours, wherein the vacuum degree of the high-temperature vacuum furnace is less than or equal to 2 KPa. And heating the high-temperature vacuum furnace to the deposition temperature of 1700 ℃, and preserving the heat for 2.5 hours. And finishing the impregnation of the semi-finished product of the automobile brake pair after the heat preservation is finished.
And discharging the product after the dipping is finished, performing surface processing by adopting a conventional mechanical processing method, weighing and measuring density. Continuing to dip the workpiece with low density according to the process to obtain the workpiece with the density of more than or equal to 1.80g/cm3The semi-finished product of the automobile brake pair.
And 6, performing high-temperature heat treatment.
And putting the semi-finished product of the automobile brake pair into a heat treatment furnace. Vacuumizing the heat treatment furnace to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; and continuously heating to 1600 ℃, and preserving the heat for 2h for high-temperature heat treatment.
Example 4
The embodiment is a preparation method of a carbon-based automobile brake pair, which comprises the following specific processes:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Placing the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, heating to the deposition temperature of 1010 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 165SLM, the propane flow is 46SLM, the hearth pressure is 4KPa, the deposition time is 530 hours, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
And (3) placing the finely processed semi-finished automobile brake pair into a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace, wherein the granularity of the silicon powder is 320 meshes. The adding amount of the silicon powder is as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained after the treatment in the step 4.
And flatly paving the semi-finished product of the automobile brake pair on the silicon powder and lightly pressing.
And stacking a plurality of graphite crucibles filled with silicon powder and semi-finished automobile brake pair products in a high-temperature vacuum furnace.
And vacuumizing the high-temperature vacuum furnace to be less than or equal to 1KPa, and keeping the vacuum for 12 hours, wherein the vacuum degree of the high-temperature vacuum furnace is less than or equal to 2 KPa. And raising the temperature of the high-temperature vacuum furnace to 1750 ℃ of deposition temperature, and preserving the heat for 2.5 hours. And finishing the impregnation of the semi-finished product of the automobile brake pair after the heat preservation is finished.
And discharging the product after the dipping is finished, performing surface processing by adopting a conventional mechanical processing method, weighing and measuring density. Continuing to dip the workpiece with low density according to the process to obtain the workpiece with the density of more than or equal to 1.80g/cm3The semi-finished product of the automobile brake pair.
And 6, performing high-temperature heat treatment.
And putting the semi-finished product of the automobile brake pair into a heat treatment furnace. Vacuumizing the heat treatment furnace to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; and continuously heating to 1600 ℃, and preserving the heat for 2h for high-temperature heat treatment.
Example 5
The embodiment is a preparation method of a carbon-based automobile brake pair, which comprises the following specific processes:
Placing the carbon fiber preform into a heat treatment furnace, vacuumizing to less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment.
Placing the carbon fiber preform subjected to the heat treatment into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1KPa, maintaining the pressure for 12 hours, heating to the deposition temperature of 1020 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 180SLM, the propane flow is 55SLM, the hearth pressure is 5KPa, the deposition time is 550 hours, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
Placing the carbon fiber preform densified by CVD into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1KPa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; and continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair.
And (4) machining the carbon brake pair semi-finished product.
And (3) placing the finely processed semi-finished automobile brake pair into a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace, wherein the granularity of the silicon powder is 320 meshes. The adding amount of the silicon powder is as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank. M isBlankAnd 4, weighing the semi-finished product of the automobile brake pair obtained after the treatment in the step 4.
And flatly paving the semi-finished product of the automobile brake pair on the silicon powder and lightly pressing.
And stacking a plurality of graphite crucibles filled with silicon powder and semi-finished automobile brake pair products in a high-temperature vacuum furnace.
And vacuumizing the high-temperature vacuum furnace to be less than or equal to 1KPa, and keeping the vacuum for 12 hours, wherein the vacuum degree of the high-temperature vacuum furnace is less than or equal to 2 KPa. And the high-temperature vacuum furnace is heated to the deposition temperature of 1800 ℃ and is kept for 2.5 hours. And finishing the impregnation of the semi-finished product of the automobile brake pair after the heat preservation is finished.
Discharging after the dipping is finished, and adopting the conventional methodThe machining method of (3) is to perform surface machining and weigh and measure the density. Continuing to dip the workpiece with low density according to the process to obtain the workpiece with the density of more than or equal to 1.80g/cm3The semi-finished product of the automobile brake pair.
And 6, performing high-temperature heat treatment.
And putting the semi-finished product of the automobile brake pair into a heat treatment furnace. Vacuumizing the heat treatment furnace to less than or equal to 1KPa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; and continuously heating to 1600 ℃, and preserving the heat for 2h for high-temperature heat treatment.
Claims (6)
1. A preparation method of a carbon-based automobile brake pair is characterized by comprising the following steps:
step 1, performing high-temperature heat treatment on the carbon fiber preform:
placing the carbon fiber preform into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1k Pa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; continuously heating to 2100 ℃, and preserving heat for 4 hours for heat treatment;
step 2, CVD deposition:
placing the carbon fiber preform subjected to the heat treatment in the step 1 into a chemical vapor deposition furnace, vacuumizing to be less than or equal to 1k Pa, maintaining the pressure for 12h, heating to the deposition temperature of 950-1020 ℃, introducing natural gas and propane for deposition, wherein the natural gas flow is 120 SLM-180 SLM, the propane flow is 25 SLM-55 SLM, the hearth pressure is 1k Pa-5 k Pa, the deposition time is 450 h-550 h, and the obtained density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product;
step 3, intermediate high-temperature heat treatment:
putting the carbon fiber preform densified in the step 2 into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1k Pa, and heating; when the temperature is raised to 1400 ℃, Ar is filled for protection; continuously heating to 2100 ℃, and preserving heat for 4 hours to carry out heat treatment to obtain a semi-finished product of the carbon brake pair;
step 4, fine machining:
machining the carbon brake pair semi-finished product;
step 5, RMI densification:
finish machining the automobile in the step 4Placing the semi-finished brake pair in a graphite crucible filled with silicon powder, and carrying out silicon melting infiltration in a high-temperature vacuum furnace; the adding amount of the silicon powder is calculated as follows: the addition amount of silicon powder/g is 1.3mBlank～1.5mBlank(ii) a M isBlankThe weight of the semi-finished product of the automobile brake pair obtained in the step 4; flatly paving the semi-finished automobile brake pair on the silicon powder and lightly pressing, and stacking a plurality of graphite crucibles filled with the silicon powder and the semi-finished automobile brake pair in a high-temperature vacuum furnace; vacuumizing to less than or equal to 1k Pa, keeping the vacuum degree to less than or equal to 2k Pa after 12h of vacuum, heating to the deposition temperature of 1600-1800 ℃, and keeping the temperature for 2-3 h; discharging after the dipping is finished, performing surface processing by adopting a mechanical processing method, weighing and measuring density; continuously densifying the workpiece with low density according to the process in the step 5 to finally obtain the workpiece with the density of 1.80g/cm3～2.10g/cm3The semi-finished product of the automobile brake pair;
and 6, final high-temperature heat treatment:
placing the semi-finished product of the automobile brake pair processed in the step 5 into a heat treatment furnace, vacuumizing until the pressure is less than or equal to 1k Pa, and heating; when the temperature is raised to 1000 ℃, Ar is filled for protection; continuously heating to 1600-2000 ℃, and preserving heat for 1-4 h for high-temperature heat treatment.
2. The method for preparing a carbon-based automobile brake pair according to claim 1, wherein the method comprises the following steps: in the step 2, the carbon fiber preform subjected to the heat treatment in the step 1 is placed in a chemical vapor deposition furnace, the carbon fiber preform is vacuumized to be less than or equal to 1k Pa, the pressure is maintained for 12 hours, the temperature is raised to 950 ℃ of deposition temperature, natural gas and propane are introduced for deposition, the natural gas flow is 120SLM, the propane flow is 25SLM, the hearth pressure is 1k Pa, the deposition time is 450 hours, and the density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
3. The method for preparing a carbon-based automobile brake pair according to claim 1, wherein the method comprises the following steps: in the step 2, the carbon fiber preform subjected to the heat treatment in the step 1 is placed in a chemical vapor deposition furnace, the carbon fiber preform is vacuumized to be less than or equal to 1k Pa, the pressure is maintained for 12 hours, the temperature is increased to 970 ℃ of deposition temperature, natural gas and propane are introduced for deposition, and the natural gas flow rate is 135SLM, propane flow rate 32SLM, hearth pressure 2k Pa, deposition time 480h and density 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
4. The method for preparing a carbon-based automobile brake pair according to claim 1, wherein the method comprises the following steps: in the step 2, the carbon fiber preform subjected to the heat treatment in the step 1 is placed in a chemical vapor deposition furnace, the carbon fiber preform is vacuumized to be less than or equal to 1k Pa, the pressure is maintained for 12 hours, the temperature is raised to a deposition temperature of 990 ℃, natural gas and propane are introduced for deposition, the natural gas flow is 150SLM, the propane flow is 39SLM, the hearth pressure is 3k Pa, the deposition time is 510 hours, and the density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
5. The method for preparing a carbon-based automobile brake pair according to claim 1, wherein the method comprises the following steps: in the step 2, the carbon fiber preform subjected to the heat treatment in the step 1 is placed in a chemical vapor deposition furnace, the carbon fiber preform is vacuumized to be less than or equal to 1k Pa, the pressure is maintained for 12 hours, the temperature is raised to be 1010 ℃, natural gas and propane are introduced for deposition, the natural gas flow is 165SLM, the propane flow is 46SLM, the hearth pressure is 4k Pa, the deposition time is 530 hours, and the density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
6. The method for preparing a carbon-based automobile brake pair according to claim 1, wherein the method comprises the following steps: in the step 2, the carbon fiber preform subjected to the heat treatment in the step 1 is placed in a chemical vapor deposition furnace, the carbon fiber preform is vacuumized to be less than or equal to 1k Pa, the pressure is maintained for 12 hours, the temperature is raised to be 1020 ℃ of deposition temperature, natural gas and propane are introduced for deposition, the natural gas flow is 180SLM, the propane flow is 55SLM, the hearth pressure is 5k Pa, the deposition time is 550 hours, and the density is 1.42g/cm3～1.50g/cm3The carbon brake pair semi-finished product.
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| CN115231938A (en) * | 2022-07-22 | 2022-10-25 | 常州翊翔炭材科技有限公司 | Preparation method of carbon/carbon composite material brake disc |
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