CN115773321B - High-strength carbon/ceramic brake disc with ceramic functional layer - Google Patents
High-strength carbon/ceramic brake disc with ceramic functional layer Download PDFInfo
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- CN115773321B CN115773321B CN202310101877.9A CN202310101877A CN115773321B CN 115773321 B CN115773321 B CN 115773321B CN 202310101877 A CN202310101877 A CN 202310101877A CN 115773321 B CN115773321 B CN 115773321B
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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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/528—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B35/71—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
- C04B35/83—Carbon fibres in a carbon matrix
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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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
- F16D65/00—Parts or details
- F16D65/02—Braking members; Mounting thereof
- F16D65/12—Discs; Drums for disc brakes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Braking Arrangements (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a high-strength carbon/ceramic brake disc with a ceramic functional layer, and belongs to the technical field of vehicle brake parts. Firstly, carrying out high-temperature graphitization treatment on a carbon/carbon blank body of a binary carbon matrix, preparing the graphitized carbon/carbon blank body of the binary carbon matrix into a carbon/ceramic brake disc blank body through a liquid phase silicon infiltration reaction, and forming a ceramic functional layer through in-situ reaction of ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank body to obtain the brake disc; the carbon/carbon blank with the binary carbon matrix can effectively protect carbon fibers from being corroded by silicon liquid and reduce the proportion of residual silicon, and the ceramic functional layer formed by in-situ reaction has good binding force with the matrix and adjustable thickness. The brake disc has the characteristics of high mechanical strength, high friction coefficient, low wear rate, good oxidation resistance and long service life, and has good application prospect.
Description
Technical Field
The invention relates to a high-strength carbon/ceramic brake disc with a ceramic functional layer, and belongs to the technical field of vehicle brake parts.
Background
The carbon/ceramic composite material is a carbon fiber reinforced carbon and silicon carbide ceramic matrix composite material, and is produced as a thermal structural material in the 80 th century at the earliest, has low density, good oxidation resistance, corrosion resistance, excellent high-temperature mechanical property and thermal physical property, and is a novel high-temperature structural material and functional material capable of meeting the use at 1650 ℃. The carbon/ceramic composite material has the advantages of abrasion resistance, high temperature resistance, small density, large heat capacity, stable wet friction performance, no attenuation of high-temperature friction coefficient and the like when being used as a brake material, and can be a first-choice brake material for new-generation automobiles, high-speed rails, airplanes, tanks and the like.
German patent DE 19727585 A1 discloses a combination of a chopped-fiber-reinforced C/SiC ceramic brake disc, which is formed from chopped carbon fibers by compression molding followed by a ceramming treatment, and a brake lining, which is formed from a sintered metal material or a non-organic binding material with a ceramic binding phase and metal particles. Chinese patent CN113548902 a discloses a method for preparing a carbon fiber reinforced silicon carbide brake disc, which comprises the steps of performing heat treatment on chopped carbon fibers, uniformly mixing chopped carbon fibers with resin and additives, molding in a molding press, performing high-temperature pyrolysis under nitrogen or inert gas protection atmosphere, and performing silicon infiltration in a vacuum infiltration furnace to obtain the carbon fiber reinforced silicon carbide brake disc. The carbon/ceramic brake disc produced by the method has insufficient mechanical strength, and is easy to crack and lose efficacy when being impacted by hard objects in the use process.
U.S. patent No. 7445095"braking system having a composite-material brake disc" discloses a combination of a carbon/ceramic brake disc with a friction layer and a composite brake pad, wherein the friction coefficient is 0.4-0.48, and the friction performance is excellent. The surface friction layer contains a large amount of chopped carbon fibers, the temperature of the friction surface of the brake disc rises rapidly during braking, the carbon fibers are oxidized and lose strength at high temperature, the abrasion rate of the brake disc is increased, and the service life is short.
Chinese patent CN105565839 a discloses a method for preparing a carbon/ceramic brake material and a method for preparing a carbon/ceramic brake disc. Adding ceramic powder into phenolic resin solution to obtain a mixture, impregnating the mixture into a carbon fiber blank, carbonizing to obtain a porous carbon/carbon-ceramic powder composite material, and carrying out siliconizing treatment in a vacuum furnace after mechanical processing to obtain the carbon/ceramic brake disc. The problem is that the porous carbon/carbon-ceramic powder composite material is difficult to machine; the carbon fiber used as the reinforcement lacks surface protection, and silicon can cause erosion damage to the fiber during siliconizing treatment, so that the mechanical strength of the brake disc is insufficient.
Chinese patent CN111892416 a discloses a method for preparing a carbon/ceramic brake material, which comprises placing a low-density carbon/carbon blank in silica powder impregnating slurry, drying after impregnation, loading the impregnated carbon/carbon blank into a siliconizing furnace, and carrying out in situ melting chemical reaction between silica powder in the carbon blank and deposited carbon on the surface of the blank at high temperature to form a SiC ceramic phase. The problem is that the silicon powder of the carbon/carbon blank body impregnated by the silicon powder impregnating slurry is concentrated on the outer layer, the silicon powder content is gradually decreased from inside to outside, so that the ceramic brake disc material is uneven, the residual silicon on the outer layer is too much, the SiC ceramic content on the inner layer is too low, and the braking performance is affected.
Chinese patent CN 113277869A discloses a carbon/ceramic brake disc with wear-resistant and oxidation-resistant coating and a preparation method thereof, wherein wear-resistant slurry containing 60% of SiC particles is brushed in a groove formed in advance on a carbon/carbon blank body, then a vapor deposition siliconizing process is adopted for coating, silica powder is not contacted with the carbon/carbon composite material disc body, and the distance between the silica powder and the carbon/carbon composite material disc body is more than or equal to 100mm. The problem is that the coating introduced by the evaporation process is thinner, cannot play a long-term wear-resisting role, and can only play an antioxidant role; the SiC particles with higher proportion in the slurry are not generated by in-situ reaction, have weak binding force with a matrix, are easy to fall off in the friction process, and cannot form a stable friction film on a friction surface, so that the wear rate of a brake disc and a dual brake pad is higher.
Chinese patent CN108299002 a discloses a C/C-SiC ventilating brake disc with silicon carbide friction function layerThe patent is directed to a process for the preparation thereof by the reaction of trichlorosilane (CH 3 SiCl 3 ) The gas phase siliconizing method uses silicon steam to react with the carbon/carbon blank to generate silicon carbide, the carbon/ceramic composite material brake disc blank is obtained, and then a layer of pure silicon carbide is deposited on the surface of the carbon/ceramic brake disc blank through a CVI process, so that a friction functional layer is formed. The carbon/ceramic brake disc prepared by the method has the advantages of high raw material cost, long preparation period and low cost performance of the brake disc.
Chinese patent CN110131343 a discloses a method for preparing an automobile brake disc, which comprises preparing an automobile brake auxiliary preform by an integral molding and compression molding process, using a polysilazane solution and a polycarbosilane solution as ceramic precursors, and obtaining a ceramic matrix by repeated impregnation-pyrolysis, thus finally preparing the carbon fiber reinforced carbon-based/ceramic-based composite material. The method has low preparation efficiency, high cost and large difficulty in industrialized application.
Disclosure of Invention
Aiming at the problems of the prior brake disc, the invention provides the high-strength carbon/ceramic brake disc with the ceramic functional layer, which is characterized in that pyrolytic carbon wrapping carbon fibers and resin carbon or asphalt carbon filling pores are introduced into a carbon fiber preform to form a carbon/carbon blank of a binary carbon matrix, silicon preferentially reacts with the resin carbon or the asphalt carbon to generate SiC in the subsequent liquid phase siliconizing process, and the pyrolytic carbon effectively protects the carbon fibers from being corroded by silicon liquid, so that the strength retention rate of the carbon fibers is higher, and the high mechanical strength of the brake disc is ensured; the ceramic functional layer generated through in-situ reaction has good binding force with a substrate, adjustable thickness and can effectively play a comprehensive role of wear resistance, oxidation resistance and friction coefficient improvement, so that the brake disc has the characteristics of high mechanical strength, high friction coefficient, low wear rate, good oxidation resistance and long service life, can be used on conventional automobiles, airplanes and high-speed rails, and can also meet the use requirements of extreme braking environments such as high-performance racing automobiles, heavy trucks and tanks.
The aim of the invention is achieved by the following technical scheme.
The high-strength carbon/ceramic brake disc with the ceramic functional layer is prepared by performing high-temperature graphitization treatment on a carbon/carbon blank of a binary carbon matrix, preparing the graphitized carbon/carbon blank of the binary carbon matrix into a carbon/ceramic brake disc blank through a liquid phase silicon infiltration reaction, and forming the ceramic functional layer through an in-situ reaction of a ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank to obtain the brake disc;
the carbon/carbon blank of the binary carbon matrix is prepared by coating pyrolytic carbon on the surface of carbon fiber of a carbon fiber preform by utilizing a chemical vapor deposition process, and filling resin carbon or asphalt carbon in the pores of the carbon fiber preform by utilizing an impregnation carbonization process; wherein the carbon fiber preform is formed by needling carbon fibers and a carbon net tire and has a density of 0.4-0.6 g/cm 3 The density of the coated pyrolytic carbon is increased to 0.8-1.3 g/cm 3 The density of the resin carbon or asphalt carbon is continuously increased to 1.0-1.5 g/cm 3 Correspondingly, the density of the carbon/ceramic brake disc blank is 1.9-2.4 g/cm 3 ；
The ceramic precursor glue solution is prepared from thermosetting resin, polymethyl silane and silicon powder according to the following proportion of 30: (15-40): (30-55) by mass ratio; the thermosetting resin is preferably phenolic resin, epoxy resin or furfuryl ketone resin, and the thermosetting resin, polymethyl silane and silicon powder are preferably mixed for 0.5-2 hours after being mixed.
The carbon fiber preform may be prepared by the steps of: spreading carbon fiber and pre-needling the carbon net tire to form a carbon fiber-carbon net tire unit layer, spreading a plurality of carbon fiber-carbon net tire unit layers layer by layer on a flat needling machine to form a 2.5D carbon fiber flat felt in a relay needling mode, and cutting according to the size of a brake disc to obtain a carbon fiber preform.
The carbon fiber is preferably 12-48K carbon fiber, wherein K represents the thousand of tows; in the needling process of the carbon fiber-carbon net tire unit layer, 0 degree/90 degree alternate lamination needling is formed by adjusting the layering direction, and the needling density is 16-30 needles/cm 2 。
The specific preparation steps of the carbon/carbon blank of the binary carbon matrix are as follows:
the density is 0.4 to 0.6g/cm 3 The carbon fiber preform is put into a chemical vapor deposition furnace, and carbon source is introduced under the conditions of high temperature of 900-1200 ℃ and vacuum degree of 500-4000 PaPerforming chemical vapor deposition on the gas and the diluent gas to form pyrolytic carbon coated with carbon fiber on the surface of the carbon fiber preform to obtain the carbon fiber-coated carbon fiber with the density of 0.80-1.3 g/cm 3 A carbon/carbon blank of a unitary carbon matrix;
wherein the carbon source gas is natural gas or propylene (C 3 H 6 ) The diluent gas is nitrogen (N) 2 ) Or hydrogen (H) 2 ) And the volume ratio of the carbon source gas to the diluent gas is (1-3): 1;
putting the carbon/carbon blank of the unit carbon matrix into a vacuum-pressure impregnation curing furnace, heating the impregnant to soften, carrying out impregnation treatment on the carbon/carbon blank of the unit carbon matrix by adopting a vacuum method or a pressure method, leading the impregnant to enter the internal pores of the carbon/carbon blank of the unit carbon matrix, discharging the residual impregnant, then heating to 170-220 ℃, preserving heat for 1-4 h, leading the impregnant in the carbon/carbon blank of the unit carbon matrix to carry out curing reaction, then putting into a carbonization furnace, controlling the carbonization treatment temperature to be 850-1000 ℃ and the carbonization time to be 2-6 h, and obtaining the carbon-carbon composite material with the density of 1.0-1.5 g/cm 3 A carbon/carbon blank of a binary carbon matrix;
wherein the impregnant is furfuryl ketone resin, phenolic resin or asphalt, and the pressure in the furnace is not less than 1.5MPa during pressure impregnation.
The specific steps of high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix are as follows: and (3) loading the carbon/carbon blank of the binary carbon matrix into a high-temperature treatment furnace, introducing nitrogen or inert gas to the furnace under the protective atmosphere, heating to 1800-2400 ℃, and preserving the temperature for 1-6 hours to complete the high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix.
The specific preparation steps of the carbon/ceramic brake disc blank are as follows: firstly, mechanically processing a graphitized carbon/carbon blank of the binary carbon matrix according to a final product drawing to obtain a molded blank; then placing the formed blank into a graphite crucible, calculating the filling amount according to the volume of the final product, adding silicon powder into the graphite crucible after filling, placing the graphite crucible into a high-temperature furnace, heating to 1600-2000 ℃, preserving heat for 1-4 hours, controlling the vacuum degree to be 200-2000 Pa, melting solid silicon material into silicon liquid, enabling the silicon liquid to enter holes of the formed blank through capillary effect, enabling Si to contact C and to be formed on the contact surface of silicon carbonChemically reacting to generate SiC to obtain the SiC powder with the density of 1.9-2.4 g/cm 3 A carbon/ceramic brake disc blank.
And spreading silicon powder at the bottom of the crucible, and placing 5-8 cushion blocks made of porous silicon carbide materials in the silicon powder to support the formed blank body, so that the silicon powder does not contact the formed blank body.
The specific steps for preparing the ceramic functional layer on the surface of the carbon/ceramic brake disc blank through in-situ reaction are as follows:
brushing the prepared ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank or soaking the carbon/ceramic brake disc blank in the prepared ceramic precursor glue solution, drying, then putting into a high-temperature furnace, heating to 1600-2000 ℃, preserving heat for 1-3 h, forming a ceramic functional layer on the surface of the carbon/ceramic brake disc blank, and then polishing and assembling required metal parts to obtain the high-strength carbon/ceramic brake disc with the ceramic functional layer.
The thickness of the ceramic functional layer is preferably 0.5 to 3mm.
The beneficial effects are that:
(1) According to the invention, a carbon/carbon blank body of a binary carbon matrix is adopted, and pyrolytic carbon wrapping carbon fibers and resin carbon or asphalt carbon filling pores are introduced into the carbon fiber preform, so that silicon preferentially reacts with the resin carbon or the asphalt carbon to generate SiC in the subsequent liquid phase siliconizing process, and the pyrolytic carbon coated on the surface of the carbon fibers can effectively protect the carbon fibers from being corroded by silicon liquid, so that the strength and toughness of the carbon fibers are maintained to the maximum extent, and the high mechanical strength of the brake disc is ensured.
(2) When resin carbon or asphalt carbon is introduced into the carbon fiber preform, the introduced impregnant is carbonized and then contracted to form pores, a channel is created for the subsequent silicon liquid to enter, and the silicon-carbon reaction after the silicon liquid does not enter the pores reserves a carbon source, so that the proportion of residual silicon is effectively reduced, and the mass ratio of the residual silicon can be controlled within 5%. Since the melting point of Si (about 1420 ℃) is much lower than that of SiC (about 2700 ℃), the high-temperature stability of the brake disc can be greatly improved.
(3) In the invention, the purpose that the pyrolytic carbon wraps the carbon fiber to protect the carbon fiber from being corroded by silicon is better exertedThe thickness of the introduced pyrolytic carbon is about 1-3 mu m, namely, the density is 0.4-0.6 g/cm 3 The density of the carbon fiber preform is increased to 0.8-1.3 g/cm 3 . In order to make the resin carbon/asphalt carbon and liquid silicon fully react, the weight ratio of resin carbon/asphalt carbon is introduced to be 25-35%, namely, the resin carbon/asphalt carbon is continuously densified to 1.0-1.5 g/cm 3 . Through the scientific proportion of the content of the pyrolytic carbon and the resin carbon/asphalt carbon in the binary matrix carbon, the proportion of residual silicon can be effectively reduced, the strength retention rate of carbon fibers can be greatly improved, and the mechanical properties of the carbon/ceramic brake disc can be improved by 10-20%.
(4) When pyrolytic carbon is introduced into the carbon fiber preform, the microstructure of the formed pyrolytic carbon is controlled by controlling the volume ratio of carbon source gas and diluent gas, the deposition temperature, the vacuum degree and the like, so that the pyrolytic carbon with a coarse layer structure is formed, and the pyrolytic carbon with an isotropic layer structure is avoided. Compared with isotropic pyrolytic carbon, the rough layer pyrolytic carbon has the characteristics of high friction coefficient and easy graphitization and pore opening, is favorable for the later ceramic reaction, and ensures that the brake disc maintains stable tribological performance.
(5) The ceramic functional layer is prepared on the surface of the brake disc through in-situ reaction, and has good bonding force with a matrix and adjustable thickness. In order to better exert the advantages of high friction coefficient, high hardness and oxidation resistance of the SiC ceramic, the mass content of SiC in the prepared ceramic functional layer is more than 92 percent and is far higher than the mass content (40-70 percent) of SiC in the brake disc body through the scientific design of the ceramic functional layer formula, so that the friction coefficient, wear resistance and oxidation resistance of the brake disc are effectively improved, and the service life of the brake disc can be remarkably prolonged.
(6) The brake disc has the characteristics of high mechanical strength, high friction coefficient, low wear rate, good oxidation resistance and long service life, not only can be used on conventional automobiles, airplanes and high-speed rails, but also can meet the use requirements of extreme braking environments such as high-performance racing automobiles, heavy trucks, tanks and the like.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a coarse layer structure pyrolytic carbon deposited on the surface of a carbon fiber preform in step (2) of example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the isotropic-structure pyrolytic carbon deposited on the surface of the carbon fiber preform in step (2) of comparative example 4.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
Example 1
(1) The method comprises the steps of pre-needling carbon fibers and a carbon net tire to form a carbon fiber-carbon net tire unit layer by adopting SYT49S-12K carbon fibers of Zhongfushenying eagle company, and forming a 2.5D carbon fiber flat felt by adopting a mode of layer-by-layer tiling and relay needling of a plurality of carbon fiber-carbon net tire unit layers on a flat needling machine, wherein the flat direction is 0 degree/90 degree alternately laminated, and the needling density in the thickness direction is 16 needles/cm 2 Cutting according to the size of the brake disc to obtain a brake disc with an outer diameter of 390 mm, a thickness of 38 mm and a density of 0.4 g/cm 3 Carbon fiber preform of (2);
(2) Putting the carbon fiber preform prepared in the step (1) into a chemical vapor deposition furnace, heating the furnace to 900 ℃, and introducing C as carbon source gas according to the volume ratio of 1:1 when the vacuum degree in the furnace reaches the regulated pressure of 500 Pa 3 H 6 N as diluent gas 2 Chemical vapor deposition was carried out for 150 hours to obtain a density of 0.91 g/cm 3 A carbon/carbon blank of a unitary carbon matrix; the surface of the carbon fiber preform is deposited with rough layer structure pyrolytic carbon by observation of a polarized light microscope, and the microscopic morphology of the pyrolytic carbon is shown in figure 1;
(3) Putting the carbon/carbon blank of the unit carbon matrix prepared in the step (2) into a vacuum-pressure impregnation curing furnace, adopting phenolic resin as an impregnant, heating and pressurizing the phenolic resin to 1.5MPa in the vacuum-pressure impregnation curing furnace to enable the phenolic resin to enter the internal pores of the product, discharging the residual phenolic resin by pressure, then slowly heating the furnace to 180 ℃ for curing reaction, taking out the product after the curing reaction for 3 hours, and loading the product into a carbonization furnace for carbonization treatment, wherein the carbonization treatment temperature is 850 ℃ and the carbonization treatment temperature is 850 DEG CThe time is 5 hours, and the density is 1.18g/cm 3 A carbon/carbon blank of a binary carbon matrix;
(4) Filling the carbon/carbon blank of the binary carbon matrix prepared in the step (3) into a high-temperature treatment furnace, introducing nitrogen for protection, slowly heating to 1800 ℃, and preserving heat for 6 hours to complete high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix;
(5) Machining the carbon/carbon blank of the binary carbon matrix subjected to the high-temperature graphitization treatment in the step (4) according to a final product drawing, machining the inner diameter, the outer diameter and the thickness in place, and punching ventilation holes to obtain a molded blank;
(6) Spreading 2500g of silicon powder at the bottom of a graphite crucible, placing 5 cushion blocks made of porous silicon carbide materials in the silicon powder, placing the molding blank body prepared in the step (5) on the cushion blocks, enabling the silicon powder not to contact the molding blank body, then placing the graphite crucible into a high-temperature furnace, controlling the vacuum degree to be 200Pa, slowly heating to 1600 ℃, preserving heat for 4 hours, melting the silicon powder into silicon liquid, entering holes of the molding blank body through capillary effect, reacting Si with C to generate SiC, and obtaining the silicon carbide ceramic with the density of 2.26g/cm 3 Is a carbon/ceramic brake disc blank;
(7) Phenolic resin, polymethyl silane and silicon powder are mixed according to the mass ratio of 30:15:55, mixing for 0.5h through mechanical stirring to prepare ceramic precursor glue solution; brushing the prepared ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank body prepared in the step (6), then drying, solidifying, then putting into a high-temperature furnace, slowly heating to 1600 ℃, and preserving heat for 3 hours to form a ceramic functional layer with the thickness of 0.5mm on the surface of the carbon/ceramic brake disc blank body;
(8) And (3) polishing the carbon/ceramic brake disc blank with the ceramic functional layer on the surface, and assembling a required metal piece to obtain the high-strength carbon/ceramic brake disc with the ceramic functional layer.
Example 2
(1) The method comprises pre-needling carbon fiber and carbon net tire to obtain carbon fiber-carbon net tire unit layer by adopting SYT49S-24K carbon fiber of Zhongfushenying company, spreading and splicing several carbon fiber-carbon net tire unit layers layer by layer on a flat needling machineForming a 2.5D carbon fiber flat felt by force needling, wherein the flat surface direction is alternately laminated at 0 degree/90 degree and the needling density in the thickness direction is 30 needles/cm 2 Cutting according to the size of the brake disc to obtain a brake disc with an outer diameter of 390 mm, a thickness of 38 mm and a density of 0.6g/cm 3 Carbon fiber preform of (2);
(2) Putting the carbon fiber preform obtained in the step (1) into a chemical vapor deposition furnace, heating the furnace to 1200 ℃, and introducing CH as a carbon source gas when the vacuum degree in the furnace reaches pressure stabilizing 4000Pa 4 H as diluent gas 2 And CH (CH) 4 And H is 2 The volume ratio is 3:1, and the density is 1.22 g/cm after 200 hours of chemical vapor deposition 3 A carbon/carbon blank of a unitary carbon matrix; the surface of the carbon fiber preform is deposited with pyrolytic carbon with a rough layer structure through observation of a polarized light microscope,
(3) Placing the carbon/carbon blank of the unit carbon matrix prepared in the step (2) into a vacuum-pressure impregnation curing furnace, adopting furfuryl ketone resin as an impregnant, heating and pressurizing the furfuryl ketone resin to 2.5MPa in the vacuum-pressure impregnation curing furnace to enable the furfuryl ketone resin to enter the internal pores of the product, discharging the residual furfuryl ketone resin by pressure, then slowly heating the furnace to 220 ℃ for curing reaction, taking out the product after 2 hours of curing reaction, loading the product into a carbonization furnace for carbonization treatment, wherein the carbonization treatment temperature is 1000 ℃ and the carbonization treatment time is 4 hours, and obtaining the product with the density of 1.45g/cm 3 A carbon/carbon blank of a binary carbon matrix;
(4) Filling the carbon/carbon blank of the binary carbon matrix prepared in the step (3) into a high-temperature treatment furnace, introducing nitrogen for protection, slowly heating to 2200 ℃, and preserving the temperature for 1h to finish the high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix;
(5) Machining the carbon/carbon blank of the binary carbon matrix subjected to the high-temperature graphitization treatment in the step (4) according to a final product drawing, machining the inner diameter, the outer diameter and the thickness in place, and punching ventilation holes to obtain a molded blank;
(6) Spreading 2500g of silicon powder at the bottom of a graphite crucible, placing 8 cushion blocks made of porous silicon carbide materials in the silicon powder, and performing the following stepsPlacing the formed blank prepared in the step (5) on a cushion block to ensure that silicon powder does not contact the formed blank, then placing a graphite crucible into a high-temperature furnace, controlling the vacuum degree to be 2000Pa, slowly heating to 2000 ℃, preserving heat for 1h, melting the silicon powder into silicon liquid, entering holes of the formed blank through capillary effect, and generating SiC through the reaction of Si and C to obtain the silicon carbide with the density of 2.09g/cm 3 Is a carbon/ceramic brake disc blank;
(7) Furfuryl ketone resin, polymethyl silane and silicon powder are mixed according to the mass ratio of 30:28:42, mixing, namely preparing ceramic precursor glue solution by mechanically stirring and mixing for 2 hours; brushing the prepared ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank body prepared in the step (6), then drying, solidifying and then putting into a high-temperature furnace, slowly heating to 2000 ℃, and preserving heat for 1h to form a ceramic functional layer with the thickness of 3mm on the surface of the carbon/ceramic brake disc blank body;
(8) And (3) polishing the carbon/ceramic brake disc blank with the ceramic functional layer on the surface, and assembling a required metal piece to obtain the high-strength carbon/ceramic brake disc with the ceramic functional layer.
Comparative example 1
(1) Adopting SYT49S-24K carbon fiber of Zhongfushenying company, adopting non-woven cloth and carbon net tyre to alternatively lay layers for needling, wherein the direction of adjacent non-woven cloth is an included angle of 0 degree/90 degree, and the needling density in the thickness direction is 20 needles/cm 2 Layer by layer, and cutting to obtain 390-mm outer diameter, 40-mm thickness and 0.50-g/cm density 3 2.5D preform of (2);
(2) The chemical vapor deposition process was the same as in step (2) of example 2, corresponding to a density of 1.28 g/cm 3 A carbon/carbon blank of a unitary carbon matrix;
(3) Performing high-temperature treatment on the carbon/carbon blank of the unit carbon matrix prepared in the step (2), wherein the implementation process is the same as that of the step (4) of the embodiment 2;
(4) Machining the carbon/carbon blank of the unit carbon matrix subjected to the high-temperature treatment in the step (3) according to a final product drawing, machining the inner diameter, the outer diameter and the thickness in place, and punching ventilation holes to obtain a molded blank;
(5) The shaped green body obtained in step (4) was subjected to ceramization in the same manner as in step (6) of example 2, and a bulk density of 2,05g/cm was obtained 3 Is a carbon/ceramic brake disc blank;
(6) And (3) polishing the carbon/ceramic brake disc blank obtained in the step (5), and assembling a required metal piece to obtain the carbon/ceramic brake disc without the ceramic functional layer.
Comparative example 2
(1) Adopting SYT49S-24K carbon fiber of Zhongfushenying company, adopting non-woven cloth and carbon net tyre to alternatively lay layers for needling, wherein the direction of adjacent non-woven cloth is an included angle of 0 degree/90 degree, and the needling density in the thickness direction is 20 needles/cm 2 Layer by layer, and cutting to obtain 390-mm outer diameter, 40-mm thickness and 0.50-g/cm density 3 2.5D preform of (2);
(2) Subjecting the carbon fiber preform obtained in the step (1) to resin impregnation and carbonization treatment in the same manner as in the step (3) of example 2, and subjecting the carbon fiber preform to resin impregnation and carbonization treatment for 4 times to obtain a carbon fiber preform having a density of 1.26 g/cm 3 The matrix carbon of (2) is a carbon/carbon blank of a unit carbon matrix of resin carbon;
(3) Performing high-temperature treatment on the carbon/carbon blank of the unit carbon matrix prepared in the step (2), wherein the implementation process is the same as that of the step (4) of the embodiment 2;
(4) Machining the carbon/carbon blank of the unit carbon matrix subjected to the high-temperature treatment in the step (3) according to a final product drawing, machining the inner diameter, the outer diameter and the thickness in place, and punching ventilation holes to obtain a molded blank;
(5) The shaped green body obtained in step (4) was subjected to ceramization in the same manner as in step (6) of example 2, and a bulk density of 2.07g/cm was obtained 3 Is a carbon/ceramic brake disc blank;
(6) And (3) polishing the carbon/ceramic brake disc blank obtained in the step (5), and assembling a required metal piece to obtain the carbon/ceramic brake disc without the ceramic functional layer.
Comparative example 3
(1) SYT49S-24K carbon fiber of Zhongfu eagle company is adoptedAlternatively laying and needling the non-woven cloth and the carbon net tyre, wherein the adjacent non-woven cloth has an included angle of 0 degree/90 degree in the direction and the needling density of 20 needles/cm in the thickness direction 2 Layer by layer, and cutting to obtain 390-mm outer diameter, 40-mm thickness and 0.60-g/cm density 3 2.5D preform of (2);
(2) Performing chemical vapor deposition on the carbon fiber preform obtained in the step (1) in the same manner as in the step (2) of the example 2, and performing chemical vapor deposition for 300 hours to obtain a carbon fiber preform with a density of 1.49 g/cm 3 A carbon/carbon blank of a unitary carbon matrix;
(3) The carbon/carbon blank of the unit carbon matrix obtained in the step (2) is subjected to impregnation carbonization treatment, and the process is the same as in the step (3) of the example 2, so that a density of 1.70g/cm is obtained 3 A carbon/carbon blank of a binary carbon matrix;
(4) Carrying out high-temperature treatment on the carbon/carbon blank of the binary carbon matrix prepared in the step (3), wherein the implementation process is the same as that of the step (4) of the embodiment 2;
(5) The carbon/carbon blank of the binary carbon matrix subjected to high temperature treatment, which is prepared in the step (4), is mechanically processed according to the drawing of the final product, the inner diameter, the outer diameter and the thickness are processed in place, and ventilation holes are formed, so that a molded blank is prepared;
(6) The shaped green body obtained in step (4) was subjected to ceramization in the same manner as in step (6) of example 2, corresponding to a bulk density of 1.89g/cm 3 Is a carbon/ceramic brake disc blank;
(7) And (3) polishing the carbon/ceramic brake disc blank obtained in the step (6), and assembling a required metal piece to obtain the carbon/ceramic brake disc without the ceramic functional layer.
Comparative example 4
(1) Adopting SYT49S-24K carbon fiber of Zhongfushenying company, adopting non-woven cloth and carbon net tyre to alternatively lay layers for needling, wherein the direction of adjacent non-woven cloth is an included angle of 0 degree/90 degree, and the needling density in the thickness direction is 20 needles/cm 2 Layer by layer, and cutting to obtain 390-mm outer diameter, 40-mm thickness and 0.60-g/cm density 3 2.5D preform of (2);
(2) The steps are%1) The prepared carbon fiber preform is put into a chemical vapor deposition furnace, the furnace temperature is increased to 1100 ℃, and when the vacuum degree in the furnace reaches to 2000Pa, CH as carbon source gas is introduced 4 H as diluent gas 2 And CH (CH) 4 And H is 2 The volume ratio is 1:2, and the density is 1.02 g/cm after 200 hours of chemical vapor deposition 3 A carbon/carbon blank of a unitary carbon matrix; the pyrolytic carbon is in an isotropic structure as shown in figure 2;
(3) Placing the carbon/carbon blank of the unit carbon matrix prepared in the step (2) into a vacuum-pressure impregnation curing furnace, adopting furfuryl ketone resin as an impregnant, heating and pressurizing the furfuryl ketone resin to 2.5MPa in the vacuum-pressure impregnation curing furnace to enable the furfuryl ketone resin to enter the internal pores of the product, discharging the residual furfuryl ketone resin by pressure, then slowly heating the furnace to 220 ℃ for curing reaction, taking out the product after 2 hours of curing reaction, loading the product into a carbonization furnace for carbonization treatment, wherein the carbonization treatment temperature is 1000 ℃ and the carbonization treatment time is 4 hours, and obtaining the product with the density of 1.24g/cm 3 A carbon/carbon blank of a binary carbon matrix;
(4) Carrying out high-temperature treatment on the carbon/carbon blank of the binary carbon matrix prepared in the step (3), wherein the implementation process is the same as that of the step (4) of the embodiment 2;
(5) The carbon/carbon blank of the binary carbon matrix subjected to high temperature treatment, which is prepared in the step (4), is mechanically processed according to the drawing of the final product, the inner diameter, the outer diameter and the thickness are processed in place, and ventilation holes are formed, so that a molded blank is prepared;
(6) The shaped green body obtained in step (4) was subjected to ceramization in the same manner as in step (6) of example 2, corresponding to a bulk density of 1.78g/cm 3 Is a carbon/ceramic brake disc blank;
(7) And (3) polishing the carbon/ceramic brake disc blank obtained in the step (5), and assembling a required metal piece to obtain the carbon/ceramic brake disc without the ceramic functional layer.
To further study and evaluate the mechanical properties and frictional wear properties of the charcoal/ceramic brake discs prepared in examples and comparative examples, the charcoal/ceramic brake discs prepared in examples and comparative examples were respectively matched with the imported charcoal/ceramic disc-dedicated brake disc, and ground bench tests were conducted in a LINK3000 bench tester according to SAEJ2522-AK Master test specifications, with the strength and test results being compared as shown in table 1 below.
TABLE 1
| Project | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Compressive Strength (MPa) | 305 | 278 | 239 | 267 | 193 | 206 |
| Flexural Strength (MPa) | 182 | 167 | 145 | 89 | 171 | 115 |
| Coefficient of friction | 0.47 | 0.46 | 0.36 | 0.41 | 0.33 | 0.35 |
| Mass wear rate (g) | 0.11 | 0.13 | 0.48 | 0.36 | 0.57 | 0.52 |
Comparative example 1 is a carbon/ceramic brake disk containing only a unit carbon matrix (pyrolytic carbon), resulting in a residual silicon mass ratio of 15.3% due to lack of resin carbon consuming Si source, a decrease in mechanical properties, and an adverse effect on high temperature friction properties. Comparative example 2 is a carbon/ceramic brake disk containing only a unit carbon matrix (resin carbon), and the surface of the carbon fiber lacks protection of pyrolytic carbon, which causes reaction erosion of liquid silicon to the carbon fiber, resulting in a great decrease in bending strength of the carbon/ceramic brake disk. Comparative example 3 contains a binary carbon matrix, but the proportion of the binary carbon matrix and the matrix is unbalanced, so that the carbon content of the matrix is too high, the opening rate of a blank is low, a siliconizing channel is not smooth, the SiC ceramic content in a carbon/ceramic brake disc is low, the product density is low, and the compression strength is low. Comparative example 4 is that the pyrolytic carbon microstructure fails to form a coarse layer structure due to unreasonable technological parameters, mainly takes isotropic carbon as a main material, is unfavorable for high-temperature graphitization open pores, and has poor siliconizing channels, so that the carbon/ceramic brake disc has low SiC ceramic content, low product density and poor performance. The ceramic functional layers were not formed in comparative examples 1 to 4, so that the friction coefficient was generally lower than that of examples and the wear rate was generally higher than that of examples. As can be seen from the test results of the table, the high-strength carbon/ceramic brake disc with the ceramic functional layer prepared by the invention maintains the strength and toughness of the carbon fiber to the maximum extent by introducing the binary matrix carbon (pyrolytic carbon and resin carbon/asphalt carbon), effectively reduces the proportion of residual silicon and greatly improves the mechanical strength of the material; the ceramic functional layer introduced by the in-situ reaction obviously improves the friction coefficient and reduces the wear rate.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high strength charcoal/ceramic brake disk with ceramic functional layer, which is characterized in that: firstly, carrying out high-temperature graphitization treatment on a carbon/carbon blank body of a binary carbon matrix, preparing the graphitized carbon/carbon blank body of the binary carbon matrix into a carbon/ceramic brake disc blank body through a liquid phase silicon infiltration reaction, and forming a ceramic functional layer through in-situ reaction of ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank body to obtain the brake disc;
the carbon/carbon blank of the binary carbon matrix is prepared by coating pyrolytic carbon on the surface of carbon fiber of a carbon fiber preform by utilizing a chemical vapor deposition process, and filling resin carbon or asphalt carbon in the pores of the carbon fiber preform by utilizing an impregnation carbonization process; wherein the carbon fiber preform is formed by needling carbon fibers and a carbon net tire and has a density of 0.4-0.6 g/cm 3 The density of the coated pyrolytic carbon is increased to 0.8-1.3 g/cm 3 The density of the resin carbon or asphalt carbon is continuously increased to 1.0-1.5 g/cm 3 Correspondingly, the density of the carbon/ceramic brake disc blank is 1.9-2.4 g/cm 3 ；
The ceramic precursor glue solution is prepared from thermosetting resin, polymethyl silane and silicon powder according to the following proportion of 30: (15-40): (30-55) by mass ratio.
2. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, characterized in that: the carbon fiber preform is prepared by the following steps: spreading carbon fiber and pre-needling the carbon net tire to form a carbon fiber-carbon net tire unit layer, spreading a plurality of carbon fiber-carbon net tire unit layers layer by layer on a flat needling machine to form a 2.5D carbon fiber flat felt in a relay needling mode, and cutting according to the size of a brake disc to obtain a carbon fiber preform.
3. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 2, characterized in that: in the needling process of the carbon fiber-carbon net tire unit layer, 0 degree/90 degree alternate lamination needling is formed by adjusting the layering direction, and the needling density is 16-30 needles/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The carbon fiber is selected from 12-48K carbon fiber.
4. A high strength charcoal/ceramic brake disk with ceramic functional layer according to any of claims 1 to 3, characterized in that: the specific preparation steps of the carbon/carbon blank of the binary carbon matrix are as follows:
the density is 0.4 to 0.6g/cm 3 Putting the carbon fiber preform into a chemical vapor deposition furnace, introducing carbon source gas and diluent gas at the high temperature of 900-1200 ℃ and the vacuum degree of 500-4000 Pa for chemical vapor deposition, and forming pyrolytic carbon coated with carbon fibers on the surface of the carbon fiber preform to obtain the carbon fiber-coated pyrolytic carbon with the density of 0.80-1.3 g/cm 3 A carbon/carbon blank of a unitary carbon matrix;
putting the carbon/carbon blank of the unit carbon matrix into a vacuum-pressure impregnation curing furnace, heating the impregnant to soften, carrying out impregnation treatment on the carbon/carbon blank of the unit carbon matrix by adopting a vacuum method or a pressure method, leading the impregnant to enter the internal pores of the carbon/carbon blank of the unit carbon matrix, discharging the residual impregnant, then heating to 170-220 ℃, preserving heat for 1-4 h, leading the impregnant in the carbon/carbon blank of the unit carbon matrix to carry out curing reaction, then putting into a carbonization furnace, controlling the carbonization treatment temperature to be 850-1000 ℃ and the carbonization time to be 2-6 h, and obtaining the carbon-carbon composite material with the density of 1.0-1.5 g/cm 3 A carbon/carbon blank of a binary carbon matrix;
wherein the carbon source gas is natural gas or propylene, the diluent gas is nitrogen or hydrogen, and the volume ratio of the carbon source gas to the diluent gas is (1-3): 1; the impregnant is furfuryl ketone resin, phenolic resin or asphalt, and the pressure in the furnace is not less than 1.5MPa during pressure impregnation.
5. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, characterized in that: the specific steps of high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix are as follows: and (3) loading the carbon/carbon blank of the binary carbon matrix into a high-temperature treatment furnace, introducing nitrogen or inert gas to the furnace under the protective atmosphere, heating to 1800-2400 ℃, and preserving the temperature for 1-6 hours to complete the high-temperature graphitization treatment of the carbon/carbon blank of the binary carbon matrix.
6. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, characterized in that: the specific preparation steps of the carbon/ceramic brake disc blank are as follows: firstly, mechanically processing a graphitized carbon/carbon blank of the binary carbon matrix according to a final product drawing to obtain a molded blank; then placing the molded blank into a graphite crucible, calculating the filling amount according to the volume of the final product, adding silicon powder into the graphite crucible after filling, placing the graphite crucible into a high-temperature furnace, heating to 1600-2000 ℃, preserving heat for 1-4 h, controlling the vacuum degree to be 200-2000 Pa, and obtaining the density to be 1.9-2.4 g/cm 3 A carbon/ceramic brake disc blank.
7. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 6, characterized in that: and spreading silicon powder at the bottom of the crucible, and placing 5-8 cushion blocks made of porous silicon carbide materials in the silicon powder to support the formed blank body, so that the silicon powder does not contact the formed blank body.
8. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, characterized in that: the thermosetting resin in the ceramic precursor glue solution is phenolic resin, epoxy resin or furfuryl ketone resin.
9. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, characterized in that: the specific steps for preparing the ceramic functional layer on the surface of the carbon/ceramic brake disc blank through in-situ reaction are as follows: brushing the prepared ceramic precursor glue solution on the surface of the carbon/ceramic brake disc blank or soaking the carbon/ceramic brake disc blank in the prepared ceramic precursor glue solution, drying, then putting into a high-temperature furnace, heating to 1600-2000 ℃, and preserving heat for 1-3 h to form a ceramic functional layer on the surface of the carbon/ceramic brake disc blank.
10. A high strength charcoal/ceramic brake disk with ceramic functional layer according to claim 1, 8 or 9, characterized in that: the thickness of the ceramic functional layer is 0.5-3 mm.
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| WO2024148738A1 (en) | 2024-07-18 |
| CN115773321A (en) | 2023-03-10 |
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