CN110606763A - Preparation method of carbon/ceramic brake disc with pure ceramic layer on surface - Google Patents

Preparation method of carbon/ceramic brake disc with pure ceramic layer on surface Download PDF

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Publication number
CN110606763A
CN110606763A CN201910998807.1A CN201910998807A CN110606763A CN 110606763 A CN110606763 A CN 110606763A CN 201910998807 A CN201910998807 A CN 201910998807A CN 110606763 A CN110606763 A CN 110606763A
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China
Prior art keywords
carbon
brake disc
impregnation
ceramic layer
ceramic
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CN201910998807.1A
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Inventor
史云强
杨川
何留阳
刘汝强
李宗乐
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Shandong Daopuan Brake Material Co Ltd
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Shandong Daopuan Brake Material Co Ltd
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Priority to CN201910998807.1A priority Critical patent/CN110606763A/en
Publication of CN110606763A publication Critical patent/CN110606763A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5057Carbides
    • C04B41/5059Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02Compositions of linings; Methods of manufacturing
    • F16D69/023Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608Green bodies or pre-forms with well-defined density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • F16D2200/0039Ceramics
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • F16D2200/0052Carbon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0082Production methods therefor
    • F16D2200/0086Moulding materials together by application of heat and pressure

Abstract

The invention relates to a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface, belonging to the technical field of preparation processes of carbon fiber reinforced ceramic matrix composite materials.

Description

Preparation method of carbon/ceramic brake disc with pure ceramic layer on surface
Technical Field
The invention relates to a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface, in particular to a method for preparing an automobile carbon/ceramic brake disc by combining chemical vapor infiltration, hot-pressing solidification and reaction melt infiltration, and belongs to the technical field of preparation processes of carbon fiber reinforced ceramic matrix composite materials.
Background
The carbon/ceramic composite material overcomes the defect that a single pure ceramic material is easy to brittle fracture, has higher fracture toughness (resistance to instantaneous fracture), and has higher strength and better thermal shock resistance. In the middle of the 90 s of the 20 th century, carbon/ceramic composite materials are beginning to be applied to the friction field, and the German aerospace agency develops a Porsche carbon/ceramic brake disc in 2002 first, and has the advantages of light weight, high temperature resistance, good braking performance and the like.
The production process of the carbon/ceramic brake disc at present mainly comprises two types of short fiber mould pressing and long fiber weaving. However, both the short fiber molded carbon/ceramic brake disc and the long fiber woven carbon/ceramic brake disc have the defect that the friction interface fiber and the matrix are exposed, so that the carbon fiber and the carbon matrix of the friction interface have the phenomenon of peeling off due to oxidation in the braking process, the friction and wear performance of the brake disc is influenced, and the phenomena of brake shaking and noise are easily caused due to the inconsistent thickness of the brake disc.
Therefore, the oxidation resistance of the friction interface of the carbon/ceramic brake disc is improved, and the phenomenon that the disc surface is oxidized and peeled off due to the exposure of the fiber and the matrix is avoided, so that the carbon/ceramic brake disc has important significance for improving the braking performance of the carbon/ceramic brake disc.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface, which is characterized in that the carbon/ceramic brake disc with the pure ceramic layer on the surface is prepared by combining chemical vapor deposition, hot pressing, solidification and reaction melt infiltration processes, combining a carbon fiber tire net with silicon carbide powder and carbon powder, mixing and hot pressing the mixture by resin, and then carrying out a siliconizing process, so that the effect of covering and protecting the carbon fiber and a matrix on the disc surface is achieved, the problem of oxidation of the carbon fiber and the carbon matrix on the disc surface is solved, and the braking performance of the carbon/ceramic brake disc is improved.
The technical scheme of the invention is as follows:
a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface comprises the following steps:
step 1: preparing a carbon fiber preform;
step 2: chemical vapor deposition
Performing high-temperature heat treatment on the carbon fiber preform, and depositing pyrolytic carbon by Chemical Vapor Infiltration (CVI) to obtain the carbon fiber preform with the density of 1.0g/cm3-1.4g/cm3The carbon/carbon composite of (a);
and step 3: web impregnation
Impregnating the tire net with an impregnating slurry containing carbon powder and silicon carbide powder;
and 4, step 4: hot press forming
Forming a whole by hot-pressing the carbon/carbon composite material obtained in the step 2 and the impregnated tire net obtained in the step 3;
and 5: siliconizing the composite material obtained in the step 4, wherein the reaction melt is silicon or silicon alloy, and the obtained density is 1.9g/cm3-3.0g/cm3A carbon/carbon-silicon carbide composite material with a surface pure ceramic layer.
Preferably, the type of the carbon fiber preform used in the step 1 is two-dimensional plain cloth weaving or three-dimensional weaving, the carbon fiber preform is annular, the outer diameter is 200mm-800mm, the inner diameter is 100mm-200mm, and the thickness is 20mm-100 mm; the carbon fiber preform had a density of about 0.45g/cm3, a carbon fiber content of about 40 vol.%, and a layer density of 14 layers/(10 mm).
Preferably, in the step 2, the heat treatment temperature of the high-temperature heat treatment of the carbon fiber preform is 2100-.
Preferably, in step 2, the deposition temperature is 900-1100 ℃, the deposition time is 200-400h, and the precursor is CH4And C3H8
Preferably, the tyre net used in the step 3 adopts a three-dimensional needling prefabricated body, the outer diameter is 200mm-800mm, the inner diameter is 100mm-200mm, the thickness is 2mm-3mm, and the density is 0.16-0.20g/cm3Outside diameter and inside diameter of tyre netThe diameter size is the same as the size of the carbon fiber preform in the step 1; the tyre net is obtained by multiple cyclic layering needling, and the needling hole density is 10-12/cm2The layer density was 14 layers/(10 mm).
The carbon fiber prefabricated body and the tire net adopt a carbon fiber brand of T700.
Preferably, in the step 3, during impregnation, the tire net is placed into an impregnation tank, the impregnation tank is vacuumized to-0.96 MPa, the impregnation slurry is introduced, air pressurization is carried out, the impregnation pressure is 1-3MPa, the impregnation time is 1-2h, the tire net is taken out after the impregnation is finished, and the tire net is dried in an oven at the temperature of 40-60 ℃.
Preferably, the dipping slurry used in the step 3 is a phenolic resin solution mixed carbon powder and SiC powder, the phenolic resin solution is formed by mixing phenolic resin and alcohol, and the mixing mass ratio is that the phenolic resin: 1:10 of alcohol; then adding hexamethylene tetramine with the mass of 1 percent of the mass of the solution as a curing agent, and carrying out ball milling and mixing for 48 hours; then adding carbon powder and silicon carbide powder into the phenolic resin solution, wherein the mixing mass ratio of the phenolic resin solution to the carbon powder to the silicon carbide powder is 50 percent (30-20 percent) to 20-30 percent; and carrying out ball milling and mixing for 48h to obtain the impregnation slurry.
And 3, impregnating slurry containing carbon powder and silicon carbide powder in the tire net, uniformly suspending the silicon carbide powder and the carbon powder on fibers of the tire net through phenolic resin, and 4, combining the impregnated tire net and the carbon/carbon composite material together through hot pressing. The pure ceramic preparation layer prepared by the steps improves the uniformity and integrity of ceramic layer phases and reduces the thermal mismatch effect among the materials.
Preferably, in step 4, the impregnated tire net obtained in step 2 is provided on both upper and lower surfaces of the carbon/carbon composite material obtained in step 1, and hot press molding is performed.
Preferably, in the step 4, the hot-pressing temperature is 160-.
Preferably, in the step 5, the reaction temperature of the siliconizing treatment is 1200-1900 ℃, the heat preservation time is 0.5-4 h, and the siliconizing treatment is naturally cooled to the room temperature along with the furnace.
The invention has the beneficial effects that:
the invention provides a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface, which combines the processes of chemical vapor deposition, hot pressing, solidification and reaction melt infiltration, combines silicon carbide powder and carbon powder with carbon fiber tire net, mixes and hot presses the mixture by resin, and prepares the carbon/ceramic brake disc with the pure ceramic layer on the surface by the siliconizing process, and has the main advantages that: 1. the method combining mould pressing and weaving deposition is adopted, and the mechanical property of the matrix in the material is ensured while the pure ceramic layer is prepared; 2. siliconizing is carried out in a reaction melt infiltration mode, the preparation of the pure ceramic layer and the preparation of the matrix ceramic can be carried out simultaneously, the process is simpler and faster, and the production period and the process cost are reduced; 3. the tire net is used for impregnating carbon powder and silicon carbide powder, and siliconizing in-situ reaction is carried out after hot pressing to generate a silicon carbide pure ceramic layer, so that the thermal stress generated in the preparation process is relieved, the cracking of a substrate layer is prevented, and the bonding performance between substrates is improved; 4. the surface pure ceramic layer plays a role in covering and protecting the disc surface carbon fibers and the matrix, solves the problem of oxidation of the disc surface carbon fibers and the carbon matrix, and improves the braking performance of the carbon/ceramic brake disc.
Drawings
FIG. 1 is a schematic view of the structure of a hot-pressed layer in step 4 of the present invention;
wherein: 1. tire net (carbon + silicon carbide), 2, carbon/carbon composite.
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
Example 1:
a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface comprises the following steps:
step 1, preparation of carbon fiber preform
Firstly, making short fiber tire nets and non-woven fabrics from carbon fibers with the mark number of T700, then circularly layering single-layer 0-degree non-woven fabrics, tire nets, 90-degree non-woven fabrics and tire nets in sequence, and then needling the non-woven fabrics and the tire nets by utilizing barbed stabs below seamed edges. The barb needling is to take the fiber of the tyre net layer to the vertical direction in the needling process, so that the weftless fabric and the tyre net are connected into a whole, and the needling hole density is 10/cm 2. And (3) repeatedly laminating and needling according to the required thickness to obtain the three-dimensional needled carbon fiber preform. The preform density was about 0.45g/cm3, the carbon fiber content was about 40 vol.%, and the layer density was about 14 layers/(10 mm). The braided preform is circular and has the dimensions outer diameter inner diameter thickness 392 mm 148 mm.
Step 2, chemical vapor deposition
And carrying out high-temperature heat treatment on the obtained carbon fiber preform, wherein the heat treatment temperature is 2100 ℃, the heat preservation time is 4 hours, and the treatment atmosphere is Ar gas. Then, depositing pyrolytic carbon by Chemical Vapor Infiltration (CVI), wherein the deposition temperature is 1000 ℃, the deposition time is 300h, and the precursor is CH4And C3H8To obtain a density of 1.2g/cm3The carbon/carbon composite of (1).
And step 3: web impregnation
The tire net required by hot pressing is obtained by multiple circular layering needling, and the density of needling holes is 10/cm2The density of the layers is about 14 layers/(10 mm), the thickness is 3mm, and the inner diameter and the outer diameter are consistent with those of the prefabricated body circular ring.
Preparing a mixed solution from phenolic resin and alcohol, wherein the mass ratio of the phenolic resin to the alcohol is 1:10, adding hexamethylene tetramine with the mass being 1% of the mass of the solution as a curing agent, carrying out ball milling and mixing for 48 hours, adding carbon powder and silicon carbide powder into the solution, wherein the mixed mass ratio of the phenolic resin solution, the carbon powder and the silicon carbide powder is 50% to 30% to 20%, and carrying out ball milling and mixing for 48 hours to obtain a mixed slurry.
The density is 0.18g/cm3And a web having a thickness of 3mm was impregnated with the slurry. During impregnation, the tire net is placed into an impregnation tank, the impregnation tank is vacuumized to-0.96 MPa, the impregnation slurry is introduced, air pressurization is carried out, the impregnation pressure is 1MPa, the impregnation time is 1h, the tire net is taken out after the impregnation is finished, and the tire net is dried in an oven at 40 ℃.
And 4, step 4: hot press forming
And (3) hot-pressing the carbon/carbon composite material obtained in the step (2) and the tire net impregnated in the step (3) into a whole, wherein the impregnated tire nets are arranged on the upper surface and the lower surface of the carbon/carbon composite material as shown in figure 1, the hot-pressing temperature is 180 ℃, the time is 1 hour, and the pressure is 5 MPa.
And 5: the composite material obtained in the step 4Siliconizing the whole material, namely, silicon is taken as reaction melt, the reaction temperature is 1600 ℃, the heat preservation time is 1h, the material is naturally cooled to the room temperature along with the furnace, and the obtained density is 2.3g/cm3A carbon/carbon-silicon carbide composite material with a surface pure ceramic layer.
Example 2:
a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface comprises the following steps:
step 1, preparation of carbon fiber preform
Firstly, making short fiber tire nets and non-woven fabrics from carbon fibers with the mark number of T700, then circularly layering single-layer 0-degree non-woven fabrics, tire nets, 90-degree non-woven fabrics and tire nets in sequence, and then needling the non-woven fabrics and the tire nets by utilizing barbed stabs below seamed edges. The barb needling is to take the fiber of the tyre net layer to the vertical direction in the needling process, so that the weftless fabric and the tyre net are connected into a whole, and the needling hole density is 10/cm 2. And (3) repeatedly laminating and needling according to the required thickness to obtain the three-dimensional needled carbon fiber preform. The preform density was about 0.45g/cm3, the carbon fiber content was about 40 vol.%, and the layer density was about 14 layers/(10 mm). The braided preform is circular and has the dimensions outer diameter inner diameter thickness 392 mm 148 mm.
Step 2, chemical vapor deposition
And carrying out high-temperature heat treatment on the obtained carbon fiber preform, wherein the heat treatment temperature is 2600 ℃, the heat preservation time is 6h, and the treatment atmosphere is Ar gas. Then, depositing pyrolytic carbon by Chemical Vapor Infiltration (CVI), wherein the deposition temperature is 1100 ℃, the deposition time is 400h, and the precursor is CH4And C3H8To obtain a density of 1.4g/cm3The carbon/carbon composite of (1).
And step 3: web impregnation
The tire net required by hot pressing is obtained by multiple circular layering needling, and the density of needling holes is 12/cm2The layer density is about 14 layers/(10 mm), the thickness is 2mm, and the inner diameter and the outer diameter are consistent with those of the prefabricated body circular ring.
Preparing a mixed solution from phenolic resin and alcohol, wherein the mass ratio of the phenolic resin to the alcohol is 1:10, adding hexamethylene tetramine with the mass being 1% of the mass of the solution as a curing agent, carrying out ball milling and mixing for 48 hours, adding carbon powder and silicon carbide powder into the solution, wherein the mixed mass ratio of the phenolic resin solution, the carbon powder and the silicon carbide powder is 50% to 25%, and carrying out ball milling and mixing for 48 hours to obtain a mixed slurry.
The density is 0.20g/cm3And 2mm thick web impregnation slurry. During impregnation, the tire net is placed into an impregnation tank, the impregnation tank is vacuumized to-0.96 MPa, the impregnation slurry is introduced, air pressurization is carried out, the impregnation pressure is 2MPa, the impregnation time is 1.5h, the tire net is taken out after the impregnation is finished, and the tire net is dried in an oven at 50 ℃.
And 4, step 4: hot press forming
And (3) hot-pressing the carbon/carbon composite material obtained in the step (2) and the tire net impregnated in the step (3) into a whole, wherein the impregnated tire nets are arranged on the upper surface and the lower surface of the carbon/carbon composite material as shown in figure 1, the hot-pressing temperature is 170 ℃, the time is 1 hour, and the pressure is 4 MPa.
And 5: carrying out siliconizing treatment on the whole composite material obtained in the step 4, wherein the reaction melt is ferrosilicon alloy, the reaction temperature is 1500 ℃, the heat preservation time is 1h, and the ferrosilicon alloy is naturally cooled to the room temperature along with the furnace to obtain the composite material with the density of 2.4g/cm3A carbon/carbon-silicon carbide composite material with a surface pure ceramic layer.
Example 3:
a preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface comprises the steps of example 1, except that in the step 2, pyrolytic carbon is deposited by chemical vapor infiltration CVI, the deposition temperature is 900 ℃, the deposition time is 200 hours, and a precursor is CH4And C3H8And obtaining the carbon/carbon composite material.
Example 4:
the preparation method of the carbon/ceramic brake disc with the pure ceramic layer on the surface comprises the following steps of 1, except that in step 3, phenolic resin and alcohol are prepared into a mixed solution, the mass ratio of the phenolic resin to the alcohol is 1:10, hexamethylenetetramine with the mass being 1% of the mass of the solution is added to serve as a curing agent, ball milling and mixing are carried out for 48 hours, carbon powder and silicon carbide powder are added to the solution, the mixed mass ratio of the phenolic resin solution, the carbon powder and the silicon carbide powder is 50%: 20%: 30%, and ball milling and mixing are carried out for 48 hours to obtain mixed slurry.
Example 5:
a process for preparing a carbon/ceramic brake disc having a surface pure ceramic layer, which comprises the steps of example 1, except that in step 3, the density is set to 0.16g/cm3And a web having a thickness of 3mm was impregnated with the slurry. During impregnation, the tire net is placed into an impregnation tank, the impregnation tank is vacuumized to-0.96 MPa, the impregnation slurry is introduced, air pressurization is carried out, the impregnation pressure is 3MPa, the impregnation time is 2 hours, the tire net is taken out after the impregnation is finished, and the tire net is dried in an oven at 60 ℃.
Example 6:
the preparation method of the carbon/ceramic brake disc with the pure ceramic layer on the surface comprises the following steps of 1, wherein in the step 4, the carbon/carbon composite material obtained in the step 2 and the tire net impregnated in the step 3 are hot-pressed to form a whole, the impregnated tire nets are arranged on the upper surface and the lower surface of the carbon/carbon composite material, the hot-pressing temperature is 160 ℃, the time is 0.5h, and the pressure is 3 MPa.
Example 7:
the preparation method of the carbon/ceramic brake disc with the pure ceramic layer on the surface comprises the following steps of 1, except that in step 5, siliconizing is carried out on the whole composite material obtained in step 4, a reaction melt is a silicon alloy, the reaction temperature is 1200 ℃, the heat preservation time is 4 hours, and the silicon alloy is naturally cooled to the room temperature along with a furnace, so that the carbon/carbon-silicon carbide composite material with the pure ceramic layer on the surface is obtained.
Example 8:
the preparation method of the carbon/carbon-silicon carbide brake disc with the pure ceramic surface layer comprises the following steps of 1, except that in step 5, siliconizing is carried out on the whole composite material obtained in step 4, the reaction melt is silicon, the reaction temperature is 1900 ℃, the heat preservation time is 1 hour, and the composite material is naturally cooled to the room temperature along with a furnace, so that the carbon/carbon-silicon carbide composite material with the pure ceramic surface layer is obtained.
Examples of the experiments
Compared with the existing common carbon/ceramic brake disc, the carbon/ceramic brake disc with the pure ceramic layer on the surface prepared according to the steps of the embodiment 1 has the advantages that the friction coefficient is higher, the braking efficiency is higher and the braking distance is shorter when the carbon/ceramic brake disc with the pure ceramic layer on the surface is braked as shown in table 1; the wear rate is lower, almost no oxidation wear phenomenon is generated on the surface of the ceramic layer of the brake disc, and the service life is obviously prolonged compared with that of a common carbon/ceramic brake disc.
TABLE 1 SAE J2522 bench test Performance data comparison
Pure ceramic layer carbon/ceramic Common carbon/ceramic
Coefficient of friction 0.5 0.45
Wear rate mum <0.01 0.03

Claims (10)

1. A preparation method of a carbon/ceramic brake disc with a pure ceramic layer on the surface is characterized by comprising the following steps:
step 1: preparing a carbon fiber preform;
step 2: chemical vapor deposition
Performing high-temperature heat treatment on the carbon fiber preform, and depositing pyrolytic carbon by Chemical Vapor Infiltration (CVI) to obtain the carbon fiber preform with the density of 1.0g/cm3-1.4g/cm3The carbon/carbon composite of (a);
and step 3: web impregnation
Impregnating the tire net with an impregnating slurry containing carbon powder and silicon carbide powder;
and 4, step 4: hot press forming
Forming a whole by hot-pressing the carbon/carbon composite material obtained in the step 2 and the impregnated tire net obtained in the step 3;
and 5: siliconizing the composite material obtained in the step 4, wherein the reaction melt is silicon or silicon alloy, and the obtained density is 1.9g/cm3-3.0g/cm3A carbon/carbon-silicon carbide composite material with a surface pure ceramic layer.
2. The preparation method of the surface pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein the type of the carbon fiber preform used in the step 1 is two-dimensional plain cloth weaving or three-dimensional weaving, the carbon fiber preform is annular, the outer diameter is 200mm-800mm, the inner diameter is 100mm-200mm, and the thickness is 20mm-100 mm; the carbon fiber preform had a density of about 0.45g/cm3, a carbon fiber content of about 40 vol.%, and a layer density of 14 layers/(10 mm).
3. The method for preparing the surface-pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein in the step 2, the heat treatment temperature of the high-temperature heat treatment of the carbon fiber preform is 2100-2600 ℃, the heat preservation time is 4-6h, and the treatment atmosphere is Ar gas.
4. The method for preparing carbon/ceramic brake disc with pure ceramic surface as claimed in claim 1, wherein in step 2, the deposition temperature is 900-1100 ℃, the deposition time is 200-400h, and the precursor is CH4And C3H8
5. The method for preparing the surface pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein the tyre net used in the step 3 adopts a three-dimensional needling preform with an outer diameter of 200mm-800mm, an inner diameter of 100mm-200mm, a thickness of 2mm-3mm and a density of 0.16-0.20g/cm3The outer diameter and the inner diameter of the tire net are the same as those of the carbon fiber preform in the step 1; the tyre net is obtained by cyclic layering needling, and the density of needling holes is 10-12/cm2The layer density was 14 layers/(10 mm).
6. The method for preparing the surface-pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein in the step 3, during impregnation, the tire net is placed into an impregnation tank, vacuum pumping is carried out until the pressure is-0.96 MPa, impregnation slurry is introduced, air pressurization is carried out, the impregnation pressure is 1-3MPa, the impregnation time is 1-2h, the tire net is taken out after the impregnation is completed, and the tire net is dried in an oven at 40-60 ℃.
7. The preparation method of the surface pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein the impregnating slurry used in the step 3 is a phenolic resin solution mixed with carbon powder and SiC powder, the phenolic resin solution is formed by mixing phenolic resin and alcohol, and the mixing mass ratio is phenolic resin: 1:10 of alcohol; then adding hexamethylene tetramine with the mass of 1 percent of the mass of the solution as a curing agent, and carrying out ball milling and mixing for 48 hours; then adding carbon powder and silicon carbide powder into the phenolic resin solution, wherein the mixing mass ratio of the phenolic resin solution to the carbon powder to the silicon carbide powder is 50 percent (30-20 percent) to 20-30 percent; and carrying out ball milling and mixing for 48h to obtain the impregnation slurry.
8. The method for preparing the surface-pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein in the step 4, the impregnated tire nets obtained in the step 2 are arranged on the upper surface and the lower surface of the carbon/carbon composite material obtained in the step 1, and are subjected to hot press molding.
9. The method for preparing the surface-pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein the hot-pressing temperature in step 4 is 160-180 ℃, the time is 0.5-1h, and the pressure is 3MPa-5 MPa.
10. The method for preparing the surface-pure ceramic layer carbon/ceramic brake disc as claimed in claim 1, wherein in the step 5, the reaction temperature of siliconizing treatment is 1200-1900 ℃, the holding time is 0.5-4 h, and the disc is naturally cooled to room temperature along with the furnace.
CN201910998807.1A 2019-10-21 2019-10-21 Preparation method of carbon/ceramic brake disc with pure ceramic layer on surface Pending CN110606763A (en)

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CN112358312A (en) * 2020-10-29 2021-02-12 湖南金博碳素股份有限公司 Carbon/carbon electrode material and preparation method and application thereof
CN114685169A (en) * 2020-12-29 2022-07-01 中国科学院上海硅酸盐研究所 Preparation method of fiber-reinforced silicon carbide ceramic matrix composite based on slurry lamination design
CN113847365A (en) * 2021-09-29 2021-12-28 湖南世鑫新材料有限公司 Carbon-ceramic brake disc with multilayer structure and preparation method thereof
CN113847365B (en) * 2021-09-29 2024-02-09 湖南世鑫新材料有限公司 Carbon ceramic brake disc with multilayer structure and preparation method thereof
WO2023237976A1 (en) * 2022-06-07 2023-12-14 Brembo S.P.A. Shaped material and manufacturing method thereof
CN115974572A (en) * 2022-12-28 2023-04-18 西安鑫垚陶瓷复合材料股份有限公司 Low-cost short-period braking material and preparation method thereof
CN115974572B (en) * 2022-12-28 2023-11-17 西安鑫垚陶瓷复合材料股份有限公司 Low-cost short-period braking material and preparation method thereof
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CN116217257A (en) * 2023-03-10 2023-06-06 西安航空制动科技有限公司 Preparation method of pure-net-tire-structure carbon/ceramic composite material brake disc blank
CN116768643A (en) * 2023-05-11 2023-09-19 湖南博云新材料股份有限公司 Low-noise carbon ceramic brake disc for aviation and preparation method thereof

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