CN111362714A - Preparation method of carbon-ceramic brake disc - Google Patents
Preparation method of carbon-ceramic brake disc Download PDFInfo
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- CN111362714A CN111362714A CN202010190744.XA CN202010190744A CN111362714A CN 111362714 A CN111362714 A CN 111362714A CN 202010190744 A CN202010190744 A CN 202010190744A CN 111362714 A CN111362714 A CN 111362714A
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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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
- F16D65/125—Discs; Drums for disc brakes characterised by the material used for the disc body
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- 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
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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- 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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- 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
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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
- F16D2200/0039—Ceramics
- F16D2200/0047—Ceramic composite, e.g. C/C composite infiltrated with Si or B, or ceramic matrix infiltrated with metal
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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
- F16D2200/0082—Production methods therefor
Abstract
The invention discloses a preparation method of a carbon ceramic brake disc, which comprises the following steps of ① preparing a carbon fiber preform, ② CVI densification, namely loading the prepared carbon fiber preform into a CVI furnace, taking natural gas as carbon source gas, carrying out CVI densification, carrying out predeposition, accelerated deposition and gap-adjusting deposition to obtain a C/C brake disc, ③ graphitization treatment, namely placing the C/C brake disc into a high-temperature heat treatment furnace to obtain the required carbon ceramic brake disc, wherein the density and the porosity of the carbon ceramic preform can be accurately and effectively controlled, and the density of the carbon ceramic preform prepared by the method can be accurately controlled to be (1.45 +/-0.05) g/cm3The open porosity was (25. + -. 5)%.
Description
Technical Field
The invention belongs to the field of carbon-ceramic composite material braking, and particularly relates to a preparation method of a carbon-ceramic brake disc.
Background
The carbon-ceramic composite brake material is a new type composite material formed by using high-strength carbon fiber as reinforcement and using pyrolytic carbon and silicon carbide as matrix and combining two phases or multiple phases, and said material integrates the advantages of powder metallurgy brake material and C/C brake material into one body, and can effectively overcome the defects of above-mentioned two materials, and possesses the advantages of light weight, high specific strength, large specific heat, stable friction property and stable mechanical property, etc., in particular, it possesses high impact toughness and strong seawater and salt fog corrosion resistance.
Currently, carbon-ceramic brake discs are being studied by some major developed countries internationally to replace the C/C brake discs currently in use. The key laboratory in oak ridge in the united states has united other research institutions and developed carbon-ceramic brake discs for the fourth generation of fighters. The German space navigation institute (DLR) and SGL company take a brake disc of a high-grade car as a background, introduce SiC powder, and prepare a carbon-ceramic brake disc by an RMI process, and the SiC powder is successfully applied to high-grade automobiles such as the Kyokejie 911 type automobile and a new Audi A8L. The research on carbon-ceramic brake discs is also in focus in China, and the research on the carbon-ceramic brake discs has been carried out by aeronautical industry 514 factories, northwest industrial university, middle and south university and the like by taking aircraft brake pads as backgrounds, wherein the carbon-ceramic brake discs of certain types of airplanes developed by the aeronautical industry 514 factories are successfully flown with airplanes for the first time.
For example, patent No. CN109095929A discloses a method for preparing a carbon-ceramic brake disc, which comprises preparing a low-density C/C composite material by a vapor deposition method, preparing a carbon/ceramic brake disc by a precursor impregnation cracking method and a melt siliconizing method, and finally processing and molding the carbon-ceramic composite material to obtain the carbon-ceramic brake disc. However, the carbon-ceramic brake material has high hardness, which results in time-consuming processing, severe cutter loss and extremely high processing cost. In addition, post-processing belongs to material reduction manufacturing, so that the material utilization rate is reduced, and the cost of the brake disc is increased. The most common method for preparing the carbon-ceramic brake disc at present is to prepare C/C + RMI by adopting CVI, and the basic idea is to prepare a C matrix by adopting a CVI method to form a C/C composite material, and then permeate a C/C porous body with liquid silicon to react to obtain a SiC matrix, so that the carbon-ceramic brake disc is prepared. A very key process for preparing the carbon-ceramic brake disc by adopting the process is how to prepare a proper and effective C/C blank. Since the density and pore distribution of the C/C bodies directly affect the subsequent RMI reaction.
This is because too high C/C density inevitably results in less pores, insufficient reaction of Si with pyrolytic carbon results in partial Si residue, and the residual Si inevitably affects the frictional wear properties of the product; the C/C density is too low, the pores are large, and Si can continuously react with carbon fibers after the reaction with pyrolytic carbon is finished, so that the overall strength of the material is damaged.
Disclosure of Invention
In view of the above, the invention aims to optimize the density and porosity of the porous C/C of the carbon-ceramic brake disc blank by designing a reasonable CVI process.
The technical scheme adopted by the invention is as follows: a preparation method of a carbon-ceramic brake disc comprises the following steps:
① the carbon fiber preform is prepared by compounding weftless unidirectional carbon cloth with carbon fiber net, laying and laminating at 0 deg./60 deg./120 deg. in the direction of carbon cloth fiber to form a layer with thickness of 15-25 mm and ensuring (15 + -1) layer/cm, bulk density of 0.6 + -0.03 g/cm3。
② CVI densification the carbon fibre preform prepared as described above was first loaded into a CVI furnace and CVI densification was carried out using natural gas as the carbon source gas, in 3 stages as follows:
A. and (4) performing preliminary deposition.
The purpose of this step is to make all carbon fiber surfaces evenly coated with a layer of compact pyrolytic carbon, and the specific process parameters are as follows: deposition temperature: 1000-1020 ℃; main gas flow rate: natural gas 40-80 SLM; flow rate of the assist gas: ethane 20-40 SLM; hearth pressure: (2 +/-0.5) kPa; deposition time: 50-100 h.
B. The deposition is accelerated.
The deposition of pyrolytic carbon is mainly accelerated at this stage to ensure sufficient pyrolytic carbon for later reaction with Si, and the specific process is as follows: deposition temperature: 1000-1020 ℃; main gas flow rate: natural gas 50-100 SLM; flow rate of the assist gas: propane 30-60 SLM; hearth pressure: (4. + -. 0.5) kPa; deposition time: 150-200 h.
C. And (4) gap adjusting deposition.
The deposition of pyrolytic carbon is mainly accelerated at the stage so as to ensure that enough pyrolytic carbon is available for later reaction with Si, and the specific process is as follows: deposition temperature: (1010 + -5) deg.C; main gas flow rate: natural gas 30-60 SLM; flow rate of the assist gas: ethane 10-20 SLM, propane 5-15 SLM; hearth pressure: (3 +/-0.5) kPa; deposition time: and (50 +/-10 h).
③ graphitizing.
And (3) placing the brake disc subjected to densification treatment into a high-temperature heat treatment furnace for graphitization treatment to obtain the required carbon-ceramic brake disc. The method comprises the following specific steps: A. vacuumizing until the vacuum value is less than or equal to 100Pa, maintaining the pressure for 12h, and then raising the temperature until the vacuum value is less than or equal to 1 kPa; B. heating to 1300 ℃ at the heating rate of 200 ℃/h, filling Ar gas to the furnace pressure (-0.05) MPa (-0.03) MPa, stopping the Ar gas, continuously heating to 2100 ℃ at the heating rate of 100 ℃/h, and preserving the heat for 1 h-4 h; C. cooling to below 150 ℃, discharging, and obtaining the required carbon-ceramic brake disc.
Compared with the traditional process, the invention has the following advantages:
⑴ the fiber distribution is more uniform and reasonable, and the matrix pyrolytic carbon is also uniformly distributed;
⑵ can accurately and effectively control the density and the open pore rate of the carbon ceramic preform, and the density of the carbon ceramic preform prepared by the method can be accurately controlled to be (1.45 +/-0.05) g/cm3The open porosity was (25. + -. 5)%.
The present invention will be described in more detail with reference to the following examples.
Detailed Description
Example (b):
testing a carbon-ceramic brake disc of a certain airplane.
⑴ A carbon fiber preform for a certain type of airplane is first prepared as follows:
the carbon fiber is 12K carbon fiber, laid in 0 deg/60 deg/120 deg and laminated in the fiber direction of the carbon cloth, and laid in the thickness of 20mm, 23mm and 25mm to ensure 15 +/-1 layer/cm and 0.6 +/-0.03 g/cm3(ii) a Respectively cutting 4, 4 and 7 parts according to the specifications of single static part, double static part and movable disc of a certain type of carbon-ceramic brake disc.
⑵ are densified by CVI.
Loading the prepared carbon fiber blank into a CVI furnace, performing CVI densification by using natural gas as a carbon source gas, and performing the following operations in 3 stages:
① are pre-deposited.
The purpose of this step is to make all carbon fiber surfaces evenly coated with a layer of compact pyrolytic carbon, and the specific process is as follows:
deposition temperature: (1005. + -. 5) ℃ C;
main gas flow rate: natural gas (50 ± 10) SLM;
flow rate of the assist gas: ethane (20 ± 5) SLM;
hearth pressure: (2 +/-0.5) kPa;
deposition time: (100 +/-10) h.
B. The deposition is accelerated.
The deposition of pyrolytic carbon is mainly accelerated at this stage to ensure sufficient pyrolytic carbon for later reaction with Si, and the specific process is as follows:
deposition temperature: (1015. + -. 5) ℃ C;
main gas flow rate: natural gas (80 ± 10) SLM;
flow rate of the assist gas: propane (40 ± 5) SLM;
hearth pressure: (4. + -. 0.5) kPa;
deposition time: (200 +/-10) h.
C. And (4) gap adjusting deposition.
The deposition of pyrolytic carbon is mainly accelerated at the stage so as to ensure that enough pyrolytic carbon is available for later reaction with Si, and the specific process is as follows:
deposition temperature: (1010 + -5) deg.C;
main gas flow rate: natural gas (50 ± 10) SLM;
flow rate of the assist gas: ethane (20 + -5) SLM, propane (10 + -5) SLM;
hearth pressure: (3 +/-0.5) kPa;
deposition time: (50 +/-10) h.
After the three stages of CVI densification, the density and the open porosity of 15 pieces of C/C are respectively measured as follows:
table 1: statistical table for density and open pore rate of carbon-ceramic brake disc blank of certain airplane
| Plate number | Density (g/cm)3) | Open porosity (%) |
| DJ1 | 1.51 | 24.3 |
| DJ2 | 1.52 | 24.1 |
| SJ1 | 1.48 | 26.4 |
| SJ2 | 1.48 | 26.2 |
| SJ3 | 1.49 | 25.4 |
| D1 | 1.48 | 26.2 |
| D2 | 1.47 | 27.1 |
| D3 | 1.48 | 26.5 |
| D4 | 1.48 | 26.6 |
⑶ graphitizing.
The C/C brake disc is placed into a high-temperature heat treatment furnace for graphitization treatment, and the porous C/C of the blank of the carbon-ceramic brake disc can be obtained, and the method specifically comprises the following steps:
① vacuumizing to a vacuum value of less than or equal to 100Pa, maintaining the pressure for 12h, and heating when the vacuum value is less than or equal to 1 kPa;
② heating to 1300 deg.C at a heating rate of 200 deg.C/h, charging Ar gas to furnace pressure (-0.05) MPa (-0.03) MPa, stopping Ar gas, heating to 2100 deg.C at a heating rate of 100 deg.C/h, and maintaining for 1-4 h;
③, cooling to below 150 ℃, discharging, and obtaining the porous C/C of the blank body of the carbon-ceramic brake disc.
The present invention has been described above by way of example. It is to be understood that the specific implementations of the invention are not limited in this respect. The invention is not limited to the specific embodiments described above, but rather, the invention is applicable to other applications without any substantial or substantial modification.
Claims (4)
1. The preparation method of the carbon-ceramic brake disc is characterized by comprising the following steps:
① preparing carbon fiber preform by compounding weftless unidirectional carbon cloth with carbon fiber net, laying and laminating at 0 deg./60 deg./120 deg. in the direction of carbon cloth fiber to form a layer/cm with thickness of 15-25 mm and volume density of 0.6 + -0.03 g/cm3；
② CVI densification, namely loading the prepared carbon fiber preform into a CVI furnace, performing CVI densification by using natural gas as a carbon source gas, and performing predeposition, accelerated deposition and gap-adjusting deposition to obtain a C/C brake disc;
③ graphitization treatment, namely putting the C/C brake disc into a high temperature heat treatment furnace, vacuumizing until the vacuum value is less than or equal to 100Pa, maintaining the pressure for 12h, then requiring the vacuum value to be less than or equal to 1kPa, heating to 1300 ℃ at the heating rate of 200 ℃/h, filling Ar gas to the furnace pressure (-0.05) MPa (-0.03) MPa, stopping the Ar gas, continuing heating to 2100 ℃ at the heating rate of 100 ℃/h, preserving the temperature for 1 h-4 h, and cooling to below 150 ℃ to obtain the required carbon-ceramic brake disc.
2. A method for preparing a carbon-ceramic brake disc as claimed in claim 1, wherein the pre-deposition process in step ② is carried out to uniformly coat the surface of all carbon fibers with a layer of dense pyrolytic carbon, and the process parameters include deposition temperature of 1000-1020 ℃, main gas flow of 40-80 SLM natural gas, auxiliary gas flow of 20-40 SLM ethane, furnace pressure of 2 +/-0.5 kPa, and deposition time of 50-100 h.
3. A method for preparing a carbon-ceramic brake disc as claimed in claim 1, wherein the deposition acceleration step ② is carried out by accelerating the deposition of pyrolytic carbon to ensure sufficient pyrolytic carbon for the later reaction with Si, and the process parameters are deposition temperature of 1000-1020 ℃, main gas flow of 50-100 SLM for natural gas, auxiliary gas flow of 30-60 SLM for propane, furnace pressure of 4 +/-0.5 kPa, and deposition time of 150-200 h.
4. The method for preparing a carbon-ceramic brake disc as claimed in claim 1, wherein the step ② is carried out by accelerating the deposition of pyrolytic carbon to ensure sufficient pyrolytic carbon for the later reaction with Si, and the process parameters comprise (1010 +/-5) deg.C, natural gas 30-60 SLM as main gas flow, ethane 10-20 SLM and propane 5-15 SLM as auxiliary gas flow, (3 +/-0.5) kPa as furnace pressure, and (50 +/-10 h) deposition time.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115745617A (en) * | 2022-11-29 | 2023-03-07 | 烟台鲁航炭材料科技有限公司 | C/SiC ceramic matrix composite with high friction performance and preparation method thereof |
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| CN103172398A (en) * | 2012-04-07 | 2013-06-26 | 西安航空制动科技有限公司 | Surface treatment method of fiber for carbon brake disc |
| CN105198473A (en) * | 2015-05-11 | 2015-12-30 | 西安航空制动科技有限公司 | Preparation method of carbon/carbon brake disc |
| CN107445641A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of preparation method of carbon brake disc |
| CN107445638A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of preparation method of carbon/carbon brake disc |
| CN109133956A (en) * | 2018-08-03 | 2019-01-04 | 深圳勒迈科技有限公司 | The preparation method of C/C-SiC composite material automobile brake disc |
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| CN115745617A (en) * | 2022-11-29 | 2023-03-07 | 烟台鲁航炭材料科技有限公司 | C/SiC ceramic matrix composite with high friction performance and preparation method thereof |
| CN115745617B (en) * | 2022-11-29 | 2023-08-22 | 烟台鲁航炭材料科技有限公司 | C/SiC ceramic matrix composite material with high friction performance and preparation method thereof |
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