CN102537155A - C/C-SiC-ZrC-ZrB2 complex-phase ceramic-based frictional braking material and preparation method thereof - Google Patents
C/C-SiC-ZrC-ZrB2 complex-phase ceramic-based frictional braking material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a C/C-SiC-ZrC-ZrB2 complex-phase ceramic-based frictional braking material and a preparation method thereof. The frictional braking material comprises a carbon-fibre prefabricated body comprising carbon fibre and a ceramic matrix, wherein a carbon interface layer is additionally deposited on the surface of the carbon fibre of the carbon-fibre prefabricated body; and the ceramic matrix is formed on the carbon-fibre prefabricated body. According to the complex-phase ceramic-based frictional braking material disclosed by the invention, the wet-state service performance of a traditional carbon/carbon braking material can be effectively improved, and the service life is prolonged.
Description
Technical field
The present invention relates in general to friction braking material.Specifically, relate to the for example complex phase ceramic base friction braking material of braking such as aircraft, bullet train usefulness of rapid.
Background technique
Friction material is the brake material of the break, clutch and the friction gearing that are used for various transport facilitys and machinery equipment.In these braking device, utilize the frictional behaviour of friction material that the kinetic energy that rotates is converted into the energy of heat energy or other form, thereby make the slewing gear braking.Desirable braking material should have following performance: enough and stable friction factor; High thermal conductivity and heat resistance; High wear resistance; Good oil resistant, wet and corrosion ability; Enough intensity; When carrying out rubbing contact, produce and seldom or not produce noise with the parts of being fitted; Do not cohere at work or interlock; The raw material source is abundant, and cost performance is high, and having favorable manufacturability can wait.
At high speed brake field (like aircraft, bullet train and Gran turismo), there are shortcomings such as quality weight and heat-resisting ability difference in traditional powder metallurgy braking material; Carbon/carbon (C/C) composite material that develops after the seventies in 20th century because light weight, can carry high, high temperature resistant energy by force, characteristics such as long service life, become present widely used aircraft brake material.But when in moist and salt mist environment, using, friction factor sharply descends, and makes braking quality unstable, is difficult to satisfy the demand of the round-the-clock and complicated military service of aircraft.In addition, the C/C composite material also need design inoxidzable coating because its pyro-oxidation resistance is poor when the preparation braking material.
Summary of the invention
The object of the present invention is to provide a kind of novel friction braking material, it can improve the green property and/or the pyro-oxidation resistance of above-mentioned C/C braking material.
According to an aspect of the present invention, a kind of friction braking material is provided, it comprises:
Prefabricated carbon fiber body by graphite fiber constitutes wherein deposits the carbon interface layer in addition on the carbon fiber surface of prefabricated carbon fiber body; With
The ceramic matrix that on the prefabricated carbon fiber body, forms (ceramic matrix and the prefabricated carbon fiber bodily form are integral, promptly attached on the prefabricated carbon fiber body and the internal voids of filling carbon fiber precast body).
The carbon interface layer can be the RESEARCH OF PYROCARBON that on carbon fiber surface, forms through chemical vapor deposition method.
Ceramic matrix can be SiC-ZrC-ZrB
2Complex phase ceramic.The preferably ceramic matrix is that the prefabricated carbon fiber body is immersed in SiC-ZrC-ZrB
2Form in the complex phase ceramic precursor solution and through firing behind the crosslinking curing.
The density of prefabricated carbon fiber body is preferably at 0.2~1.0g/cm
3Between, and the global density of friction braking material is preferably at 1.9~3.0g/cm
3Between.
The thickness of carbon interface layer is preferably between 0.1~10 μ m.
The prefabricated carbon fiber body can be for forming through continuous needle behind no latitude carbon cloth and the carbon fibre web tire lamination again, the overall structure fabric that also can be compiled into for graphite fiber.
The friction factor of friction braking material is preferably between 0.1~0.6.
The open-cell porosity of friction braking material is preferably less than 10%.
According to a further aspect in the invention, a kind of preparation method of friction braking material is provided, has comprised:
Adopt graphite fiber to constitute the prefabricated carbon fiber body;
Chemical vapor carbon deposition interface layer on the carbon fiber surface of prefabricated carbon fiber body;
Preparation liquid phase ceramic forerunner;
The prefabricated carbon fiber body that deposits the carbon interface layer is immersed in the liquid phase ceramic forerunner;
Prefabricated carbon fiber body behind the maceration extract phase ceramics precursor is carried out crosslinking curing to be handled; And
Thereby the material of crosslinking curing being handled the back gained carries out ceramic treatment formation friction braking material.
This method can also comprise: repeated impregnations, crosslinking curing handle and the ceramic treatment step no longer increases until the density of the friction braking material of final gained; Perhaps, repeated impregnations, crosslinking curing handle and the ceramic treatment step until the open-cell porosity of the friction braking material of final gained less than 10%.
The molding mode of prefabricated carbon fiber body and volume fraction have very big influence to the mechanical property and the frictional behaviour of final friction material.In the present invention, can be with constituting the prefabricated carbon fiber body through continuous needle again behind no latitude carbon cloth and the carbon fibre web tire lamination; Also can be compiled into the overall structure fabric and constitute the prefabricated carbon fiber body with graphite fiber.
The chemical vapor deposition step can comprise: with hydrocarbon gas (for example methane or propane) is carbon source; Adopt the isothermal chemical vapor deposition method at carbon fiber surface pyrolytic deposition carbon interface layer; Depositing temperature is 900~1100 ℃; Stagnation pressure is 5~10kPa, and the hydrocarbon gas flow is 2~4L/min, and sedimentation time is 10~20h.
Preparation liquid phase ceramic forerunner step can comprise: respectively with Polycarbosilane, gather carbon zirconium oxygen alkane and gather carbon boron azane and be dissolved in by 50% mass ratio and be prepared into corresponding precursor solution in toluene or the xylene solvent, again three kinds of precursor solutions are configured to SiC-ZrC-ZrB by required proportioning
2The liquid phase ceramic forerunner.
Impregnation steps can comprise: the prefabricated carbon fiber body vacuum impregnation that will deposit the carbon interface layer is in the liquid phase ceramic forerunner that configures, and the temperature of liquid phase ceramic forerunner is 50 ℃, and vacuum degree control is below 1kPa, and dip time is 2h.
The crosslinking curing treatment step can comprise: the material that will flood the back gained carries out crosslinking curing in baking oven handles, and temperature is 60~120 ℃, and the time is 3h, and atmosphere is atmosphere environment.
The ceramic treatment step can comprise: the material of gained behind the crosslinking curing is put into heat treatment furnace, and the heating rate of heat treatment furnace is 2 ℃/min, and heat treatment temperature is 1500 ℃, and holding time is 2h, and heat-treating atmosphere is an argon gas atmosphere.
As stated, in the present invention, in order to keep the excellent mechanical property of friction material, the combination interface of prefabricated carbon fiber body and complex phase ceramic matrix preparation in addition has one deck RESEARCH OF PYROCARBON interface layer.The carbon interface layer can play on the one hand in preparation complex phase ceramic matrix process the protective action to graphite fiber; The strong combination between graphite fiber and the complex phase ceramic matrix can be prevented on the other hand, thereby the excellent toughness of material can be kept.
Same existing C/C aircraft brake material is compared, and the friction braking material that obtains according to the present invention has following advantage:
(1) matrix adopting complex phase ceramic has overcome the carbon base body shortcoming that friction factor sharply descends under hygrometric state condition, because the high temperature oxidation resistance of complex phase ceramic self need not prepare inoxidzable coating, has simplified manufacturing process simultaneously;
(2) ceramic matrix is by SiC, ZrC and ZrB
2Three kinds of components are composited, and the friction factor of prepared brake material can be regulated between 0.1~0.6 as required, thereby can be applicable to the performance requirement of the different traffic tool to braking material more widely.
Description of drawings
Fig. 1 is C/C-SiC-ZrC-ZrB of the present invention
2The typical microstructure photo of complex phase ceramic base friction braking material; And
Fig. 2 is C/C-SiC-ZrC-ZrB of the present invention
2The typical case of the complex phase ceramic base friction braking material curve that brakes.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.It will be appreciated by those skilled in the art that the following embodiment who illustrates for example only is used to explain the present invention but not is used for it is made any restriction.For example, the order of each step that describes below is also not exclusive and unmodifiable, can embodiment of the present invention as long as it meets normal logical order.In addition, though with SiC-ZrC-ZrB
2The complex phase ceramic base is that example has specified the present invention, but it will be understood by those skilled in the art that friction braking material of the present invention also can adopt other any suitable ceramic matrix.
Embodiment 1
The prefabricated carbon fiber body adopts T700 12K PANCF not have the latitude carbon cloth and one deck T700 12KPANCF carbon fibre web tire is compound, forms the overall structure fabric through continuous needle, and volume density is 0.28g/cm
3
With methane is carbon source, adopts the carbon fiber surface deposition RESEARCH OF PYROCARBON interface layer of chemical vapor deposition stove at the prefabricated carbon fiber body.Process conditions are following: depositing temperature is 1000 ℃, and stagnation pressure is 5kPa; Methane flow is 2L/min, and sedimentation time is 20h; The volume density that obtains material after the deposition is 0.55g/cm
3
With Polycarbosilane, to gather carbon zirconium oxygen alkane, gather carbon boron azane be the complex phase ceramic precursor, is configured to solution with xylol by mass ratio 50% respectively, three kinds of solution mixed at 1: 4: 4 being made into the complex phase ceramic precursor solution again by mass ratio.The prefabricated carbon fiber body that has deposited the RESEARCH OF PYROCARBON interface layer is placed vacuum vessel, add the complex phase ceramic precursor solution and flood; The temperature of complex phase ceramic precursor solution is 50 ℃ during dipping, and vacuum degree control keeps 2h below 1kPa.Placing baking oven to carry out crosslinking curing the material behind the dipping handles; Crosslinking temperature is 60 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material behind the crosslinking curing is put into heat treatment furnace carry out ceramic treatment, heating rate is 2 ℃/min, and heat treatment temperature is 1500 ℃, and holding time is 2h, and heat-treating atmosphere is the argon gas inert atmosphere.Material after the potteryization is carried out ultrasonic cleaning, remove the surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step till the open-cell porosity of final gained friction braking material is less than 10%.
Embodiment 2
The prefabricated carbon fiber body adopts T700 12K PANCF not have the latitude carbon cloth and one deck T700 12KPANCF carbon fibre web tire is compound, forms the overall structure fabric through continuous needle, and volume density is 0.50g/cm
3
With propane is carbon source, adopts the carbon fiber surface deposition RESEARCH OF PYROCARBON interface layer of chemical vapor deposition stove at the prefabricated carbon fiber body.Process conditions are following: depositing temperature is 950 ℃, and stagnation pressure is 10kPa, and the propane flow is 4L/min, and sedimentation time is 10h, and the volume density of deposition back material is 0.81g/cm
3
With Polycarbosilane, to gather carbon zirconium oxygen alkane, gather carbon boron azane be the complex phase ceramic precursor, is configured to solution with xylol by mass ratio 50% respectively, three's solution mixed at 1: 4: 2 being made into the complex phase ceramic precursor solution again by mass ratio.With the vacuum vessel that places of the prefabricated carbon fiber body that has deposited the RESEARCH OF PYROCARBON interface layer, add the complex phase ceramic precursor solution and flood; To drive the temperature of liquid solution be 50 ℃ to complex phase ceramic before during dipping, and vacuum degree control keeps 2h below 1kPa.Placing baking oven to carry out crosslinking curing the material behind the dipping handles; Crosslinking temperature is 80 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material behind the crosslinking curing is put into heat treatment furnace carry out ceramic treatment, heating rate is 2 ℃/min, and heat treatment temperature is 1500 ℃, and holding time is 2h, and heat-treating atmosphere is the argon gas inert atmosphere.Material after the potteryization is carried out ultrasonic cleaning, remove the surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step till the density of final gained friction braking material no longer increases.
Embodiment 3
The prefabricated carbon fiber body adopts the T700 carbon fiber knit to become 2.5D overall structure fabric, and volume density is 0.82g/cm
3
With propane is carbon source, adopts chemical vapor deposition stove to prepare the RESEARCH OF PYROCARBON interface layer at the carbon fiber surface of prefabricated carbon fiber body.Process conditions are following: depositing temperature is 950 ℃; Stagnation pressure is 10kPa; The propane flow is 4L/min; Sedimentation time is 10h, and the density of deposition back material reaches 1.1g/cm
3
With Polycarbosilane, to gather carbon zirconium oxygen alkane, gather carbon boron azane be the complex phase ceramic precursor, is configured to solution with toluene by mass ratio 50% respectively, three's solution mixed at 1: 2: 4 being made into the complex phase ceramic precursor solution again by mass ratio.The prefabricated carbon fiber body that has deposited the RESEARCH OF PYROCARBON interface layer is placed vacuum vessel, add the complex phase ceramic precursor solution and flood; The temperature of complex phase ceramic precursor solution is 50 ℃ during dipping, and vacuum degree control keeps 2h below 1kPa.Placing baking oven to carry out crosslinking curing the material behind the dipping handles; Crosslinking temperature is 120 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material behind the crosslinking curing is put into heat treatment furnace carry out ceramic treatment, heating rate is 2 ℃/min, and heat treatment temperature is 1500 ℃, and holding time is 2h, and heat-treating atmosphere is the argon gas inert atmosphere.Material after the potteryization is carried out ultrasonic cleaning, remove the surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step till the open-cell porosity of final gained friction braking material is less than 10%.
Fig. 1 is the C/C-SiC-ZrC-ZrB through above-mentioned prepared
2The typical microstructure of complex phase ceramic base friction braking material, the zone after white box is amplified among the corresponding left figure of right figure.Black part is divided into graphite fiber and RESEARCH OF PYROCARBON among the figure, and grey color part is the SiC phase, and white portion is ZrC and ZrB
2Phase.In the friction braking material in the present invention, graphite fiber plays and strengthens toughness reinforcing effect; SiC-ZrC-ZrB
2Three-phase is nanometer disperse distribution in the complex phase ceramic matrix, when friction catch produces high temperature, can form the ceramic coating of self-healing, thereby can improve the high-temperature oxidation resistance of C/C composite material.
Adopt the MM-1000 frictional testing machine to test the braking quality of friction braking material of the present invention, test condition is: inertia 3.8kgfcms
2, specific pressure 100N/cm
2, linear velocity 25m/s, the test of simulated aircraft normal braking.Typical case's brake curve is seen Fig. 2.Test result shows, complex phase ceramic base braking material stable friction factor of the present invention; The particularly important is, than the dry friction test, in the wet friction test, the friction factor of brake disc slightly promotes, and this result is superior to present C/C composite material brake disc.
The The performance test results of the friction braking material for preparing in the embodiments of the invention is as shown in table 1, and wherein Comparative Examples is the C/C braking material.
Table 1: the The performance test results of friction braking material
Performance parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples |
Density (g/cm 3) | ?2.25 | ?2.01 | ?2.46 | ?1.70 |
Flexural strength (MPa) | ?156 | ?178 | ?184 | ?160 |
Average dry friction coefficient | ?0.25 | ?0.15 | ?0.45 | ?0.42 |
Average wet friction coefficient | ?0.27 | ?0.21 | ?0.48 | ?0.15 |
Wear rate (g/ face) | ?+0.25 | ?+0.05 | ?+0.02 | ?-0.05 |
The performance test results shows: C/C-SiC-ZrC-ZrB of the present invention
2The friction factor of complex phase ceramic base friction braking material can be regulated in the scope of broad, and wet friction coefficient ratio dry friction coefficient slightly improves, and the wet friction coefficient of the C/C braking material of Comparative Examples sharply descends than dry friction coefficient.Friction braking material of the present invention is owing to formed oxide film in friction process, wear rate shows as weightening finish, and Comparative Examples C/C braking material is because the oxidation weight loss of material with carbon element, and wear rate is a negative value.
In sum, complex phase ceramic base friction braking material of the present invention can improve the hygrometric state military service performance of existing C/C braking material effectively, increases the service life.
Claims (10)
1. friction braking material comprises:
Prefabricated carbon fiber body by graphite fiber constitutes wherein deposits the carbon interface layer in addition on the carbon fiber surface of prefabricated carbon fiber body; With
The ceramic matrix that on the prefabricated carbon fiber body, forms.
2. friction braking material according to claim 1, wherein ceramic matrix is SiC-ZrC-ZrB
2Complex phase ceramic.
3. according to the friction braking material of claim 2, wherein the density of prefabricated carbon fiber body is at 0.2~1.0g/cm
3Between, and the global density of friction braking material is at 1.9~3.0g/cm
3Between.
4. according to the friction braking material of claim 2, wherein the thickness of carbon interface layer is between 0.1~10 μ m.
5. according to the friction braking material of claim 2, wherein the friction factor of friction braking material is between 0.1~0.6.
6. the preparation method of a friction braking material comprises:
Adopt graphite fiber to constitute the prefabricated carbon fiber body;
Chemical vapor carbon deposition interface layer on the carbon fiber surface of prefabricated carbon fiber body;
Preparation liquid phase ceramic forerunner;
The prefabricated carbon fiber body that deposits the carbon interface layer is immersed in the liquid phase ceramic forerunner;
Prefabricated carbon fiber body behind the maceration extract phase ceramics precursor is carried out crosslinking curing to be handled; And
Thereby the material of crosslinking curing being handled the back gained carries out ceramic treatment formation friction braking material.
7. according to the method for claim 6, also comprise:
Repeated impregnations, crosslinking curing handle and the ceramic treatment step until the open-cell porosity of the friction braking material of final gained less than 10%.
8. according to the method for claim 6; Wherein chemical vapor deposition step comprises: be carbon source with the hydrocarbon gas; Adopt the isothermal chemical vapor deposition method at carbon fiber surface pyrolytic deposition carbon interface layer, depositing temperature is 900~1100 ℃, and stagnation pressure is 5~10kPa; The hydrocarbon gas flow is 2~4L/min, and sedimentation time is 10~20h.
9. according to the method for claim 6; Wherein preparing liquid phase ceramic forerunner step comprises: respectively with Polycarbosilane, gather carbon zirconium oxygen alkane and gather carbon boron azane and be dissolved in by 50% mass ratio and be prepared into corresponding precursor solution in toluene or the xylene solvent, again three kinds of precursor solutions are configured to SiC-ZrC-ZrB by required proportioning
2The liquid phase ceramic forerunner.
10. according to the method for claim 6; Wherein the ceramic treatment step comprises: the material of gained behind the crosslinking curing is put into heat treatment furnace, and the heating rate of heat treatment furnace is 2 ℃/min, and heat treatment temperature is 1500 ℃; Holding time is 2h, and heat-treating atmosphere is an argon gas atmosphere.
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CN201310690282.8A CN103693984B (en) | 2011-12-29 | 2011-12-29 | Fibre reinforced complex phase ceramic base friction braking material and preparation method thereof |
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CN103693984A (en) | 2014-04-02 |
CN103693984B (en) | 2015-08-26 |
CN102537155B (en) | 2014-02-26 |
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