CN102537155B - 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, the complex phase ceramic base friction braking material that relates to the braking use such as rapid such as aircraft, bullet train.
Background technique
Friction material is the brake material for the break of various transport facilitys and machinery equipment, clutch and friction gearing.In these braking device, the energy that the frictional behaviour of utilizing friction material is heat energy or other form by the kinetic transformation rotating, thus make 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 the parts with being fitted carry out rubbing contact, generation seldom or not produces noise; Do not cohere at work or interlock; Raw material source is abundant, and cost performance is high, has good technology capability etc.
At high speed brake field (as aircraft, bullet train and Gran turismo), there is the shortcomings such as the heavy and heat-resisting ability of quality is poor in traditional powder metallurgy braking material; Carbon/carbon (C/C) composite material of 20 century 70s development later, because quality is light, can carry the features such as high, high temperature resistant energy is strong, long service life, becomes now widely used aircraft brake material.But while using, friction factor sharply declines, and makes braking quality unstable, be difficult to meet the demand of the round-the-clock and complicated military service of aircraft in moist and salt mist environment.In addition, C/C composite material, because its pyro-oxidation resistance is poor, also needs to design inoxidzable coating when preparing 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 green property and/or the pyro-oxidation resistance of above-mentioned C/C braking material.
According to an aspect of the present invention, provide a kind of friction braking material, it comprises:
The carbon fabric perform consisting of carbon fiber wherein deposits in addition carbon interface layer on the carbon fiber surface of carbon fabric perform; With
The ceramic matrix forming on carbon fabric perform (ceramic matrix and carbon fabric perform form one, are attached on carbon fabric perform and the internal voids of filling carbon fiber precast body).
Carbon interface layer can be the RESEARCH OF PYROCARBON forming on carbon fiber surface by chemical vapor deposition method.
Ceramic matrix can be SiC-ZrC-ZrB
2complex phase ceramic.Preferably ceramic matrix is that carbon fabric perform is immersed in to SiC-ZrC-ZrB
2in complex phase ceramic precursor solution and by firing and form after crosslinking curing.
The density of carbon fabric perform 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.
Carbon fabric perform can be for without forming through continuous needle after latitude carbon cloth and carbon fibre web tire lamination again, the overall structure fabric that also can be compiled into for carbon 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, provide a kind of preparation method of friction braking material, having comprised:
Adopt carbon fiber to form carbon fabric perform;
Chemical vapor carbon deposition interface layer on the carbon fiber surface of carbon fabric perform;
Preparation liquid phase ceramic forerunner;
The carbon fabric perform that deposits carbon interface layer is immersed in liquid phase ceramic forerunner;
Carbon fabric perform after maceration extract phase ceramics precursor is carried out to crosslinking curing processing; And
After crosslinking curing is processed, thereby the material of gained carries out ceramic treatment and forms friction braking material.
The method can also comprise: repeated impregnations, crosslinking curing process and ceramic treatment step until the density of the friction braking material of final gained no longer increase; Or repeated impregnations, crosslinking curing processing and ceramic treatment step are until the open-cell porosity of the friction braking material of final gained is less than 10%.
The molding mode of carbon fabric perform and volume fraction have a significant impact the mechanical property of final friction material and frictional behaviour.In the present invention, can be by without forming carbon fabric perform through continuous needle again after latitude carbon cloth and carbon fibre web tire lamination; Also can be compiled into overall structure fabric and form carbon fabric perform with carbon fiber.
Chemical vapor deposition step can comprise: the hydrocarbon gas (for example methane or propane) of take is carbon source, adopt isothermal chemical vapor deposition method at carbon fiber surface pyrolytic deposition carbon interface layer, depositing temperature is 900～1100 ℃, stagnation pressure is 5～10kPa, hydrocarbon gas flow is 2～4L/min, and sedimentation time is 10～20h.
Preparation liquid phase ceramic forerunner step can comprise: respectively Polycarbosilane, poly-carbon zirconium oxygen alkane and poly-carbon boron azane are dissolved in and in toluene or xylene solvent, are prepared into corresponding precursor solution by 50% mass ratio, then three kinds of precursor solutions are configured to SiC-ZrC-ZrB by required proportioning
2liquid phase ceramic forerunner.
Impregnation steps can comprise: by the carbon fabric perform vacuum impregnation that deposits carbon interface layer, in the liquid phase ceramic forerunner configuring, the temperature of liquid phase ceramic forerunner is 50 ℃, and vacuum degree control is below 1kPa, and dip time is 2h.
Crosslinking curing treatment step can comprise: the material of gained after dipping is carried out to crosslinking curing processing in baking oven, and temperature is 60～120 ℃, and the time is 3h, and atmosphere is atmosphere environment.
Ceramic treatment step can comprise: the material of gained after 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 argon gas atmosphere.
As mentioned above, in the present invention, in order to keep the mechanical property of friction material excellence, the combination interface of carbon fabric perform and complex phase ceramic matrix is prepared with one deck RESEARCH OF PYROCARBON interface layer in addition.Carbon interface layer can play the protective action to carbon fiber in preparing complex phase ceramic matrix process on the one hand; The strong combination between carbon fiber and complex phase ceramic matrix can be prevented on the other hand, thereby the excellent toughness of material can be kept.
With existing C/C aircraft brake material, compare, the friction braking material tool obtaining according to the present invention has the following advantages:
(1) matrix adopting complex phase ceramic, has overcome the carbon base body shortcoming that friction factor sharply declines under hygrometric state condition, due to the high temperature oxidation resistance of complex phase ceramic self, does not need to prepare inoxidzable coating simultaneously, has simplified manufacturing process;
(2) ceramic matrix is by SiC, ZrC and ZrB
2three kinds of components are composited, and the friction factor of prepared brake material can regulate as required between 0.1～0.6, thereby can be more widely applicable for the performance requirement of the different traffic tool to braking material.
Accompanying drawing explanation
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 brake cruve of complex phase ceramic base friction braking material.
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 is for example only for explaining the present invention but not for making any restriction to it.For example, the order of each step the following describes is also not exclusive and unmodifiable, as long as it meets normal logical order and can implement the present invention.In addition, although with SiC-ZrC-ZrB
2complex phase ceramic base is that example describes the present invention in detail, 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
Carbon fabric perform adopts T700 12K PANCF compound without latitude carbon cloth and one deck T700 12KPANCF carbon fibre web tire, through continuous needle, forms overall structure fabric, and volume density is 0.28g/cm
3.
Take methane as carbon source, adopt chemical vapor deposition stove at the carbon fiber surface deposition RESEARCH OF PYROCARBON interface layer of carbon fabric perform.Process conditions are as follows: 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 deposition is 0.55g/cm
3.
Take Polycarbosilane, poly-carbon zirconium oxygen alkane, poly-carbon boron azane is complex phase ceramic precursor, 50% is configured to solution in mass ratio respectively, then three kinds of solution are mixed and are made into complex phase ceramic precursor solution in mass ratio at 1: 4: 4 with dimethylbenzene.The carbon fabric perform that has deposited RESEARCH OF PYROCARBON interface layer is placed in to vacuum vessel, adds complex phase ceramic precursor solution to flood; During dipping, the temperature of complex phase ceramic precursor solution is 50 ℃, and vacuum degree control, below 1kPa, keeps 2h.Material after dipping is placed in to baking oven and carries out crosslinking curing processing; Crosslinking temperature is 60 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material after crosslinking curing is put into heat treatment furnace and 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 argon gas inert atmosphere.Material after ceramic is carried out to ultrasonic cleaning, remove surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step until the open-cell porosity of final gained friction braking material is less than 10%.
embodiment 2
Carbon fabric perform adopts T700 12K PANCF compound without latitude carbon cloth and one deck T700 12KPANCF carbon fibre web tire, through continuous needle, forms overall structure fabric, and volume density is 0.50g/cm
3.
Take propane as carbon source, adopt chemical vapor deposition stove at the carbon fiber surface deposition RESEARCH OF PYROCARBON interface layer of carbon fabric perform.Process conditions are as follows: depositing temperature is 950 ℃, and stagnation pressure is 10kPa, and propane flow is 4L/min, and sedimentation time is 10h, and after deposition, the volume density of material is 0.81g/cm
3.
Take Polycarbosilane, poly-carbon zirconium oxygen alkane, poly-carbon boron azane is complex phase ceramic precursor, 50% is configured to solution in mass ratio respectively, then three's solution is mixed and is made into complex phase ceramic precursor solution in mass ratio at 1: 4: 2 with dimethylbenzene.By deposited RESEARCH OF PYROCARBON interface layer carbon fabric perform be placed in vacuum vessel, add complex phase ceramic precursor solution to flood; Before during dipping, to drive the temperature of liquid solution be 50 ℃ to complex phase ceramic, and vacuum degree control, below 1kPa, keeps 2h.Material after dipping is placed in to baking oven and carries out crosslinking curing processing; Crosslinking temperature is 80 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material after crosslinking curing is put into heat treatment furnace and 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 argon gas inert atmosphere.Material after ceramic is carried out to ultrasonic cleaning, remove surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step until the density of final gained friction braking material no longer increases.
embodiment 3
Carbon fabric perform adopts T700 carbon fiber knit to become 2.5D overall structure fabric, and volume density is 0.82g/cm
3.
Take propane as carbon source, adopt chemical vapor deposition stove to prepare RESEARCH OF PYROCARBON interface layer at the carbon fiber surface of carbon fabric perform.Process conditions are as follows: depositing temperature is 950 ℃; Stagnation pressure is 10kPa; Propane flow is 4L/min; Sedimentation time is 10h, and after deposition, the density of material reaches 1.1g/cm
3.
Take Polycarbosilane, poly-carbon zirconium oxygen alkane, poly-carbon boron azane is complex phase ceramic precursor, 50% is configured to solution in mass ratio respectively, then three's solution is mixed and is made into complex phase ceramic precursor solution in mass ratio at 1: 2: 4 with toluene.The carbon fabric perform that has deposited RESEARCH OF PYROCARBON interface layer is placed in to vacuum vessel, adds complex phase ceramic precursor solution to flood; During dipping, the temperature of complex phase ceramic precursor solution is 50 ℃, and vacuum degree control, below 1kPa, keeps 2h.Material after dipping is placed in to baking oven and carries out crosslinking curing processing; Crosslinking temperature is 120 ℃, and crosslinking time is 3h, and crosslinked atmosphere is atmosphere environment.Material after crosslinking curing is put into heat treatment furnace and 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 argon gas inert atmosphere.Material after ceramic is carried out to ultrasonic cleaning, remove surface ceramic powder, then dry.Repeat above-mentioned dipping, crosslinking curing, ceramic treatment and baking step until the open-cell porosity of final gained friction braking material is less than 10%.
The C/C-SiC-ZrC-ZrB of Fig. 1 for preparing by above-mentioned technique
2the typical microstructure of complex phase ceramic base friction braking material, the region in the corresponding left figure of right figure after white box amplification.In figure, black part is divided into carbon fiber and RESEARCH OF PYROCARBON, and grey color part is SiC phase, and white portion is ZrC and ZrB
2phase.In friction braking material in the present invention, carbon fiber plays and strengthens toughness reinforcing effect; SiC-ZrC-ZrB
2in complex phase ceramic matrix, three-phase is nanometer disperse distribution, can form the ceramic coating of self-healing, thereby can improve the high-temperature oxidation resistance of C/C composite material when friction catch produces high temperature.
Adopt 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 cruve is shown in Fig. 2.Test result shows, complex phase ceramic base braking material stable friction factor of the present invention; The particularly important is, than dry friction test, in wet friction test, the friction factor of brake disc slightly promotes, and this result is better than current C/C composite material brake disc.
The performance test results of the friction braking material of preparing in embodiments of the invention is as shown in table 1, and wherein comparative example is C/C braking material.
Table 1: the performance test results of friction braking material
| Performance parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| 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 regulate in wider scope, and wet friction coefficient ratio dry friction coefficient is slightly improved, and the wet friction coefficient of the C/C braking material of comparative example sharply declines than dry friction coefficient.Friction braking material of the present invention owing to having formed oxide film in friction process, and wear rate shows as weightening finish, and comparative example C/C braking material is due to the oxidation weight loss of material with carbon element, and wear rate is 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 (3)
1. a preparation method for friction braking material, comprising:
Adopt carbon fiber to form carbon fabric perform, wherein this carbon fabric perform is for without forming through continuous needle after latitude carbon cloth and carbon fibre web tire lamination again;
Chemical vapor carbon deposition interface layer on the carbon fiber surface of carbon fabric perform, wherein this chemical vapor deposition step comprises: take hydrocarbon gas as carbon source, adopt isothermal chemical vapor deposition method at carbon fiber surface pyrolytic deposition carbon interface layer, depositing temperature is 900～1100 ℃, stagnation pressure is 5～10kPa, hydrocarbon gas flow is 2～4L/min, and sedimentation time is 10～20h;
Preparation liquid phase ceramic forerunner, wherein this preparation liquid phase ceramic forerunner step comprises: respectively Polycarbosilane, poly-carbon zirconium oxygen alkane and poly-carbon boron azane are dissolved in and in toluene or xylene solvent, are prepared into corresponding precursor solution by 50% mass ratio, then three kinds of precursor solutions are configured to SiC-ZrC-ZrB by required proportioning
2liquid phase ceramic forerunner;
The carbon fabric perform that deposits carbon interface layer is immersed in liquid phase ceramic forerunner, wherein this impregnation steps comprises: by the carbon fabric perform vacuum impregnation that deposits carbon interface layer in the liquid phase ceramic forerunner configuring, the temperature of liquid phase ceramic forerunner is 50 ℃, vacuum degree control is below 1kPa, and dip time is 2h;
Carbon fabric perform after maceration extract phase ceramics precursor is carried out to crosslinking curing processing, wherein this crosslinking curing treatment step comprises: the material of gained after dipping is carried out to crosslinking curing processing in baking oven, temperature is 60～120 ℃, and the time is 3h, and atmosphere is atmosphere environment; And
After crosslinking curing is processed, thereby the material of gained carries out ceramic treatment and forms friction braking material, wherein this ceramic treatment step comprises: the material of gained after crosslinking curing is put into heat treatment furnace, the heating rate of heat treatment furnace is 2 ℃/min, heat treatment temperature is 1500 ℃, holding time is 2h, heat-treating atmosphere is argon gas atmosphere, thus prepared SiC-ZrC-ZrB
2three-phase in complex phase ceramic matrix is nanometer disperse and distributes.
2. according to the method for claim 1, also comprise:
Repeated impregnations, crosslinking curing process and ceramic treatment step until the density of the friction braking material of final gained no longer increase.
3. according to the method for claim 1, also comprise:
Repeated impregnations, crosslinking curing processing and ceramic treatment step are until the open-cell porosity of the friction braking material of final gained is less than 10%.
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| CN201110449309.5A CN102537155B (en) | 2011-12-29 | 2011-12-29 | C/C-SiC-ZrC-ZrB2 complex-phase ceramic-based frictional braking material and preparation method thereof |
| 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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| CN103332963B (en) * | 2013-06-19 | 2014-08-27 | 陕西科技大学 | Method for modifying C/C composite material at low temperature by microwave-ultraviolet process |
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| CN113511900A (en) * | 2021-05-28 | 2021-10-19 | 中国科学院上海硅酸盐研究所 | Preparation method of zirconium boride reinforced SiC-AlN solid solution main phase nano multiphase ceramic sintered body |
| CN113416080B (en) * | 2021-06-25 | 2022-05-10 | 上海大学 | Carbon nano modified carbon fiber preform, carbon/carbon composite material, carbon/ceramic composite material and preparation method thereof |
| CN113735593B (en) * | 2021-09-30 | 2022-09-30 | 陕西科技大学 | SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and preparation method thereof |
| CN115773321B (en) * | 2023-02-13 | 2023-05-09 | 西安超码科技有限公司 | High-strength carbon/ceramic brake disc with ceramic functional layer |
| CN116835989B (en) * | 2023-06-16 | 2024-03-22 | 中南大学 | C/C-SiC-ZrC-ZrB 2 Composite material and preparation method and application thereof |
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| CN103693984A (en) | 2014-04-02 |
| CN102537155A (en) | 2012-07-04 |
| CN103693984B (en) | 2015-08-26 |
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