CN1570188A - Carbon-carbon/aluminium composite material preparation method - Google Patents
Carbon-carbon/aluminium composite material preparation method Download PDFInfo
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- CN1570188A CN1570188A CN 200410018285 CN200410018285A CN1570188A CN 1570188 A CN1570188 A CN 1570188A CN 200410018285 CN200410018285 CN 200410018285 CN 200410018285 A CN200410018285 A CN 200410018285A CN 1570188 A CN1570188 A CN 1570188A
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Abstract
A carbon-carbon/aluminum composite material preparing process for high performance materials is provided. The process is as follows: the forming of the carbon fiber blank: the carbon fiber blank is prepared by using arrangement and needling method; the forming of carbon-carbon precast products: the precast product is prepared by binding fiber using densification technology; the combination of the carbon-carbon precast product and aluminum: the carbon-carbon/aluminum composite material is prepared by using vacuum pressure impregnation method or compression moulding method. The invention solves two problems: the preparation of the precast product and interface reaction control.
Description
Technical field
The present invention relates to a kind of preparation method of matrix material, specifically is a kind of preparation method of carbon-to-carbon/aluminum composite.The preparation field that is used for high performance material.
Background technology
Usually carbon/aluminum composite preparation process comprised for two steps: 1. the preparation of prefabricated carbon fiber spare; 2. be compounded to form material with aluminium.Preparation prefabricated carbon fiber spare has several different methods at present, and row shop fiber is still the main method of making prefabricated carbon fiber spare but utilize framework or mould to make by hand.Because carbon fiber self is comparatively soft, the prefabricated carbon fiber spare that uses current techniques to make mainly relies on external means such as framework, mould to keep preform structure and porosity, thereby can not carry out machining processes change prefabricated component shape.And in art breading subsequently, molten aluminum liquid is pressed into and make carbon/aluminum composite in the prefabricated component.In this course, prefabricated carbon fiber spare will bear certain pressure and temperature, and the prefabricated carbon fiber spare of making thus conformal ability is relatively poor, in the process that aluminium liquid infiltrates, easily deforms, thereby causes Fiber Distribution can not realize design requirements.And when carbon fiber and aluminium liquid when high temperature contacts, deal with improperly and can cause serious surface reaction, not only cause the carbon fiber damage, and form strong interfacial bond, cause made carbon/aluminum composite that low stress damage easily takes place.For avoiding the surface reaction between carbon aluminium, use various coatings to protect carbon fiber, stop or weaken surface reaction.
Find by literature search, Wang Haowei etc. are published in " aviation journal " (1993, Vol14) employed preparation method in " liquid phase method is made the C/Al matrix material ": at first carbon fiber is carried out surface treatment, deposit the SiC coating of a layer thickness about the dozens of nanometer at fiber surface with chemical Vapor deposition process; Carbon fiber after will handling then is layered in the mould according to the volume fraction and the direction row of design; Adopt vacuum pressure impregnation or pressure die casting method afterwards, under the effect of pressure, aluminium liquid is infiltrated in the mould, promptly be prepared into carbon/aluminum composite after the cooling.Conventional carbon/aluminum composite preparation method's deficiency mainly contains two aspects: 1. made prefabricated component self is poor, and is yielding in subsequent technique a little less than the conformal ability, and easily causes the inhomogeneous of Fiber Distribution; 2. for the control surface reaction, under the condition of using coating, also need strict control process parameters, preparation condition is required comparatively harshness, increased preparation difficulty and cost.
Summary of the invention
The present invention is directed to difficult these two critical problems of control of carbon/aluminum composite prefabricated component preparation difficulty and surface reaction, be based on existing carbon-carbon composite preparation method and carbon/aluminum composite preparation method, a kind of preparation method of carbon-to-carbon/aluminum composite is proposed, make it can effectively solve in carbon/aluminum composite preparation process the prefabricated component preparation and surface reaction is controlled this two difficult problems, help to simplify technology, reduce cost, thereby application lays the first stone for carbon/aluminum composite obtains widely.
The present invention is achieved by the following technical solutions, and method steps is as follows:
(1) moulding of carbon fiber blank
In this step, form carbon fiber blank by row shop, needle punching.Particularly, row shop is the material performance requirement according to design, the carbon fiber of preseting length is layered in the mould according to unidirectional or multidirectional row, and reaches the volume content of setting; The acupuncture rule is to handle by needle loom piling up good whole felt, make carbon fiber commissure each other, thereby acquisition carbon fiber blank, and can be by the carbon fiber volume content on the control acupuncture time control base substrate thickness direction, because the fiber on the thickness direction is to be produced by the fiber that pricker drives in the plane.In this step, can make material on specific direction, have specific performance properties by Fiber Distribution direction, quantitative design in the carbon fiber blank, thereby realize the customization of material property.
(2) moulding of carbon-to-carbon prefabricated component
By the densification process consolidation fibre, make prefabricated component have certain conformal ability, thereby form porous carbon-to-carbon prefabricated component.In this step, adopt chemical gas phase cementation process (CVI) in the certain thick RESEARCH OF PYROCARBON of carbon fiber surface deposition, usually the RESEARCH OF PYROCARBON bed thickness between 1～4 micron.Make carbon fiber be connected to each other together by RESEARCH OF PYROCARBON, thereby make the carbon-to-carbon prefabricated component have certain conformal ability, and can bear certain pressure, reduce subsequently with the aluminium recombination process in deflection, thereby can realize the distribution of carbon fiber in material that design.And pyrolytic carbon layer can effectively be protected carbon fiber, stops the generation of the surface reaction of carbon fiber and aluminum substrate, thereby obtains good material property.And RESEARCH OF PYROCARBON has high thermal and low thermal expansivity, and the adding of RESEARCH OF PYROCARBON can effectively improve material thermal conductivity, reduces material thermal expansion coefficient.
(3) carbon-to-carbon prefabricated component and aluminium are compound
In this step, make aluminium liquid enter the carbon-to-carbon prefabricated component, fill the space in the prefabricated component, solidify the final carbon-to-carbon/aluminum composite that forms in back.In this step, can use vacuum pressure impregnating method or pressure casting method will make prefabricated component and aluminum substrate compound.
Vacuum pressure impregnating method technology is as follows: the carbon-to-carbon prefabricated component is packed in the mould, put into process furnace behind the die sealing; Process furnace top body of heater and bottom body of heater heat up respectively, make closed tin and aluminium liquid reach design temperature; Vacuumize vacuum tightness≤1 * 10 in the burner hearth
-6Behind the MPa, will fill the crucible jack-up of aluminium liquid, the mould mouth immerses in the aluminium liquid, feeds pressure 1 * 10 in stove
6The nitrogen of MPa, under the effect of mould external and internal pressure difference, aluminium liquid enters mould, infiltrate in the prefabricated component, behind the insulation 1h, the mould furnace cooling.Preform temperatures and temperature of aluminum liquid are 750 ℃.
Pressure casting method technology is as follows: when die temperature, temperature of aluminum liquid all reached design temperature, the carbon-to-carbon prefabricated component that will be heated to preset temperature in process furnace was put into mould, pour into aluminium liquid after, pressure head presses down, simultaneously pumping with exhaust blower.Pressure reached after the preset value pressurize 1 minute.The prefabricated component preheating temperature is 450 ℃, and temperature of aluminum liquid is 800 ℃, and die temperature is 300 ℃, and press pressure is 10MPa.
The structure design of carbon-to-carbon prefabricated component and preparation are the decisive steps that acquisition has the carbon-to-carbon/aluminum composite of required performance.In this step of carbon fiber blank moulding, by selecting to have the kinds of fibers of different performance, design different volumes content, the arrangement mode of fiber, the fibre content on specific direction, thus obtain specific preform structure and performance; Pass through densification process; can apply one deck carbon at fiber surface on the one hand; play the effect of protection carbon fiber; and can further adjust the porosity of prefabricated component; formed on the other hand carbon base body can fixed carbon fiber; structure when making the fiber base substrate keep moulding, and make prefabricated component have certain intensity, thus reduce the distortion of prefabricated component in subsequent technique.
When using casting die to prepare carbon/aluminum composite, it is shorter that fiber and aluminum substrate are in the pyritous time, thereby surface reaction more easy to control, but owing to pressure that prefabricated component bears in the preparation process is bigger, easily cause the prefabricated component distortion, thereby make Fiber Distribution inhomogeneous.And when using vacuum pressure impregnating method, aluminium liquid relies on negative pressure to drive and enters prefabricated component, and the pressure that prefabricated component bears is less, and is not yielding, but surface reaction more easily takes place carbon fiber and aluminum substrate Long contact time at high temperature.Consider that prepared carbon-to-carbon prefabricated component self has certain intensity, can bear certain pressure, and carbon fiber all is wrapped in the pyrolytic carbon layer, the response capacity of RESEARCH OF PYROCARBON and aluminium is relatively poor, thereby carbon/aluminium surface reaction is limited to effect of material performance.Thereby use these two kinds of methods all can prepare high performance carbon-to-carbon/aluminum composite.
The RESEARCH OF PYROCARBON that forms by chemical vapor infiltration is generally the synusia structure, and the anisotropy degree is higher, and the RESEARCH OF PYROCARBON crystalline structure that forms under different technology conditions can vary continuously to three-dimensional carbonization structure from isotropy.The RESEARCH OF PYROCARBON diversity structure has determined the diversity of its performance.
Compare with conventional carbon/aluminum composite preparation method, maximum difference of the present invention is that thickness reaches the introducing of 1～4 micron pyrolytic carbon layer.The effect of RESEARCH OF PYROCARBON is many-sided, not only will play the effect of protection and fixed carbon fiber in preparation process; After forming carbon-to-carbon/aluminum composite, RESEARCH OF PYROCARBON can obtain the matrix material with higher heat-conductivity as the high performance composition of a kind of high heat conduction, low bulk under the situation of not using high heat conducting fiber; And when carbon-to-carbon/aluminum composite carry load, pyrolytic carbon layer can improve the fracture characteristics of material as the stress sustained release dosage, improves the mechanical property of material.And because the diversity of RESEARCH OF PYROCARBON performance, the RESEARCH OF PYROCARBON of the different structure that obtains under different deposition process conditions has different performances, thereby the design means of carbon/aluminum composite has further been enriched in the introducing of RESEARCH OF PYROCARBON.The present invention can solve and be applied to not have as yet in the field of engineering technology this good physics and the technical barrier of chemical property material according to the good physics and the chemical property that obtain.
Embodiment
Example 1. preparation Nomex carbon-to-carbon/aluminum composites
At first with several layers, thickness after the whole felt of 0.2～2cm piles up, connect for whole through acupuncture, and reach the fiber volume fraction of design, after 1050 ℃ of following carbonizations, after chemical vapor infiltration is handled, make Nomex carbon-to-carbon prefabricated component again; Adopt technique of vacuum pressure for dipping electrical and aluminium to be compounded to form carbon-to-carbon/aluminum composite afterwards.Wherein carbon fiber volume content 6%, RESEARCH OF PYROCARBON volume content 17%, and other are aluminum substrate.
Made Nomex carbon-to-carbon/aluminum composite weave construction is: the fiber in the prefabricated component plane is a chaotic distribution, and is roughly suitable in the ratio of arranging of all directions, thereby makes that made material property is an isotropy in the plane.Carbon fiber in the prefabricated component all is wrapped in the pyrolytic carbon layer of 1～4 μ m, and pyrolytic carbon layer is good with combining of carbon fiber.After compound with aluminium, the bonding state of pyrolytic carbon layer and aluminum substrate is also very good.
Carbon fiber in the whole prefabricated component is commissure each other, and is fixed by RESEARCH OF PYROCARBON, thereby makes prefabricated component have certain intensity.Can find from the pattern of carbon-to-carbon prefabricated component and made carbon-to-carbon/aluminum composite pattern contrast, Fiber Distribution and the Fiber Distribution in carbon-to-carbon/aluminum composite in the prefabricated component are basic identical, explanation is in recombination process, the deflection of carbon-to-carbon prefabricated component is very little, and the structure of carbon-to-carbon prefabricated component is well remained in carbon-to-carbon/aluminum composite.This shows that pyrolytic carbon layer has played tangible reinforcement effect really to carbon fiber blank.
Made Nomex carbon-to-carbon/aluminum composite flexural strength is 200MPa, and thermal conductivity is 272W/mK, and thermal expansivity is 4.3 * 10
-6
Example 2. preparation carbon felt carbon fiber laminate carbon-to-carbon/aluminum composites
At first, unidirectional row lays the T300 carbon fiber of meter thickness on the whole felt of individual layer, and the whole felt of 2～20 laminar surfaces row having been spread carbon fiber piles up, and forms the sandwich structure of carbon fiber-carbon felt-carbon fiber.Again with this structure through the acupuncture commissure as a whole and reach the initial density of design after; Under 1050 ℃, carry out carbonizing treatment, after chemical vapor infiltration is made carbon fiber carbon mat laminate carbon back framework material.Adopting pressure casting method afterwards, is 10MPa at pressure, and the prefabricated component preheating temperature is 450 ℃, and temperature of aluminum liquid is 800 ℃, and die temperature is 300 ℃, and press pressure is 10MPa, pressurize 1 minute.The cooling back forms carbon felt carbon fiber laminate carbon-to-carbon/aluminum composite.In made carbon felt carbon fiber laminate carbon-to-carbon/aluminum composite, carbon fiber volume content is 21%, and the RESEARCH OF PYROCARBON volume content is 33%, and other are aluminum substrate.
Its weave construction is the sandwich structure that unidirectional carbon fiber dimension layer-carbon carpet veneer is alternately arranged.In unidirectional carbon fiber dimension layer, carbon fiber is unidirectional arranging; In the carbon carpet veneer, carbon fiber is planar arranged in a jumble.All all complete being wrapped in the pyrolytic carbon layer of carbon fiber do not contact with aluminum substrate fully, and the interface is difficult to observe interfacial product in conjunction with good.
Made carbon felt carbon fiber laminate carbon-to-carbon/the aluminum composite flexural strength is 710MPa, and modulus is 90GPa, and thermal conductivity is 128W/mK, and thermal expansivity is 1.6 * 10
-6
Example 3. preparation unidirectional carbon fiber dimensions strengthen carbon-to-carbon/aluminum composite
Unidirectional row spreads the T300 carbon fiber to design volume content in graphite jig, handle through chemical vapor infiltration, in fiber surface deposition RESEARCH OF PYROCARBON, adopt technique of vacuum pressure for dipping electrical that aluminium liquid is infiltrated in the prefabricated component, the carbon-to-carbon prefabricated component is packed in the steel die, put into process furnace behind the die sealing, top body of heater and bottom body of heater heat up respectively, closed tin and temperature of aluminum liquid reach 750 ℃, vacuumize in the burner hearth, when vacuum tightness is 1 * 10
-6MPa will fill the crucible jack-up of aluminium liquid, and the airtight mould mouth that prefabricated component arranged is immersed in the aluminium liquid, feeds nitrogen afterwards in stove, and pressure is 1 * 10
6MPa, under the effect of mould external and internal pressure difference, aluminium liquid enters mould, infiltrates in the prefabricated component, is incubated after 1 hour, the mould furnace cooling is obtained the unidirectional carbon fiber dimension strengthen carbon-to-carbon/aluminum composite.Wherein carbon fiber volume content is 40%, and the RESEARCH OF PYROCARBON volume content is 23%, and other are aluminum substrate.
Its weave construction is: carbon fiber is arranged along a direction fully, thereby made carbon-to-carbon/aluminum composite has anisotropic material property.All all complete being wrapped in the pyrolytic carbon layer of carbon fiber do not contact with aluminum substrate fully, and the interface is difficult to observe interfacial product in conjunction with good.
The material property that is obtained (along fibre axis to) be: flexural strength is 540MPa, and thermal conductivity 100MPa, thermal expansivity are 0.38 * 10
-6
Claims (5)
1, a kind of preparation method of carbon-to-carbon/aluminum composite is characterized in that, method steps is as follows:
(1) moulding of carbon fiber blank: form carbon fiber blank by row shop, needle punching, the row shop is that carbon fiber is layered in the mould according to unidirectional or multidirectional row, and reach the volume content of setting, the acupuncture rule is to handle by needle loom piling up good whole felt, make carbon fiber commissure each other, thereby obtain carbon fiber blank;
(2) moulding of carbon-to-carbon prefabricated component: by the densification process consolidation fibre, make prefabricated component have the conformal ability, can carry out machining, thereby form porous carbon-to-carbon prefabricated component, adopt the chemical gas phase cementation process to deposit pyrolytic carbon layer at carbon fiber surface, carbon fiber is connected to each other together by RESEARCH OF PYROCARBON;
(3) carbon-to-carbon prefabricated component and aluminium are compound: use vacuum pressure impregnating method or pressure casting method that prefabricated component and aluminum substrate is compound, aluminium liquid enters the carbon-to-carbon prefabricated component, fills the space in the prefabricated component, solidifies the final carbon-to-carbon/aluminum composite that forms in back.
2, the preparation method of carbon-to-carbon/aluminum composite according to claim 1 is characterized in that, step (2), and at the sedimentary pyrolytic carbon layer of carbon fiber surface, its thickness is 1～4 micron.
3, the preparation method of carbon-to-carbon/aluminum composite according to claim 1, it is characterized in that, in the step (3), vacuum pressure impregnating method technology is as follows: the carbon-to-carbon prefabricated component is packed in the steel die, put into process furnace behind the die sealing, top body of heater and bottom body of heater heat up respectively, make closed tin and temperature of aluminum liquid all reach 750 ℃, vacuumize in the burner hearth, when vacuum tightness≤1 * 10
-6Behind the MPa, will fill the crucible jack-up of aluminium liquid, the airtight mould mouth that prefabricated component arranged is immersed in the aluminium liquid, feed nitrogen afterwards in stove, pressure is 1 * 10
6MPa, under the effect of mould external and internal pressure difference, aluminium liquid enters mould, infiltrates in the prefabricated component, is incubated after 1 hour, with the mould furnace cooling.
4, the preparation method of carbon-to-carbon/aluminum composite according to claim 1, it is characterized in that, in the step (3), pressure casting method technology is as follows: when die temperature be 300 ℃, when temperature of aluminum liquid is 800 ℃, the carbon-to-carbon prefabricated component that will be heated to 450 ℃ in process furnace is put into mould, pour into aluminium liquid after, pressure head presses down, pumping with exhaust blower simultaneously, wherein pressure reached behind the 10MPa pressurize 1 minute.
5, the preparation method of carbon-to-carbon/aluminum composite according to claim 1, it is characterized in that, in the step (1), the fiber on the thickness direction is to be produced by the fiber that pricker drives in the plane, by the carbon fiber volume content on the control acupuncture time control base substrate thickness direction.
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| JP2009256117A (en) * | 2008-04-14 | 2009-11-05 | Toyo Tanso Kk | Carbon fiber carbon composite molded body, carbon fiber-reinforced carbon composite material and its manufacturing method |
| CN101323919B (en) * | 2008-07-25 | 2010-06-09 | 哈尔滨工业大学 | Method for preparing metal-matrix composite by vacuum pressure infiltration |
| CN101805200A (en) * | 2010-03-17 | 2010-08-18 | 上海大学 | Method for producing carbon/carbone composite material for bearings |
| CN101392357B (en) * | 2007-09-19 | 2012-12-12 | 中国科学院金属研究所 | Proximal melting state diffusion technology for preparing SiC fiber/aluminum base composite material |
| CN103243280A (en) * | 2013-04-28 | 2013-08-14 | 河南科技大学 | Carbon fiber reinforced aluminum-based composite material and preparation method thereof |
| CN105541363A (en) * | 2015-12-23 | 2016-05-04 | 北京航空航天大学 | High-temperature composite material and preparation method thereof |
| CN106938937A (en) * | 2015-11-25 | 2017-07-11 | 通用电气公司 | The method for handling ceramic fibre |
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| CN115160007A (en) * | 2022-06-15 | 2022-10-11 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-carbon composite structure and preparation method thereof |
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| CN101392357B (en) * | 2007-09-19 | 2012-12-12 | 中国科学院金属研究所 | Proximal melting state diffusion technology for preparing SiC fiber/aluminum base composite material |
| CN102007090A (en) * | 2008-04-14 | 2011-04-06 | 东洋炭素株式会社 | Carbon fiber carbon composite molded body, carbon fiber-reinforced carbon composite material and manufacturing method thereof |
| JP2009256117A (en) * | 2008-04-14 | 2009-11-05 | Toyo Tanso Kk | Carbon fiber carbon composite molded body, carbon fiber-reinforced carbon composite material and its manufacturing method |
| CN101323919B (en) * | 2008-07-25 | 2010-06-09 | 哈尔滨工业大学 | Method for preparing metal-matrix composite by vacuum pressure infiltration |
| CN101805200A (en) * | 2010-03-17 | 2010-08-18 | 上海大学 | Method for producing carbon/carbone composite material for bearings |
| CN103243280A (en) * | 2013-04-28 | 2013-08-14 | 河南科技大学 | Carbon fiber reinforced aluminum-based composite material and preparation method thereof |
| CN106938937B (en) * | 2015-11-25 | 2023-11-28 | 通用电气公司 | Method for treating ceramic fibers |
| CN106938937A (en) * | 2015-11-25 | 2017-07-11 | 通用电气公司 | The method for handling ceramic fibre |
| CN106957178A (en) * | 2015-11-25 | 2017-07-18 | 通用电气公司 | Device and method for handling ceramic fibre |
| CN105541363A (en) * | 2015-12-23 | 2016-05-04 | 北京航空航天大学 | High-temperature composite material and preparation method thereof |
| CN108405867B (en) * | 2018-03-09 | 2019-11-08 | 湖南东映碳材料科技有限公司 | A kind of preparation method of unidirectional high thermal conductivity Cf/Al composite material |
| CN108405867A (en) * | 2018-03-09 | 2018-08-17 | 湖南东映碳材料科技有限公司 | A kind of unidirectional high heat conduction CfThe preparation method of/Al composite materials |
| CN115160007A (en) * | 2022-06-15 | 2022-10-11 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-carbon composite structure and preparation method thereof |
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