CN106591744A - Mold for composite material preparation and preparation method - Google Patents
Mold for composite material preparation and preparation method Download PDFInfo
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- CN106591744A CN106591744A CN201510663282.8A CN201510663282A CN106591744A CN 106591744 A CN106591744 A CN 106591744A CN 201510663282 A CN201510663282 A CN 201510663282A CN 106591744 A CN106591744 A CN 106591744A
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- carbon fiber
- composite material
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- titanium alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
- C22C47/062—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element from wires or filaments only
- C22C47/064—Winding wires
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
- C22C47/12—Infiltration or casting under mechanical pressure
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/10—Refractory metals
- C22C49/11—Titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
Abstract
The invention provides a mold for composite material preparation and a preparation method. The mold is technically characterized by comprising a mold body; a mold cover is arranged on the upper portion of the mold body and is provided with a pressure head for pressurizing; and an infrared heater is arranged around the mold body. The composite material preparation method includes the steps that firstly, continuous SiC fibers are prepared through a chemical vapor deposition method or polyacrylonitrile carbon fibers are wound onto one graphite inner ring; secondly, the SiC fibers or the outer surface of the carbon fiber ring are/is coated with a carbon coating; thirdly, the SiC fibers or the carbon fiber ring coated with the coating are/is taken down; fourthly, a titanium alloy is placed on a fiber prefabricated body and is heated till the titanium alloy is molten; fifthly, the pressure head is adopted for applying pressure on the molten titanium alloy, so that the SiC fibers or the carbon fiber ring can be wrapped by the molten titanium alloy; and sixthly, the infrared heater is closed, and cooling is performed till room temperature is achieved. By adopting the technical scheme, the interface reaction control is accurate, the composite material performance is remarkably improved, and the utilizing rate is high.
Description
Technical field
The present invention relates to technical field of composite preparation, specifically a kind of composite die for preparation and preparation method.
Background technology
With the continuous improvement of aero-engine thrust-weight ratio, higher and higher requirement is proposed to the structural material of electromotor, the aero-engine that particularly thrust-weight ratio is more than 12, require the higher specific strength of structural material and specific stiffness, more excellent high-temperature behavior, such as elevated temperature strength and creep resistant, higher antioxidation and corrosion resistance.But existing nickel base superalloy is already close to its ultimate-use (limiting service) temperature, and density is too high, requirement of the high thrust-weight ratio engine to structural material can not have increasingly been met.Continuous SiC fiber strengthens titanium matrix composite and has higher specific strength and specific stiffness, higher high temperature resistant and creep resistant and antioxidative ability, the overall performance of electromotor can be greatly improved while loss of weight, therefore becomes the candidate material of high thrust-weight ratio aero-engine most with prospects.At present, the preparation method of continuous SiC fiber enhancing Intermatallic Ti-Al compound based composites has a lot, mainly including paper tinsel-fiber-paper tinsel method, powder cloth method, pressure casting method, plasma spraying method, basal body coating layer method etc..
Paper tinsel-fiber-paper tinsel method is that titanium-aluminium alloy is processed into into foil, then at a certain distance arranges fiber, is fixed between foil, forms prefabricated section, and Jing vacuum hotpressings or high temperature insostatic pressing (HIP) are consolidated molding.The method its advantage is process is simple, microstructure is controllable, chemical composition is accurate, impurity content is low, but its shortcoming prepares high titanium alloy foil price, Irregular Shaped Parts preparation difficulty and difficult quality guarantee, paper tinsel-fiber-paper tinsel method is carrying out compound tense, easily produce the travelling of fiber, so as to cause fiber skewness, when the part of complex appearance is formed with, due to the performance that the damage of fiber is easily caused in forming process so as to reduce composite.
Powder cloth method is that titanium-aluminium alloy is processed into into powder, and using binding agent cloth-like thin slice is made into, and powder pieces of cloth and fiber are superimposed, Jing vacuum hot pressing formations, and it has the disadvantage that fiber skewness, powder are easy in itself oxidation.
Pressure casting method is that fiber preform is put in the mould of a heating, pour the titanium alloy of thawing into, then pass to high pressure argon gas, in forcing liquid metal infiltrated fiber prefabricated component gap, so as to make continuous fiber reinforcing titanium aluminum matrix composite, it has the disadvantage for as the composite of the high temperature resistant matrix such as titanium alloy, high temperature alloy, because temperature is higher in preparation process, so that interfacial reaction acutely, causes composite property to be seriously affected.
Plasma spraying method is titanium alloy molten drop to be sprayed on the fiber for laying using plasma apparatus, vacuum hotpressing or high temperature insostatic pressing (HIP) are carried out after lamination, to prepare continuous fiber reinforcing titanium aluminum matrix composite, but it has the disadvantage to easily cause fibre damage in Plasma Spraying Process Using, therefore the composite property for preparing is affected.
Basal body coating layer method is to evaporate titanium alloy by the method for physical heating and be deposited on fiber, and the advantage of the method is a lot, but it is of the prior art have the disadvantage that titanium alloy high cost, stock utilization be low, efficiency is very low, need special depositing device, complex process.
The content of the invention
The purpose of the present invention, exactly solves problem present in above technology, and provides a kind of composite die for preparation and preparation method for this.
A kind of composite die for preparation, including die ontology, the top of die ontology is provided with die cover, and the pressure head for pressurization is provided with die cover, and infrared heater is provided with around die ontology.
Selectively, the quantity of the infrared heater is 1-12.
A kind of composite material and preparation method thereof, comprises the following steps：
Continuous SiC fiber is prepared using chemical vapour deposition technique or polyacrylonitrile carbon fiber is wound on a graphite internal ring, form a carbon fiber ring；
Second step, by the outer surface of the SiC fibers prepared or carbon fiber ring carbon coating is coated；
3rd step, the SiC fibers or carbon fiber ring that are coated with coating are removed, and prepare fiber preform；
4th step, in the mould that fiber preform is put in vacuum chamber, places titanium alloy above fiber preform, covers die cover, opens infrared heater, is heated to melt titanium alloy；
5th step, pressure is applied using pressure head to the titanium alloy for melting so as to which SiC fibers or carbon fiber ring cladding get up；
6th step, closes infrared heater so as to room temperature is cooled to, so as to prepare composite material parts.
Selectively, the material with carbon element of magnetic control spattering target is coated to the SiC fibers surface of SiC fibers using the method for rf magnetron sputtering, and the technological parameter of rf magnetron sputtering is operating air pressure 4.0-6.0Pa, argon flow amount 17-22sccm, heating-up temperature 450-510 DEG C, sputtering power 700-850W；The method of carbon fiber outer surface coating carbon coating is carbon fiber ring and graphite internal ring to be put in chemical vapour deposition technique stove, outside deposition a layer thickness of chemical vapour deposition technique fibrous ring after winding is adopted for 2 μm -5 μm of carbon coating, the reaction raw material wherein used by chemical vapour deposition technique is argon and C2H2Gaseous mixture, the proportioning of two kinds of components is 0.5:1-1.5:1, depositing temperature is 1000 DEG C ± 30 DEG C.
Selectively, the titanium alloy of the melting is infiltrated under pressure in the gap between SiC fibers, until being filled up completely with full；The titanium alloy of melting can't be infiltrated in the gap between carbon fiber.
Selectively, the material of the magnetic control spattering target is TiC, Al2O3、Y2O3, any one in TiN.
Selectively, the infrared heater is heated to 1600-1740 DEG C.
Selectively, it can be based on the plasma asistance of sensing heating that the chemical vapour deposition technique and radio frequency magnetron sputtering method are.
Selectively, it is described to adopt the fibre diameter that chemical vapour deposition technique prepares continuous SiC fiber for 100 μm.
Selectively, it is described also carbon nano-tube fibre to be wound on a graphite internal ring in carbon fiber forming process.
Advantages of the present invention：
1, using physical vaporous depositions such as rf magnetron sputterings in the surface coating coatings of fiber, to the control of interfacial reaction precisely, interfacial reaction degree is reduced, the performance for making composite is significantly improved；
2, fiber is evenly distributed；
3, the infiltration of titanium alloy is realized under vacuum conditions, reduce the oxidation of titanium alloy；
4, the near-net-shape of titanium matrix composite part is directly realized by, shorten manufacturing cycle, process is simple, efficiency is improved, and stock utilization is high, reduces cost.
Description of the drawings
Fig. 1 is the structural representation of the mould of the present invention.
Specific embodiment
In order that the present invention is easier to be understood, technical scheme is described in detail below in conjunction with accompanying drawing and embodiment.
Embodiment 1
As shown in figure 1, a kind of composite die for preparation, the mould includes die ontology 1, and the top of die ontology 1 is provided with die cover 2, and the pressure head 3 for pressurization is provided with die cover 2, and infrared heater 4 is provided with around die ontology 1.
A kind of composite material and preparation method thereof, comprises the following steps：Comprise the following steps：The first step, prepares continuous SiC fiber or polyacrylonitrile carbon fiber is wound on a graphite internal ring using chemical vapour deposition technique, forms a carbon fiber ring；Second step, by the outer surface of the SiC fibers prepared or carbon fiber ring carbon coating is coated；3rd step, the SiC fibers or carbon fiber ring that are coated with coating are removed, and prepare fiber preform；4th step, in the mould that fiber preform is put in vacuum chamber, places titanium alloy above fiber preform, covers die cover 2, opens infrared heater 4, is heated to melt titanium alloy；5th step, using the titanium alloy of 3 pairs of meltings of pressure head pressure is applied so as to which SiC fibers or carbon fiber ring cladding get up；6th step, closes infrared heater 4 so as to room temperature is cooled to, so as to prepare composite material parts.
Embodiment 2
As shown in figure 1, a kind of composite die for preparation, the mould includes die ontology 1, and the top of die ontology 1 is provided with die cover 2, and the pressure head 3 for pressurization is provided with die cover, and 1-12 infrared heater 4 is provided with around die ontology 1.
A kind of composite material and preparation method thereof, comprises the following steps：The first step, prepares continuous SiC fiber or polyacrylonitrile carbon fiber is wound on a graphite internal ring using chemical vapour deposition technique, forms a carbon fiber ring, described to adopt the fibre diameter that chemical vapour deposition technique prepares continuous SiC fiber for 100 μm；Second step, by the outer surface of the SiC fibers prepared or carbon fiber ring carbon coating is coated, and the material with carbon element of magnetic control spattering target is coated to the SiC fibers surface of SiC fibers using the method for rf magnetron sputtering, and the material of the magnetic control spattering target is TiC, Al2O3、Y2O3, any one in TiN, the technological parameter of rf magnetron sputtering is operating air pressure 4.0-6.0Pa, argon flow amount 17-22sccm, heating-up temperature 450-510 DEG C, sputtering power 700-850W；The method of carbon fiber outer surface coating carbon coating is carbon fiber ring and graphite internal ring to be put in chemical vapour deposition technique stove, outside deposition a layer thickness of chemical vapour deposition technique fibrous ring after winding is adopted for 2 μm -5 μm of carbon coating, the reaction raw material wherein used by chemical vapour deposition technique is argon and C2H2Gaseous mixture, the proportioning of two kinds of components is 0.5:1-1.5:1, depositing temperature is 1000 DEG C ± 30 DEG C；3rd step, the SiC fibers or carbon fiber ring that are coated with coating are removed, and prepare fiber preform；4th step, in the die ontology 1 that fiber preform is put in vacuum chamber, places titanium alloy above fiber preform, covers die cover 2, opens infrared heater 4, and the infrared heater 4 is heated to 1600-1740 DEG C, is heated to melt titanium alloy；5th step, using the titanium alloy of 3 pairs of meltings of pressure head pressure is applied so as to SiC fibers or carbon fiber ring cladding are got up, the titanium alloy of the melting is infiltrated under pressure in the gap between SiC fibers, until being filled up completely with full；The titanium alloy of melting can't be infiltrated in the gap between carbon fiber；6th step, close infrared heater 4, allow to cool to room temperature, so as to prepare composite material parts, it can be the plasma asistance for being based on sensing heating that the chemical vapour deposition technique and radio frequency magnetron sputtering method are, described also carbon nano-tube fibre can be wound on a graphite internal ring in carbon fiber forming process.
In aforementioned process, the continuous SiC fiber prepared can be put in the sputtering chamber of quartz glass manufacture, to sputtering chamber evacuation, vacuum reaches 1.0 × 10-3Argon is filled with after Pa, purity of argon is 99.999%, and the material of magnetic control spattering target is coated to the surface of fiber, the target is column Y2O3Target, the size of column target is length 200mm, diameter 40mm, wall thickness 2mm, forms the fiber of band coating, and the technological parameter of rf magnetron sputtering is：Argon operating air pressure 5.0Pa, argon flow amount 20sccm, 500 DEG C of heating-up temperature, sputtering power 800W, continuous wire travelling speed is 2mm/min.
Embodiment 3
A kind of composite material and preparation method thereof, comprises the following steps：The first step, polyacrylonitrile carbon fiber is wound on a graphite internal ring, forms a carbon fiber ring；Second step, carbon fiber ring is put in the chemical vapour deposition technique stove of quartz glass manufacture, open sensing heater, the heating power of sensing heater is 6kw, open sensing heating plasma, the power of sensing heating plasma is 1.2kw, adopts outside deposition a layer thickness of chemical gaseous phase depositing process carbon fiber ring after winding for 3.5 μm of carbon coating, and the raw material of wherein chemical vapor deposition reaction used is argon and C2H2Gaseous mixture, the volume proportion of two kinds of components is 1.2:1, depositing temperature is 1000 DEG C.Reacting gas enters reactor via air inlet, reacts and generates the surface that carbon coating deposits to carbon fiber ring, and reacted tail gas is discharged via gas outlet；3rd step, in the die ontology 1 that the carbon fiber ring that one or more surfaces deposited carbon coating is put in vacuum chamber, places TC4 titanium alloys above carbon fiber ring；4th step, open infrared heater 4, it is heated to 1740 DEG C, TC4 titanium alloys are made to melt to form melting TC4 titanium alloys, pressure is applied using the TC4 titanium alloys of 3 pairs of meltings of pressure head, the pressure of applying is 2MPa, and pressing time is 0.5 hour, it is set to coat carbon fiber ring, but the TC4 titanium alloys of melting can't be infiltrated in the gap in carbon fiber ring between carbon fiber；5th step, closes infrared heater 4 so as to room temperature is cooled to, so as to prepare carbon fiber reinforced titanium matrix composite parts.
Embodiment 4
A kind of composite material and preparation method thereof, comprises the following steps：The first step, carbon nano-tube fibre is wound on a graphite internal ring, forms a carbon nano-tube fibre ring；Second step, carbon nano-tube fibre ring is put in the chemical vapour deposition technique stove of quartz glass manufacture, open sensing heater, the heating power of sensing heater is 6kw, open sensing heating plasma, the power of sensing heating plasma is 1.2kw, adopts outside deposition a layer thickness of chemical vapour deposition technique method carbon nano-tube fibre ring after winding for 3.0 μm of carbon coating, and the raw material of wherein chemical vapour deposition technique reaction is argon and C2H2Gaseous mixture, the volume proportion of two kinds of components is：1.2:1, depositing temperature is 1000 DEG C.Reacting gas enters reactor via air inlet, reacts and generates the surface that carbon coating deposits to carbon fiber ring 8, and reacted tail gas is discharged via gas outlet；3rd step, in the mould 2 that the carbon nano-tube fibre ring that one or more surfaces deposited carbon coating is put in vacuum chamber, places TC4 titanium alloys above carbon nano-tube fibre ring；4th step, open infrared heater, it is heated to 1740 DEG C, TC4 titanium alloys are made to melt to form melting TC4 titanium alloys, pressure is applied using the TC4 titanium alloys of 3 pairs of meltings of pressure head above, the pressure of applying is 2MPa, and pressing time is 0.5 hour, it is set to coat on carbon nano-tube fibre ring, but the TC4 titanium alloys of melting can't be infiltrated in the gap between the carbon nano-tube fibre in carbon nano-tube fibre ring；5th step, closes infrared heater 4 so as to room temperature is cooled to, so as to prepare the enhanced titanium matrix composite parts of carbon nano-tube fibre.
Claims (10)
1. a kind of composite die for preparation, including die ontology, it is characterised in that：The top of the die ontology is provided with die cover, and the pressure head for pressurization is provided with die cover, and infrared heater is provided with around die ontology.
2. a kind of composite die for preparation according to claim 1, it is characterised in that：The quantity of the infrared heater is 1-12.
3. a kind of composite material and preparation method thereof, it is characterised in that：Comprise the following steps：
The first step, prepares continuous SiC fiber or polyacrylonitrile carbon fiber is wound on a graphite internal ring using chemical vapour deposition technique, forms a carbon fiber ring；
Second step, by the outer surface of the SiC fibers prepared or carbon fiber ring carbon coating is coated；
3rd step, the SiC fibers or carbon fiber ring that are coated with coating are removed, and prepare fiber preform；
4th step, in the mould that fiber preform is put in vacuum chamber, places titanium alloy above fiber preform, covers die cover, opens infrared heater, is heated to melt titanium alloy；
5th step, pressure is applied using pressure head to the titanium alloy for melting so as to which SiC fibers or carbon fiber ring cladding get up；
6th step, closes infrared heater so as to room temperature is cooled to, so as to prepare composite material parts.
4. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：The material with carbon element of magnetic control spattering target is coated to the SiC fibers surface of SiC fibers using the method for rf magnetron sputtering, and the technological parameter of rf magnetron sputtering is operating air pressure 4.0-6.0Pa, argon flow amount 17-22sccm, heating-up temperature 450-510 DEG C, sputtering power 700-850W；The method of carbon fiber outer surface coating carbon coating is carbon fiber ring and graphite internal ring to be put in chemical vapour deposition technique stove, outside deposition a layer thickness of chemical vapour deposition technique fibrous ring after winding is adopted for 2 μm -5 μm of carbon coating, reaction raw material wherein used by chemical vapour deposition technique is the gaseous mixture of argon and C2H2, and the proportioning of two kinds of components is 0.5:1-1.5:1, depositing temperature is 1000 DEG C ± 30 DEG C.
5. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：The titanium alloy of the melting is infiltrated under pressure in the gap between SiC fibers, until being filled up completely with full；The titanium alloy of melting can't be infiltrated in the gap between carbon fiber.
6. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：The material of the magnetic control spattering target is any one in TiC, Al2O3, Y2O3, TiN.
7. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：The infrared heater is heated to 1600-1740 DEG C.
8. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：It can be based on the plasma asistance of sensing heating that the chemical vapour deposition technique and radio frequency magnetron sputtering method are.
9. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：It is described to adopt the fibre diameter that chemical vapour deposition technique prepares continuous SiC fiber for 100 μm.
10. a kind of composite material and preparation method thereof according to claim 3, it is characterised in that：It is described also carbon nano-tube fibre to be wound on a graphite internal ring in carbon fiber forming process.
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| CN201510663282.8A CN106591744B (en) | 2015-10-15 | 2015-10-15 | A kind of composite material die for preparation and preparation method |
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| CN201510663282.8A CN106591744B (en) | 2015-10-15 | 2015-10-15 | A kind of composite material die for preparation and preparation method |
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| CN106591744A true CN106591744A (en) | 2017-04-26 |
| CN106591744B CN106591744B (en) | 2019-01-29 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1519389A (en) * | 2003-01-20 | 2004-08-11 | 中国科学院金属研究所 | Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre |
| JP2006144030A (en) * | 2004-11-16 | 2006-06-08 | Bridgestone Corp | High thermal conductivity composite material and manufacturing method therefor |
| CN102912263A (en) * | 2012-10-11 | 2013-02-06 | 北京理工大学 | Carbon fiber reinforced titanium alloy compound material and preparation method thereof |
| CN102925825A (en) * | 2012-11-16 | 2013-02-13 | 中国航空工业集团公司北京航空制造工程研究所 | Preparation method for continuous fiber reinforced titanium-titanium aluminum hybrid matrix composite material |
| CN203545695U (en) * | 2013-11-01 | 2014-04-16 | 刘新保 | Microwave pressurizing synthesizing device |
-
2015
- 2015-10-15 CN CN201510663282.8A patent/CN106591744B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1519389A (en) * | 2003-01-20 | 2004-08-11 | 中国科学院金属研究所 | Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre |
| JP2006144030A (en) * | 2004-11-16 | 2006-06-08 | Bridgestone Corp | High thermal conductivity composite material and manufacturing method therefor |
| CN102912263A (en) * | 2012-10-11 | 2013-02-06 | 北京理工大学 | Carbon fiber reinforced titanium alloy compound material and preparation method thereof |
| CN102925825A (en) * | 2012-11-16 | 2013-02-13 | 中国航空工业集团公司北京航空制造工程研究所 | Preparation method for continuous fiber reinforced titanium-titanium aluminum hybrid matrix composite material |
| CN203545695U (en) * | 2013-11-01 | 2014-04-16 | 刘新保 | Microwave pressurizing synthesizing device |
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