CN105908107A - SiC fiber-reinforced TiAl-based composite with Mo coating and preparation method of SiC fiber-reinforced TiAl-based composite - Google Patents
SiC fiber-reinforced TiAl-based composite with Mo coating and preparation method of SiC fiber-reinforced TiAl-based composite Download PDFInfo
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- CN105908107A CN105908107A CN201610421289.3A CN201610421289A CN105908107A CN 105908107 A CN105908107 A CN 105908107A CN 201610421289 A CN201610421289 A CN 201610421289A CN 105908107 A CN105908107 A CN 105908107A
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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
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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
- C22C47/20—Making alloys containing metallic or non-metallic fibres or filaments by subjecting to pressure and heat an assembly comprising at least one metal layer or sheet and one layer of fibres or filaments
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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
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides an SiC fiber-reinforced TiAl-based composite with an Mo coating and a preparation method of the SiC fiber-reinforced TiAl-based composite. The preparation method comprises the steps of firstly, preparing a layer of C coating with the thickness of 2-4[mu]m on the surface of SiC fiber by using a chemical vapor deposition process; then, uniformly depositing an Mo metal coating with the thickness of 0.5-2[mu]m on the surface of the SiC fiber with the C coating by using a magnetron sputtering deposition process; and finally, preparing the SiC fiber-reinforced TiAl-based composite with the Mo coating by using a foil-fiber-foil process or a fiber coating process. The interface reaction speed of the fiber and a matrix and the consumption speed of the C coating of the fiber under a high-temperature condition are effectively reduced, and the Mo coating is excellent in thermal stability, does not participate in the interface reaction, is not diffused and can be used for effectively relieving the thermal residual stress at the interface of the composite.
Description
Technical field
The present invention relates to the technology of preparing of magnetron sputtering physical deposition techniques and metal-base composites, it is possible to utilize fibre
Composite material interface performance is improved by dimension coating.
Background technology
SiC Fiber Reinforced Ti Al based composites compared to tradition titanium matrix composite have higher use temperature and
Preferably creep-resistant property, it is possible to meet the aerospace components demand to material property further, so SiC fiber
Strengthen TiAl based composites and obtain the concern of countries in the world.
But during high temperature preparation and high-temperature service, interfacial reaction can occur between TiAl matrix and SiC fiber,
And compared to conventional titanium alloy, the poor TiAl-base alloy matrix of plasticity is easier to out under the effect of thermal residual strain
Split, so that the mechanical property of composite deteriorates.Therefore, need to consider to introduce interface modification coating to reach to slow down boundary
Face is reacted and improves the purpose of composite material interface thermal residual strain.
At present, Application comparison interface modification coating technology widely is to coat one layer of C coating, knot at SiC fiber surface
Fruit shows that C coating can efficiently reduce fiber damage in preparation process, but this coating hinders interfacial reaction
Limited in one's ability, and at high temperature easily loss is serious, and additionally C element at high temperature can diffuse into TiAl in a large number
Alloy substrate, makes matrix the most brittle, causes the overall performance of composite to decline.Harbin Institute of Technology
Having invented a kind of TiN coating SiC Fiber Reinforced Ti based composites, research shows that this coating the most effectively slow down fibre
Tie up the extent of reaction with matrix and good interface bond strength (number of patent application is also obtained
201110003731.8), but TiN coating is fragile material, is prone to first under mechanical load and thermal residual strain effect
First ftracture, additionally, literature research shows, this coating preparation process easily makes fibre strength reduce.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of Mo coating SiC Fiber Reinforced Ti Al base composite wood
The preparation method of material, economically feasible, it is easy to preparation, it is possible to improve the interface performance of TiAl based composites further.
The technical solution adopted for the present invention to solve the technical problems is: a kind of Mo coating SiC Fiber Reinforced Ti Al base
Composite, if the TiAl-base alloy foil replaced including dried layer and Mo coating SiC fiber, described Mo coating
SiC fiber refers to the SiC fiber surface uniform deposition Mo metal using magnetron sputtered deposition technology in existing C coating
The fiber that coating prepares.
Described Mo metal coating thickness is 0.5-2 μm, and described C coating layer thickness is 2-4 μm.
The present invention also provides for the preparation method of a kind of Mo coating SiC Fiber Reinforced Ti Al based composites, including following step
Rapid: to prepare, at SiC fiber surface, the C coating that a layer thickness is 2-4 μm initially with chemical vapor deposition method；Then
Use magnetron sputtering deposition technique at the Mo metal that SiC fiber surface uniform deposit thickness is 0.5-2 μm of existing C coating
Coating；Paper tinsel-fiber-paper tinsel method or fiber coat method is finally used to prepare Mo coating SiC Fiber Reinforced Ti Al base composite wood
Material；Described paper tinsel-fiber-paper tinsel method is with the TiAl-base alloy foil being stacked alternately and the SiC fiber vacuum with Mo coating
Hot pressing forms；Described fiber coat method is to continue one layer of TiAl alloy coating of deposition on the SiC fiber have Mo coating,
If hot pressing forms after dried layer deposited the SiC fibre compact stacking of TiAl alloy coating.
The method of TiAl-base alloy Wire EDM is processed growth 50mm, width by described paper tinsel-fiber-paper tinsel method
10mm, thickness are the foil of 300 μm, and pass through mechanical lapping by thinning for thickness for 150-200 μm；To prepare
Mo coating SiC fiber and TiAl-base alloy foil use the method for one layer of fiber of one layer of foil the most neatly to fold
Put, put in vacuum hotpressing stove hot pressing for Mo coating SiC Fiber Reinforced Ti Al based composites.
Described fiber coat method continues preparation by using magnetron sputtered deposition technology on the SiC fiber with C, Mo coating
The TiAl alloy coating of one layer of 50-200 μm；By some SiC fibre compact heaps with C, Mo and TiAl alloy coating
Buttress, in mould, puts in vacuum hotpressing stove hot pressing for Mo coating SiC Fiber Reinforced Ti Al based composites.
The invention has the beneficial effects as follows: for Mo coating SiC fiber reinforcement γ-TiAl based composites, Mo coating
Introducing effectively slow down the interfacial reaction of fiber and matrix, significantly slow down C coating that fiber carries at high-temperature condition
Under depletion rate, and the excellent heat stability of Mo coating, be not involved in interfacial reaction, do not spread；
For Mo coating SiC Fiber Reinforced Ti 2AlNb based composites, it is steady that Mo coating has good heat equally
Qualitative, and Mo coating slow down interfacial reaction, is delayed C coating consumption, dissolving on a small quantity of Mo atom makes simultaneously
Ti2AlNb matrix alloy near fiber by βization, can effectively alleviate the thermal residual strain at composite material interface.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of the present invention；
Fig. 2 is the schematic diagram of Mo coating SiC fiber；
Fig. 3 is the scanning electron micrograph of gained composite in embodiment 1, and wherein, a figure is As-deposited state
SiCf/C/Ti2The scanning electron micrograph of AlNb composite, b figure is As-deposited state SiCf/C/Mo/Ti2AlNb is combined
The scanning electron micrograph of material, c figure is the SiC of 940 DEG C of beat exposure 100hf/C/Ti2Sweeping of AlNb composite
Retouching electron micrograph, d figure is the SiC of 940 DEG C of beat exposure 100hf/C/Mo/Ti2The scanning electron of AlNb composite
Microphoto；
Fig. 4 is the scanning electron micrograph of gained composite in embodiment 2, and wherein, a figure is As-deposited state
SiCfThe scanning electron micrograph of/C/ γ-TiAl composite, b figure is As-deposited state SiCf/ C/Mo/ γ-TiAl composite
Scanning electron micrograph, c figure is the SiC of 900 DEG C of beat exposure 200hfThe scanning electron of/C/ γ-TiAl composite
Microphoto, d figure is the SiC of 900 DEG C of beat exposure 200hfThe scanning electron micrograph of/C/ γ-TiAl composite.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings, and the present invention includes but are not limited to following embodiment.
The present invention is having the pure Mo coating of SiC fiber surface sputtering sedimentation one layer of C coating, and sputter deposition process will not be as changing
Learn vapour deposition and reduce fibre strength and surface quality, and the method economically feasible like that because of high temperature exposure, it is easy to
Preparation.Additionally, Mo coating coating while slowing down interfacial reaction itself also has good heat endurance；Mo element
β phase stable element as Ti alloy can make SiC Fiber Reinforced Ti Al based composites generate more near interface
β-Ti, plasticity preferable β-Ti can slow down the thermal residual strain of interface, and then improve the mechanical property of composite.
The present invention uses paper tinsel-fiber-paper tinsel method or fiber coat method to prepare Mo coating SiC Fiber Reinforced Ti Al base composite wood
Material, preparation flow is as shown in Figure 1.Described paper tinsel-fiber-paper tinsel method is i.e. with the TiAl-base alloy foil being stacked alternately and Mo
The method that coating SiC fiber prepares composite by HTHP in vacuum hotpressing stove；Described fiber coat method is
Refer on the SiC fiber of existing Mo coating, continue one layer of TiAl alloy coating of deposition, TiAl will be prepared in a mold and close
The method preparing composite by HTHP after the SiC fibre compact stacking of gold plating.In two kinds of preparation methods
Mo coating SiC fiber refers to the SiC fiber surface uniform deposition using magnetron sputtered deposition technology in existing C coating
The fiber that the Mo metal coating of 0.5-2 μ m-thick prepares, wherein C coating layer thickness is 2-4 μm, utilizes chemical gaseous phase to sink
Prepared by long-pending technique, the effect of C coating is to improve fibrous mechanical property further, and protection fiber is susceptible to damage.
In the present invention, paper tinsel-fiber-paper tinsel method prepares Mo coating SiC Fiber Reinforced Ti Al based composites mainly by following
Several steps realize:
(1) chemical vapor deposition method (CVD) is used to prepare the C coating of one layer of 2-4 μm at SiC fiber surface；
(2) then use magnetron sputtering deposition technique (PVD) at the SiC fiber surface uniform deposition of existing C coating
The Mo metal coating of 0.5-2 μ m-thick；
(3) method of TiAl-base alloy Wire EDM is processed growth 50mm, wide 10mm, thickness are 300 μm
Foil, and by mechanical lapping by thinning for thickness for 150-200 μm；
(4) the Mo coating SiC fiber prepared in (2) (3) step is used one layer with TiAl-base alloy foil
The method of one layer of fiber of foil the most neatly stacks, and puts in vacuum hotpressing stove and prepares Mo coating by HTHP
SiC Fiber Reinforced Ti Al based composites；
(5) the method edge of the composite Wire EDM prepared is perpendicular to machine direction and cuts into block,
Being respectively put in stainless steel tube by a part of sample and carry out soldering and sealing on vacuum seal equipment, steel pipe is put after completing by soldering and sealing
Enter and chamber type electric resistance furnace carries out beat exposure process, analog composite material Microstructural evolution at high temperature.
In the present invention, fiber coat method prepares Mo coating SiC Fiber Reinforced Ti Al based composites mainly by following several
Individual step realizes:
(1) chemical vapor deposition method (CVD) is used to prepare the C coating of one layer of 2-4 μm at SiC fiber surface；
(2) magnetron sputtering deposition technique (PVD) is used to have the SiC fiber surface uniform deposition 0.5-2 μm of the coating of C
Thick Mo metal coating；
(3) magnetron sputtering deposition skill is used on the SiC fiber with C, Mo coating then obtained in step (2)
Art (PVD) continues the TiAl alloy coating of one layer of 50-200 μm of preparation；
(4) it is stacked in preparing the SiC fibre compact with C, Mo and TiAl alloy coating in mould, then
Mould is put into vacuum hotpressing stove is prepared Mo coating SiC Fiber Reinforced Ti Al based composites at high temperature under high pressure；
(5) the method edge of the composite Wire EDM prepared is perpendicular to machine direction and cuts into block,
Being respectively put in stainless steel tube by a part of sample and carry out soldering and sealing on vacuum seal equipment, steel pipe is put after completing by soldering and sealing
Enter and chamber type electric resistance furnace carries out beat exposure process, analog composite material Microstructural evolution at high temperature.
Embodiment 1
(1) initially with direct current heating chemical vapour deposition (CVD) device SiC fiber surface prepare as
Pyrolysis C coating 1 shown in Fig. 2, thickness is 2 μm；
(2) the SiC fiber of existing C coating is wrapped on the rotating cage that sputter sputtering uses, in winding process really
Protect and do not overlap between fiber.After winding fiber, rotating cage is put into JGP-560A type high vacuum rectangular target magnetron sputtering
Instrument carries out the preparation of Mo coating, and splash-proofing sputtering process parameter is 875W/0.63Pa/40min, preparation effect as in figure 2 it is shown,
And the thickness of Mo coating 2 is 1.3 μm.After sputtering, fiber is taken out, be cut to the segment of long 100mm
Final vacuum preserves in case using；
(3) by Ti that nominal composition is Ti-21Al-29Nb (at%)2The method of AlNb base alloy Wire EDM
Process long 50mm, wide 10mm, thickness are the foil 5 of 300 μm, put in acetone soln clear with ultrasonic wave
After washing 30min removal foil surface and oil contaminant, remove the oxide on foil surface by the method for mechanical lapping and reduce foil
Thickness is to 150-200 μm.Finally foil is put into Kroll reagent (5%HF, 10%HNO3, 85%H2O) leaching in
Take out to place into after bubble 3min and absolute ethyl alcohol carries out Ultrasonic Cleaning 30min post-drying, and foil is put into dry
Case preserves in case using；
(4) Mo coating SiC fiber step (2) prepared knits out length with traditional Mo silk weave
100mm, wide 10mm, with the Ti that obtains in step (3) after 4 layers of fiber of interval 0.1mm2AlNb base Alloy Foil
Material the most neatly stacks according to the order of one layer of fiber of one layer of foil；
(5) then the mould stacking foil and fiber is put in ZKG-13 type vacuum hotpressing stove, heat pressing process
Parameter is 980 DEG C/70MPa/100min, cools to room temperature after having prepared with the furnace, i.e. obtains Mo coating SiC fine
Dimension strengthens Ti2AlNb based composites.The As-deposited state SEM scanned photograph of this composite as shown in Figure 3 b, is compared
The Ti of Mo coating is not had in Fig. 3 a2AlNb based composites, due to the introducing of Mo coating so that near fiber
Matrix generate one layer of obvious ring-type β-Ti, plasticity preferable β-Ti and can effectively alleviate the residual thermal stress at interface.
Take thickness by the method for Wire EDM and be 2mm sample and put into outside internal diameter 8mm along being perpendicular to machine direction
The stainless steel tube of footpath 10mm carries out on vacuum seal equipment soldering and sealing, by sample soldering and sealing in vacuum higher than 10-4Pa
Under above vacuum environment, soldering and sealing after completing the steel pipe with sample put into chamber type electric resistance furnace is carried out 700 DEG C,
At 800 DEG C, 900 DEG C and 1000 DEG C, the Vacuum Heat exposure of 100 and 200h processes, and analog composite material is at high temperature
Microstructural evolution.Comparison diagram 3c and 3d it can be seen that in high temperature environments, has the SiC fiber of Mo coating
Strengthen Ti2The interface of AlNb based composites is more stable.
Embodiment 2
(1) initially with direct current heating chemical vapour deposition (CVD) device SiC fiber surface prepare as
Pyrolysis C coating 1 shown in Fig. 2, thickness is 2 μm；
(2) the SiC fiber of existing C coating is wrapped on the rotating cage that sputter sputtering uses, in winding process really
Protect and do not overlap between fiber.After winding fiber, rotating cage is put into JGP-560A type high vacuum rectangular target magnetron sputtering
Instrument carries out the preparation of Mo coating, and splash-proofing sputtering process parameter is 875W/0.63Pa/40min, preparation effect as in figure 2 it is shown,
And Mo coating 2 thickness is 1.3 μm.After sputtering, fiber is taken out, after being cut to the segment of long 100mm
Vacuum preserves in case using；
(3) after treating the sputtering of Mo coating, Mo metal targets being taken out, changing nominal composition is
The gamma-TiAl alloy target of Ti-43Al-9V (at%), continues to deposit one layer of gamma-TiAl alloy coating in Mo coating.Spatter
Penetrating power is 600W, and sputtering pressure is 0.8Pa, after the gamma-TiAl alloy coating of SiC fiber surface reaches 80 μm,
Stop sputtering and take out fiber；
(4) by preparing the fiber with C, Mo and gamma-TiAl alloy coating, to cut into a length of 100mm little
Intensive after Duan it is stacked in mould, notes padding aluminium oxide ceramics pad up and down at mould, prevent in hot pressing
Composite and die bonds in journey；
(5) then being put into by mould in ZKG-13 type vacuum hotpressing stove, technological parameter is 1150 DEG C/150MPa/40
Min, cools to room temperature with the furnace after having prepared, i.e. obtain Mo coating SiC fiber reinforcement γ-TiAl based composites.
The As-deposited state SEM scanned photograph of this composite as shown in Figure 4 b, compared to the γ-TiAl not having Mo coating in Fig. 4 a
Based composites, the thickness of its conversion zone is the most thinner, illustrates that Mo coating serves the work slowing down interfacial reaction
With.
Take thickness by the method for Wire EDM and be 2mm sample and put into outside internal diameter 8mm along being perpendicular to machine direction
The stainless steel tube of footpath 10mm carries out on vacuum seal equipment soldering and sealing, by sample soldering and sealing in vacuum higher than 10-4Pa
Under above vacuum environment, soldering and sealing after completing the steel pipe with sample put into chamber type electric resistance furnace is carried out 700 DEG C,
At 800 DEG C, 900 DEG C and 1000 DEG C, the Vacuum Heat exposure of 100 and 200h processes, and analog composite material is at high temperature
Microstructural evolution.Comparison diagram 4c and 4d, it can be seen that the SiC fiber reinforcement γ-TiAl base having Mo coating is multiple
Condensation material interface heat endurance will be significantly better than the composite not having Mo coating.
Claims (5)
1. a Mo coating SiC Fiber Reinforced Ti Al based composites, it is characterised in that: if including dried layer TiAl alternately
Base alloy foil and Mo coating SiC fiber, described Mo coating SiC fiber refers to use magnetron sputtering deposition
The fiber that technology prepares at the SiC fiber surface uniform deposition Mo metal coating of existing C coating.
Mo coating SiC Fiber Reinforced Ti Al based composites the most according to claim 1, it is characterised in that: institute
The Mo metal coating thickness stated is 0.5-2 μm, and described C coating layer thickness is 2-4 μm.
3. a preparation method for Mo coating SiC Fiber Reinforced Ti Al based composites, its feature described in claim 1
It is to comprise the steps: that preparing a layer thickness initially with chemical vapor deposition method at SiC fiber surface is
The C coating of 2-4 μm；Then use magnetron sputtering deposition technique uniform at the SiC fiber surface of existing C coating
Deposit thickness is the Mo metal coating of 0.5-2 μm；Paper tinsel-fiber-paper tinsel method or fiber coat method is finally used to prepare
Mo coating SiC Fiber Reinforced Ti Al based composites；Described paper tinsel-fiber-paper tinsel method is with the TiAl being stacked alternately
Base alloy foil and the SiC fiber vacuum hot pressing with Mo coating form；Described fiber coat method is to have
Continuing one layer of TiAl alloy coating of deposition on the SiC fiber of Mo coating, being coated with if dried layer be deposited TiAl alloy
After the SiC fibre compact stacking of layer, hot pressing forms.
The preparation method of Mo coating SiC Fiber Reinforced Ti Al based composites the most according to claim 3, it is special
Levy and be: described paper tinsel-fiber-paper tinsel method the method for TiAl-base alloy Wire EDM is processed growth 50mm,
Wide 10mm, thickness are the foil of 300 μm, and pass through mechanical lapping by thinning for thickness for 150-200 μm；Will system
The standby Mo coating SiC fiber obtained and TiAl-base alloy foil use the method for one layer of fiber of one layer of foil at mould
Tool neatly stacks, puts in vacuum hotpressing stove hot pressing for Mo coating SiC Fiber Reinforced Ti Al base composite wood
Material.
The preparation method of Mo coating SiC Fiber Reinforced Ti Al based composites the most according to claim 3, it is special
Levy and be: described fiber coat method will use magnetron sputtering deposition skill on the SiC fiber with C, Mo coating
Art continues the TiAl alloy coating of one layer of 50-200 μm of preparation；It is coated with some with C, Mo and TiAl alloy
The SiC fibre compact of layer is stacked in mould, puts into hot pressing in vacuum hotpressing stove and increases for Mo coating SiC fiber
Strong TiAl based composites.
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| CN106521369A (en) * | 2016-11-29 | 2017-03-22 | 中国科学院金属研究所 | Dense precursor belt of SiC fiber-reinforced titanium-based composite and preparation method of dense precursor belt |
| CN106947949A (en) * | 2017-04-06 | 2017-07-14 | 中南大学 | A kind of SiC continuous fibers of double coatings containing Al/Cu and its preparation method and application |
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| CN110241366A (en) * | 2019-08-02 | 2019-09-17 | 西北工业大学 | A kind of Mo coating SiC Fiber Reinforced Ti Al based composites and preparation method thereof |
| CN113481479A (en) * | 2021-07-02 | 2021-10-08 | 吉林大学 | SiC fiber reinforced refractory alloy composite material and preparation method and application thereof |
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| CN113481479A (en) * | 2021-07-02 | 2021-10-08 | 吉林大学 | SiC fiber reinforced refractory alloy composite material and preparation method and application thereof |
| CN113481479B (en) * | 2021-07-02 | 2022-08-05 | 吉林大学 | SiC fiber reinforced refractory alloy composite material and preparation method and application thereof |
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Application publication date: 20160831 |