CN110241366A - A kind of Mo coating SiC Fiber Reinforced Ti Al based composites and preparation method thereof - Google Patents
A kind of Mo coating SiC Fiber Reinforced Ti Al based composites and preparation method thereof Download PDFInfo
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- CN110241366A CN110241366A CN201910710170.1A CN201910710170A CN110241366A CN 110241366 A CN110241366 A CN 110241366A CN 201910710170 A CN201910710170 A CN 201910710170A CN 110241366 A CN110241366 A CN 110241366A
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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
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/12—Intermetallic matrix material
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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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Abstract
The present invention provides a kind of Mo coating SiC Fiber Reinforced Ti Al based composites and preparation method thereof, and chemical vapor deposition process is used to prepare a layer thickness in SiC fiber surface as 2-4 μm of C coating first；Then use magnetron sputtering depositing operation in the SiC fiber surface uniform deposit thickness of existing C coating for 0.5-2 μm of Mo metal coating；Mo coating SiC Fiber Reinforced Ti Al based composites are finally prepared using foil-fiber-foil method or fiber coat method.The depletion rate of the C coating that the present invention effectively slows down the interfacial reaction of fiber and matrix and fiber carries in the case of a high temperature, the excellent heat stability of Mo coating, it is not involved in interfacial reaction, is not also spread, the thermal residual strain at composite material interface can be effectively relieved.
Description
Technical field
The present invention relates to magnetron sputtering physical deposition techniques and the technologies of preparing of metal-base composites, can utilize fibre
Dimension coating improves composite material interface performance.
Background technique
SiC Fiber Reinforced Ti Al based composites compared to traditional titanium composite material have it is higher using temperature and
Better creep-resistant property, can demand of the further satisfaction aerospace components to material property, so SiC fiber reinforcement
TiAl based composites have obtained the concern of countries in the world.
However during high temperature preparation and high-temperature service, interfacial reaction can occur between TiAl matrix and SiC fiber, and
And compared to conventional titanium alloy, the poor TiAl-base alloy matrix of plasticity is easier to crack under the action of thermal residual strain, from
And deteriorate the mechanical property of composite material.Therefore, it need to consider that introduce interface modification coating slows down interfacial reaction and change to reach
The purpose of kind composite material interface thermal residual strain.
Currently, being to coat one layer of C coating in SiC fiber surface using more extensive interface modification coating technology, as a result
Show that the damage of fiber during the preparation process can be effectively reduced in C coating, but this coating hinders the ability of interfacial reaction
It is limited, and it is easy loss at high temperature seriously, in addition C element can largely diffuse into TiAl alloy matrix at high temperature, make
Matrix is further brittle, and the overall performance of composite material is caused to decline.A kind of TiN coating has been invented by Harbin Institute of Technology
SiC Fiber Reinforced Ti based composites, research shows that the coating not only effectively slow down the extent of reaction of fiber and matrix but also
It is also obtained good interface bond strength (number of patent application 201110003731.8), but TiN coating is fragile material,
It is easy to crack first under mechanical load and thermal residual strain effect, in addition, literature research shows to be easy in the coating preparation process
Reduce fibre strength.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of Mo coating SiC Fiber Reinforced Ti Al based composites
Preparation method, economically feasible is easily prepared, can further increase the interface performance of TiAl based composites.
The technical solution adopted by the present invention to solve the technical problems is: a kind of Mo coating SiC Fiber Reinforced Ti Al base is multiple
Condensation material, including the alternate TiAl-base alloy foil of several layers and Mo coating SiC fiber, the Mo coating SiC fiber refer to
The fiber being prepared using magnetron sputtered deposition technology in the SiC fiber surface uniform deposition Mo metal coating of existing C coating.
For the Mo metal coating with a thickness of 0.5-2 μm, the C coating layer thickness is 2-4 μm.
The present invention also provides a kind of preparation methods of Mo coating SiC Fiber Reinforced Ti Al based composites, including following step
It is rapid: chemical vapor deposition process being used to prepare a layer thickness in SiC fiber surface as 2-4 μm of C coating first；Then magnetic is used
Control the Mo metal coating that sputter deposition craft is 0.5-2 μm in the SiC fiber surface uniform deposit thickness of existing C coating；Finally
Mo coating SiC Fiber Reinforced Ti Al based composites are prepared using foil-fiber-foil method or fiber coat method；Foil-the fibre
Dimension-foil method is formed with the TiAl-base alloy foil being stacked alternately and the SiC fiber vacuum hot pressing with Mo coating；The fibre
Dimension coating is to continue to deposit one layer of TiAl alloy coating on the SiC fiber for having Mo coating, and several layers deposited TiAl and close
Hot pressing forms after the SiC fibre compact stacking of gold plating.
The method of TiAl-base alloy Wire EDM is processed growth 50mm, width by the foil-fiber-foil method
10mm, with a thickness of 300 μm of foils, and it is 150-200 μm that thickness, which is thinned, by mechanical lapping；The Mo coating that will be prepared
SiC fiber is neatly stacked with TiAl-base alloy foil using the method for one layer of foil, one layer of fiber in a mold, is put into Vacuum Heat
Hot pressing is in pressure furnace for Mo coating SiC Fiber Reinforced Ti Al based composites.
The fiber coat method will continue to prepare on the SiC fiber with C, Mo coating using magnetron sputtered deposition technology
One layer 50-200 μm of TiAl alloy coating；Several SiC fibre compacts with C, Mo and TiAl alloy coating are stacked in
In mold, hot pressing is put into vacuum hotpressing stove for Mo coating SiC Fiber Reinforced Ti Al based composites.
The beneficial effects of the present invention are: for Mo coating SiC fiber reinforcement γ-TiAl based composites, Mo coating draws
Enter the interfacial reaction for effectively slowing down fiber and matrix, slows down the consumption of the included C coating of fiber in the case of a high temperature significantly
Speed, and the excellent heat stability of Mo coating, are not involved in interfacial reaction, also do not spread；
For Mo coating SiC Fiber Reinforced Ti 2AlNb based composites, Mo coating equally has good thermal stability,
And Mo coating slows down interfacial reaction, delays the consumption of C coating, while a small amount of of Mo atom is dissolved in so that near fiber
The thermal residual strain at composite material interface can be effectively relieved by βization in Ti2AlNb matrix alloy.
Detailed description of the invention
Fig. 1 is preparation technology flow chart of the invention；
Fig. 2 is the schematic diagram of Mo coating SiC fiber；
Fig. 3 is the scanning electron micrograph of gained composite material in embodiment 1, wherein a figure is As-deposited state SiCf/C/
Ti2The scanning electron micrograph of AlNb composite material, b figure are As-deposited state SiCf/C/Mo/Ti2The scanning electricity of AlNb composite material
Sub- microphoto, c figure are the SiC of 940 DEG C of heat exposure 100hf/C/Ti2The scanning electron micrograph of AlNb composite material, d figure
It is the SiC of 940 DEG C of heat exposure 100hf/C/Mo/Ti2The scanning electron micrograph of AlNb composite material；
Fig. 4 is the scanning electron micrograph of gained composite material in embodiment 2, wherein a figure is As-deposited state SiCf/C/
The scanning electron micrograph of γ-TiAl composite material, b figure are As-deposited state SiCfThe scanning of/C/Mo/ γ-TiAl composite material
Electron micrograph, c figure are the SiC of 900 DEG C of heat exposure 200hfThe scanning electron micrograph of/C/ γ-TiAl composite material, d
Figure is the SiC of 900 DEG C of heat exposure 200hfThe scanning electron micrograph of/C/ γ-TiAl composite material.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples, and the present invention includes but are not limited to following implementations
Example.
For the present invention in the pure Mo coating of one layer of SiC fiber surface sputtering sedimentation for having C coating, sputter deposition process will not be as changing
Learning vapor deposition reduces fibre strength and surface quality, and this method economically feasible because of high temperature exposure like that, easily prepared.
In addition, Mo coating coating while slowing down interfacial reaction itself also has good thermal stability；β of the Mo element as Ti alloy
Phase stable element can make SiC Fiber Reinforced Ti Al based composites generate more β-Ti near interface, and plasticity is preferable
β-Ti can slow down the thermal residual strain of interface, and then improve the mechanical property of composite material.
The present invention prepares Mo coating SiC Fiber Reinforced Ti Al base composite wood using foil-fiber-foil method or fiber coat method
Material, preparation flow are as shown in Figure 1.Foil-fiber-foil the method is with the TiAl-base alloy foil and Mo coating being stacked alternately
The method that SiC fiber prepares composite material by high temperature and pressure in vacuum hotpressing stove；The fiber coat method refers to
Continue to deposit one layer of TiAl alloy coating on the SiC fiber for having Mo coating, the SiC of TiAl alloy coating will be prepared in a mold
The method that composite material is prepared by high temperature and pressure after fibre compact stacking.Mo coating SiC fiber in two kinds of preparation methods is
Refer to the Mo metal coating system using magnetron sputtered deposition technology in the SiC fiber surface uniform deposition 0.5-2 μ m-thick of existing C coating
Standby obtained fiber, wherein C coating layer thickness is 2-4 μm, is prepared using chemical vapor deposition process, the effect of C coating is into one
Step improves fibrous mechanical property, protects fiber not subject to damage.
Foil-fiber-foil method preparation Mo coating SiC Fiber Reinforced Ti Al based composites mainly pass through following in the present invention
What several steps were realized:
(1) one layer 2-4 μm of C coating is prepared in SiC fiber surface using chemical vapor deposition process (CVD)；
(2) then using magnetron sputtering depositing operation (PVD) in the SiC fiber surface uniform deposition 0.5-2 for having C coating
The Mo metal coating of μ m-thick；
(3) by method processing growth 50mm, the wide 10mm of TiAl-base alloy Wire EDM, with a thickness of 300 μm
Foil, and it is 150-200 μm that thickness, which is thinned, by mechanical lapping；
(4) the Mo coating SiC fiber being prepared in (2) (3) step and TiAl-base alloy foil are used into one layer of foil
The method of one layer of fiber neatly stacks in a mold, is put into vacuum hotpressing stove and prepares Mo coating SiC fiber by high temperature and pressure
Enhance TiAl based composites；
It is (5) method for the composite material Wire EDM being prepared is blocking along cutting perpendicular to machine direction,
A part of sample is respectively put into stainless steel tube in vacuum seal equipment and carries out soldering and sealing, steel pipe is put into case after the completion of soldering and sealing
Heat exposure processing, the Microstructural evolution of analog composite material at high temperature are carried out in formula resistance furnace.
Fiber coat method preparation Mo coating SiC Fiber Reinforced Ti Al based composites mainly pass through following several in the present invention
What a step was realized:
(1) one layer 2-4 μm of C coating is prepared in SiC fiber surface using chemical vapor deposition process (CVD)；
(2) using magnetron sputtering depositing operation (PVD) in the SiC fiber surface uniform deposition 0.5-2 μ m-thick for having C coating
Mo metal coating；
(3) magnetron sputtered deposition technology is used on the SiC fiber with C, Mo coating then obtained in step (2)
(PVD) continue the TiAl alloy coating of one layer 50-200 μm of preparation；
(4) the SiC fibre compact with C, Mo and TiAl alloy coating will be prepared to be stacked in mold, then by mould
Tool is put into vacuum hotpressing stove prepares Mo coating SiC Fiber Reinforced Ti Al based composites at high temperature under high pressure；
It is (5) method for the composite material Wire EDM being prepared is blocking along cutting perpendicular to machine direction,
A part of sample is respectively put into stainless steel tube in vacuum seal equipment and carries out soldering and sealing, steel pipe is put into case after the completion of soldering and sealing
Heat exposure processing, the Microstructural evolution of analog composite material at high temperature are carried out in formula resistance furnace.
Embodiment 1
(1) it is prepared first in SiC fiber surface such as Fig. 2 institute using direct current heating chemical vapor deposition (CVD) device
The pyrolysis C coating 1 shown, with a thickness of 2 μm；
(2) the SiC fiber of existing C coating is wrapped on the rotating cage that sputter sputtering uses, fibre is ensured in winding process
It is not overlapped between dimension.It winds and rotating cage is put into JGP-560A type high vacuum rectangular target magnetic control sputtering device after fiber carries out Mo painting
Layer preparation, splash-proofing sputtering process parameter 875W/0.63Pa/40min, preparation effect as shown in Fig. 2, and Mo coating 2 with a thickness of
1.3μm.Fiber is taken out after sputtering, vacuum saves in case using after being cut to the segment of long 100mm；
It (3) is the Ti of Ti-21Al-29Nb (at%) by nominal composition2The method of AlNb based alloy Wire EDM
It processes long 50mm, wide 10mm, with a thickness of foil 5 of 300 μm, is put into acetone soln and is removed with ultrasonic cleaning 30min
After foil surface and oil contaminant, the oxide on foil surface is removed with the method for mechanical lapping and reduces foil thickness to 150-200 μm.
Foil is finally put into Kroll reagent (5%HF, 10%HNO3, 85%H2O taking-up places into dehydrated alcohol after impregnating 3min in)
It is dried after middle progress ultrasonic cleaning 30min, and foil is put into drying box and is saved in case using；
(4) the Mo coating SiC fiber that step (2) is prepared is knit out into long 100mm with traditional Mo silk weave, it is wide
10mm is spaced after 4 layers of fiber of 0.1mm and Ti obtained in step (3)2AlNb based alloy foil is according to one layer of foil, one layer of fibre
The sequence of dimension neatly stacks in a mold；
(5) then the mold for stacking foil and fiber is put into ZKG-13 type vacuum hotpressing stove, hot pressing parameters
For 980 DEG C/70MPa/100min, room temperature is cooled to after the completion of preparation with the furnace to get Mo coating SiC Fiber Reinforced Ti is arrived2AlNb
Based composites.The As-deposited state SEM scanned photograph of the composite material is as shown in Figure 3b, compared to not having Mo coating in Fig. 3 a
Ti2AlNb based composites, due to the introducing of Mo coating, so that the matrix near fiber generates one layer of apparent ring-type β-
The residual thermal stress at interface can be effectively relieved in Ti, the preferable β-Ti of plasticity.
It is taken with the method for Wire EDM edge perpendicular to machine direction with a thickness of 2mm sample and is put into internal diameter 8mm outer diameter
Soldering and sealing is carried out in the stainless steel tube of 10mm in vacuum seal equipment, sample soldering and sealing is higher than 10 in vacuum degree-4Pa's or more is true
The steel pipe with sample is put into chamber type electric resistance furnace under Altitude, after the completion of soldering and sealing carry out 700 DEG C, 800 DEG C, 900 DEG C and
The Vacuum Heat exposure treatment of 100 and 200h at 1000 DEG C, the Microstructural evolution of analog composite material at high temperature.Comparison diagram 3c
With 3d as can be seen that under high temperature environment, there is the SiC Fiber Reinforced Ti of Mo coating2The interface of AlNb based composites is more steady
It is fixed.
Embodiment 2
(1) it is prepared first in SiC fiber surface such as Fig. 2 institute using direct current heating chemical vapor deposition (CVD) device
The pyrolysis C coating 1 shown, with a thickness of 2 μm；
(2) the SiC fiber of existing C coating is wrapped on the rotating cage that sputter sputtering uses, fibre is ensured in winding process
It is not overlapped between dimension.It winds and rotating cage is put into JGP-560A type high vacuum rectangular target magnetic control sputtering device after fiber carries out Mo painting
Layer preparation, splash-proofing sputtering process parameter 875W/0.63Pa/40min, preparation effect as shown in Fig. 2, and Mo coating 2 with a thickness of 1.3
μm.Fiber is taken out after sputtering, vacuum saves in case using after being cut to the segment of long 100mm；
(3) after to the sputtering of Mo coating, Mo metal targets are taken out, replacement nominal composition is Ti-43Al-9V (at%)
Gamma-TiAl alloy target, continue on Mo coating deposit one layer of gamma-TiAl alloy coating.Sputtering power is 600W, sputters gas
Pressure is 0.8Pa, after the gamma-TiAl alloy coating of SiC fiber surface reaches 80 μm, stops sputtering and takes out fiber；
(4) it is close after 100mm segment for preparing the fiber with C, Mo and gamma-TiAl alloy coating and be cut into length
Collection is stacked in mold, is paid attention to padding aluminium oxide ceramics gasket up and down in mold, is prevented the composite material in hot pressing
With die bonds；
(5) then mold being put into ZKG-13 type vacuum hotpressing stove, technological parameter is 1150 DEG C/150MPa/40min,
Room temperature is cooled to after the completion of preparation with the furnace to get Mo coating SiC fiber reinforcement γ-TiAl based composites are arrived.The composite material
As-deposited state SEM scanned photograph it is as shown in Figure 4 b, it is anti-compared to there is no the γ-TiAl based composites of Mo coating in Fig. 4 a
It answers the thickness of layer obvious thinner, illustrates that Mo coating plays the role of slowing down interfacial reaction.
It is taken with the method for Wire EDM edge perpendicular to machine direction with a thickness of 2mm sample and is put into internal diameter 8mm outer diameter
Soldering and sealing is carried out in the stainless steel tube of 10mm in vacuum seal equipment, sample soldering and sealing is higher than 10 in vacuum degree-4Pa's or more is true
The steel pipe with sample is put into chamber type electric resistance furnace under Altitude, after the completion of soldering and sealing carry out 700 DEG C, 800 DEG C, 900 DEG C and
The Vacuum Heat exposure treatment of 100 and 200h at 1000 DEG C, the Microstructural evolution of analog composite material at high temperature.Comparison diagram 4c
And 4d, it can be seen that having the SiC fiber reinforcement γ-TiAl based composite material interface thermal stability of Mo coating to be significantly better than does not have
The composite material of Mo coating.
Claims (5)
1. a kind of Mo coating SiC Fiber Reinforced Ti Al based composites, it is characterised in that: closed including the alternate TiAl base of several layers
Goldleaf material and Mo coating SiC fiber, the Mo coating SiC fiber refer to using magnetron sputtered deposition technology in existing C coating
The fiber that is prepared of SiC fiber surface uniform deposition Mo metal coating.
2. Mo coating SiC Fiber Reinforced Ti Al based composites according to claim 1, it is characterised in that: the Mo
For metal coating with a thickness of 0.5-2 μm, the C coating layer thickness is 2-4 μm.
3. the preparation method of Mo coating SiC Fiber Reinforced Ti Al based composites described in a kind of claim 1, it is characterised in that packet
It includes following step: chemical vapor deposition process being used to prepare a layer thickness in SiC fiber surface as 2-4 μm of C coating first；So
Magnetron sputtering depositing operation is used to apply in the SiC fiber surface uniform deposit thickness of existing C coating for 0.5-2 μm of Mo metal afterwards
Layer；Mo coating SiC Fiber Reinforced Ti Al based composites are finally prepared using foil-fiber-foil method or fiber coat method；It is described
Foil-fiber-foil method be to be formed with the TiAl-base alloy foil being stacked alternately and the SiC fiber vacuum hot pressing with Mo coating；
The fiber coat method is to continue to deposit one layer of TiAl alloy coating on the SiC fiber for having Mo coating, and several layers are deposited
Hot pressing forms after the SiC fibre compact stacking of TiAl alloy coating.
4. the preparation method of Mo coating SiC Fiber Reinforced Ti Al based composites according to claim 3, feature exist
In: the method for TiAl-base alloy Wire EDM is processed growth 50mm, width 10mm, thickness by the foil-fiber-foil method
For 300 μm of foil, and it is 150-200 μm that thickness, which is thinned, by mechanical lapping；By the Mo coating SiC fiber being prepared with
TiAl-base alloy foil is neatly stacked in a mold using the method for one layer of foil, one layer of fiber, is put into hot pressing in vacuum hotpressing stove
Prepare Mo coating SiC Fiber Reinforced Ti Al based composites.
5. the preparation method of Mo coating SiC Fiber Reinforced Ti Al based composites according to claim 3, feature exist
In: the fiber coat method will continue one layer of preparation using magnetron sputtered deposition technology on the SiC fiber with C, Mo coating
50-200 μm of TiAl alloy coating；Several SiC fibre compacts with C, Mo and TiAl alloy coating are stacked in mold
It is interior, hot pressing is put into vacuum hotpressing stove for Mo coating SiC Fiber Reinforced Ti Al based composites.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031466A (en) * | 2011-01-10 | 2011-04-27 | 哈尔滨工业大学 | TiN coating silicon carbide fiber reinforced titanium-based composite material and preparation method thereof |
| CN105908107A (en) * | 2016-06-15 | 2016-08-31 | 西北工业大学 | SiC fiber-reinforced TiAl-based composite with Mo coating and preparation method of SiC fiber-reinforced TiAl-based composite |
| CN110029292A (en) * | 2019-03-11 | 2019-07-19 | 中国航发北京航空材料研究院 | A kind of preparation method of the modified C coated fiber enhancing titanium composite material of graphene layer |
-
2019
- 2019-08-02 CN CN201910710170.1A patent/CN110241366A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031466A (en) * | 2011-01-10 | 2011-04-27 | 哈尔滨工业大学 | TiN coating silicon carbide fiber reinforced titanium-based composite material and preparation method thereof |
| CN105908107A (en) * | 2016-06-15 | 2016-08-31 | 西北工业大学 | SiC fiber-reinforced TiAl-based composite with Mo coating and preparation method of SiC fiber-reinforced TiAl-based composite |
| CN110029292A (en) * | 2019-03-11 | 2019-07-19 | 中国航发北京航空材料研究院 | A kind of preparation method of the modified C coated fiber enhancing titanium composite material of graphene layer |
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Application publication date: 20190917 |