CN106424741B - SiC particulate enhances intermetallic compound base laminar composite Ti/Al3The preparation method of Ti - Google Patents
SiC particulate enhances intermetallic compound base laminar composite Ti/Al3The preparation method of Ti Download PDFInfo
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- CN106424741B CN106424741B CN201610821138.7A CN201610821138A CN106424741B CN 106424741 B CN106424741 B CN 106424741B CN 201610821138 A CN201610821138 A CN 201610821138A CN 106424741 B CN106424741 B CN 106424741B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
- B22F2007/045—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method accompanied by fusion or impregnation
Abstract
The present invention is to provide a kind of SiC particulate enhancing intermetallic compound base laminar composite Ti/Al3The preparation method of Ti.(1) Al powder, SiC powder and stearic acid are milled in the ball mill uniformly mixed；(2) powder after ball milling is added in grinding tool and SiC particulate reinforced aluminum matrix composites is prepared using powder metallurgy process；(3) SiC particulate reinforced aluminum matrix composites are rolled into after foil plate between 450 DEG C~500 DEG C and are cut into identical size jointly with TC4 foils；(4) TC4 foils and SiC particulate reinforced aluminum matrix composites are alternately arranged；(5) it is put into vacuum hotpressing stove and carries out hot pressed sintering, be evacuated to 3 × 10 first‑2Then Pa is gradually heated to 675 DEG C~680 DEG C, keep the temperature 4 hours, then is slowly increased to 750 DEG C and keeps the temperature 3 hours.The composite material comprehensive mechanical property that the present invention prepares is excellent, and cost is lower.
Description
Technical field
The present invention relates to a kind of preparation methods of compound base layer-shaped composite material between grain reinforced metal, specifically relate to
A kind of and method being added to ceramic particle SiC in laminar composite.
Background technology
Ti-Al series intermetallic compounds because of it with density small (half of its density less than nickel-base alloy), specific strength it is high,
The features such as hardness is high, elasticity modulus is high, corrosion-resistant, mechanical behavior under high temperature and antioxygenic property are excellent, becomes people in recent years and grinds
The hot spot for studying carefully exploitation is widely used in aerospace structure material.Ti-Al series intermetallic compounds include mainly Ti3Al、
TiAl and Al3Ti, wherein Al3Ti is because it is with higher elasticity modulus (216GPa), stronger oxidation resistance and lower close
Spend (3.3g/cm3) and it is especially noticeable.But its practical application is set to be restricted because its temperature-room type plasticity toughness is too low.
In recent years about design/manufacture of laminar composite and the research of mechanical property because of its extensive concern, layer
Shape composite material can integrate each constituent element a little, make up respective deficiency, and material is made to have excellent comprehensive performance.Currently, layer
Shape composite material preparation process mainly has diffusion welding (DW) connection, roll-bonding method and hot pressing sintering method.Diffusion Welding is a kind of normal
Combined Machining Technology, can be to many of the same race or do not carry out between same material compound.Diffusion welding (DW) connection can be applied to
The high temperature alloy of hardly possible weldering, especially cast superalloy can get joint performance identical with substrate performance using Diffusion Welding,
Not macroscopical deformation, the smaller advantage of connector residual stress；But the mechanical property at Diffusion Welding product interface is relatively poor, and
Requirement to production equipment is also relatively high.Composite technique for rolling is divided into method hot rolling by blank heating temperature and cold rolling is compound.One
As hot (temperature) rolling compound is suitable for small mount, multi items, block formula method produces；Cold rolling is compound to be suitable for high-volume, coiled serialization
Production.In addition, foreign countries also develop non-isothermal rolling in the recent period, it is divided into that symmetric rolling is compound and asymmetrical rolling by top and bottom rolls condition
Compound, wherein asymmetrical rolling is compound can be greatly lowered roll-force, improve composite quality and efficiency.But preparing lamellar composite
Interlamellar spacing during material, Thickness ratio are difficult to control, and the performance to be difficult to material is adjusted and controls.Hot pressed sintering
Method is staggeredly to be superimposed metal foil in a certain way, certain temperature is heated under conditions of vacuum, while by applying
Add certain pressure to bring it about reaction, be reacted to after a certain period of time, then is diffused annealing under certain temperature and pressure,
So that metal is reacted between layers and generates metallic bond.The intensity of key is by pressure, the type etc. of temperature, synthesis speed, alloy
The influence of factors.The easily prepared metal foil of this method, simple for process, production efficiency is high, and equipment manufacturing cost is cheap.Stratiform
Ni-Al, Ti-Al material are exactly to be prepared using this method.
The component of reinforced particulate mainly has SiC, Al2O3、SiO2With ceramic particles and the graphite particle such as TiC.Because
The aluminum matrix composite of SiC particles enhancing has many advantages, such as low-density, cheap, dimensionally stable, thus as preferably,
The most new structural material of future.SiC particles reinforced metal-base composites have low-density, low bulk, high heat conduction,
The excellent properties such as high elastic modulus, high rigidity, high rigidity have huge application in high-tech sectors such as aerospace, naval vessels
Foreground.
Invention content
The purpose of the present invention is to provide between a kind of SiC particulate of intensity that can increase substantially composite material enhancing metal
Compound base layer-shaped composite material Ti/Al3The preparation method of Ti.
The object of the present invention is achieved like this：
(1) it is Al powder 1% by SiC powder and mass percent that 100gAl powder, mass percent are Al powder 1%~3%
Stearic acid be milled in the ball mill it is uniformly mixed；(2) powder after ball milling is added in grinding tool and uses powder metallurgy
Method prepares SiC particulate reinforced aluminum matrix composites；(3) SiC particulate is enhanced into aluminum-base composite between 450 DEG C~500 DEG C
Material is rolled into after foil plate and is cut into identical size jointly with TC4 foils；(4) TC4 foils and SiC particulate are enhanced into aluminum-base composite
Materials arranged in alternating, while ensureing that upper and lower surface is TC4 foils；(5) it is then placed in vacuum hotpressing stove and carries out hot pressed sintering,
It is evacuated to 3 × 10 first-2Then Pa is gradually heated to 675 DEG C~680 DEG C, keep the temperature 4 hours, then is slowly increased to 750 DEG C of heat preservations
3 hours, SiC ceramic particle is added to Ti/Al3In Ti laminar composites.
The present invention can also include：
1, the actual conditions for being gradually heated to 675 DEG C~680 DEG C of processes are：First from room temperature under the pressure of 4MPa
660 DEG C are to slowly warm up to, is taken as 1h；Pressure is reduced to 2MPa, 30min is kept the temperature at 660 DEG C；After pressure is down to 0Mpa,
Temperature is risen to 680 DEG C from 660 DEG C, is taken as 20min.
2, the actual conditions for being slowly increased to 750 DEG C of processes are：Temperature rises to 730 DEG C, takes 30min, keeps the temperature 1h；It rises
Temperature takes 30min to 750 DEG C.
3, the concrete technology of the powder metallurgy process is：Used time 1h is warming up to 350 DEG C of heat preservation 1h, then heats to 620
Furnace cooling after DEG C heat preservation 2h, pressure remains at 35.5~40MPa.
4, SiC particulate reinforced aluminum matrix composites and TC4 foils thickness ratio are 1.8~2.4 times after rolling.
In order to further increase Ti/Al3The comprehensive mechanical property of Ti laminar composites, the present invention enhance SiC particulate
Ti/Al3The preparation method of Ti laminar composites is studied, and is solved using reinforcement particle not reaching for many years and is carried
High Ti/Al3SiC particulate is successfully introduced into Ti/Al by the problem in science of Ti laminar composite intensity by two-step process3Ti layers
In shape composite material, the mechanical index such as intensity, the plasticity of laminar composite are further increased, solve to prepare problem.The present invention
The advantages of be prepare SiC particulate enhancing Ti/Al3Ti laminar composites and Ti/Al3Ti laminar composites are compared to synthesis
Mechanical property higher, while compared with the preparation means of fiber reinforcement stratiform composite material, cost is lower, the synthesis mechanics of material
Performance is better.
Description of the drawings
Fig. 1 is SiC particulate enhancing Ti/Al3Ti laminar composite metallographs, analysis find zero defect.
Fig. 2 is SiC particulate enhancing Ti/Al3Ti laminar composite microcosmos area photos, analysis find SiC particulate success
Be introduced into laminar composite, and it is evenly dispersed in the intermediate layer.
Fig. 3 is SiC particulate enhancing Ti/Al3Ti laminar composite X ray diffracting spectrums.
Fig. 4 a are SiCp-Ti/Al3Compression stress-strain of Ti vertical stack directions in the case where strain rate is 0.001/s is bent
Line.Fig. 4 b are Ti/Al3The compressive stress strain curve of Ti vertical stack directions in the case where strain rate is 0.001/s.Analysis is found
Ti/Al after introducing SiC particulate3The intensity of Ti laminar composites significantly improves, and compression strength improves 215MPa or so, and material
The breaking strain of material is increased to 4.5% from 3.7%.
Specific implementation mode
The SiC-Ti/Al of the present invention3The novel processing step of Ti laminar composites includes：(1) 1000 mesh (13 μ are selected
M) SiC powder and TC4 alloy foils that the Al powder and 1000 mesh (13 μm) purity that purity is 99.7% are 99.9%；(2) claim
100gAl powder and mass percent are measured as the SiC powder of Al powder 1%~3%, the stearic acid that mass percent is Al powder 1% is added
As dispersant, ball milling is uniformly mixed to achieve the effect that in high energy ball mill；(3) grinding tool is added simultaneously in the powder after ball milling
SiC particulate reinforced aluminum matrix composites are prepared using PM technique, powder metallurgical technique is that 1h is warming up to 350 DEG C of heat preservations
1h, then heats to furnace cooling after 620 DEG C of heat preservation 2h, and 35.5~40MPa is remained at from heating initiation pressure；(4) exist
SiC particulate reinforced aluminum matrix composites are rolled into after foil plate between 450 DEG C~500 DEG C be cut into jointly with TC4 alloys it is identical
Size；Ultrasonic cleaning, ethyl alcohol leaching is used in combination in the oxidation film for removing SiC particulate reinforced aluminum matrix composites foil and TC4 foils surface
It is dry after bubble；(5) TC4 foils and SiC particulate reinforced aluminum matrix composites foil are staggered, while ensure that upper and lower surface is equal
For TC4 paillons, it is then placed in vacuum hotpressing stove and carries out hot pressed sintering, be evacuated to 3 × 10 first-2Then Pa is gradually heated
To 675 DEG C, 4 hours are kept the temperature, then is slowly increased to 750 DEG C and keeps the temperature 3 hours.It to keep applying different pressures in heating and insulating process
Power is to ensure that the composite material prepared has high consistency.SiC ceramic particle is successfully added to Ti/Al by this method3Ti
In laminar composite.
The optimal processing parameter of hot pressed sintering is：660 DEG C are to slowly warm up to from room temperature under the pressure of 4MPa first, the time
For 1h；It is also not up to the fusing point of aluminium at this time, but therefore aluminium gradually appears ruckbildung is reduced to 2MPa by pressure, at 660 DEG C
Heat preservation 30min makes temperature stablize while so that foil is come into full contact with and ensureing that titanium atom and aluminium atom are fully spread；From 660
680 DEG C, time 20min DEG C are warming up to, 4h is kept the temperature；Therefore pressure, which is down to 0MPa, prevents molten aluminum quilt for aluminium foil fusing during this
It squeezes out；Temperature rises to 730 DEG C, time 30min, keeps the temperature 1h；750 DEG C, time 30min are warming up to, 3h is kept the temperature；In this process
Middle heat preservation 1-2h or so pressure illustrates that Ti-Al solid-liquid reactions terminate solid thermal expansion and make in pressure when beginning to ramp up to 1MPa or so
It rises, pressure is risen into 2MPa at this time；Increase the interface bond strength of composite material and the consistency of composite material.
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now pass through specific embodiment
Technical scheme of the present invention is described in detail, embodiment is for illustrating the present invention, rather than limiting the invention, at this
Simple modifications are done to the present invention under the concept thereof of invention, belong to the scope of protection of present invention.
Step A：Electronic balance weighs the SiC particulate and pure Al powder (Al powder 100g, the quality point of SiC particulate of required quality
Number is 1~3wt.%), 1wt.% stearic acid is added in ball grinder as dispersant, planet is used under argon gas protective condition
Formula ball mill ball milling 3h makes SiC particulate be dispersed in pure Al powder.
Step B：The SiC particulate and Al powder that mixing is completed after dry 12h, are put into hot pressing grinding tool in vacuum drying chamber
In, it is prepared according to powder metallurgy optimised process.
Step C：The SiC particulate reinforced Al matrix composite surface for being pressed into block materials polishing is totally rolled using double roller
Machine rolls it.Rolling mill practice is implemented by best rolling mill practice：The roads 1-2 secondary control deformation rate is in 5% or so, 3-4 passages
Deformation rate is controlled in 10%-20% ranges, deformation rate is gradually increased at last in 20%-30% in the roads 5-6 secondary control deformation rate
When road finish to gauge, material deformation rate is determined by required plate thickness, keeps the temperature 20min between every time at 470 DEG C.
Step D：Required square is cut into the SiC particulate reinforced Al matrix composite foil after rolling using plate shearing machine
Size.It will be cleaned up after SiC/Al foils and the polishing of Ti foil sand for surface paper；Then it is used in ultrasonic cleaner and second is added
Alcohol cleans foil；Finally dry up drying for standby.
Step E：By the Ti foils and SiC particulate reinforced Al matrix composite foil stacked arrangement after drying, following table in guarantee
Face is Ti foils.It is put into vacuum sintering funace, is prepared using vacuum heating-press sintering optimised process.
Claims (5)
1. a kind of SiC particulate enhancing intermetallic compound base laminar composite Ti/Al3The preparation method of Ti, it is characterized in that：
(1) it is the hard of Al powder 1% by SiC powder and mass percent that 100gAl powder, mass percent are Al powder 1%~3%
Resin acid is milled to uniformly mixed in the ball mill；(2) powder after ball milling is added in grinding tool and uses powder metallurgy process
Prepare SiC particulate reinforced aluminum matrix composites；(3) by SiC particulate reinforced aluminum matrix composites between 450 DEG C~500 DEG C
It is rolled into after foil plate and is cut into identical size jointly with TC4 foils；(4) by TC4 foils and SiC particulate reinforced aluminum matrix composites
It is alternately arranged, while ensureing that upper and lower surface is TC4 foils；(5) it is then placed in vacuum hotpressing stove and carries out hot pressed sintering, first
It is evacuated to 3 × 10-2Pa, is then gradually heated to 675 DEG C~680 DEG C, keeps the temperature 4 hours, then to be slowly increased to 750 DEG C of heat preservations 3 small
When, SiC ceramic particle is added to Ti/Al3In Ti laminar composites.
2. SiC particulate enhancing intermetallic compound base laminar composite Ti/Al according to claim 13The preparation side of Ti
Method, it is characterized in that the actual conditions for being gradually heated to 675 DEG C~680 DEG C of processes are：First from room under the pressure of 4MPa
Temperature is to slowly warm up to 660 DEG C, takes as 1h；Pressure is reduced to 2MPa, 30min is kept the temperature at 660 DEG C；Pressure is down to 0Mpa
Afterwards, temperature is risen to 680 DEG C from 660 DEG C, taken as 20min.
3. SiC particulate enhancing intermetallic compound base laminar composite Ti/Al according to claim 23The preparation side of Ti
Method, it is characterized in that the actual conditions for being slowly increased to 750 DEG C of processes are：Temperature rises to 730 DEG C, takes 30min, keeps the temperature 1h；
750 DEG C are warming up to, 30min is taken.
4. SiC particulate enhancing intermetallic compound base laminar composite Ti/Al according to claim 33The preparation side of Ti
Method, it is characterized in that the concrete technology of the powder metallurgy process is：Used time 1h is warming up to 350 DEG C of heat preservation 1h, then heats to 620
Furnace cooling after DEG C heat preservation 2h, pressure remains at 35.5~40MPa.
5. SiC particulate enhancing intermetallic compound base laminar composite Ti/Al according to claim 43The preparation side of Ti
Method, it is characterized in that SiC particulate reinforced aluminum matrix composites and TC4 foils thickness ratio are 1.8~2.4 times after rolling.
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| CN107299301B (en) * | 2017-05-27 | 2020-01-14 | 黄永兰 | Continuous fiber anti-freezing aluminum-based composite material and preparation method thereof |
| CN109913678B (en) * | 2019-03-15 | 2020-10-30 | 武汉大学 | TiAl3Particle reinforced aluminum-based composite material and preparation method and application thereof |
| CN110227734B (en) * | 2019-05-14 | 2021-04-27 | 太原理工大学 | Method for improving Mg/Ti connection interface performance |
| CN110180913B (en) * | 2019-05-14 | 2020-10-23 | 太原理工大学 | Method for improving Mg/Al connection interface performance |
| CN111485141B (en) * | 2020-06-05 | 2021-12-14 | 天钛隆（天津）金属材料有限公司 | SiC particle reinforced aluminum titanium matrix composite material and preparation method thereof |
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| JPS6244507A (en) * | 1985-08-20 | 1987-02-26 | Toyo Kohan Co Ltd | Method for sintering and joining hard sintered alloy film to steel stock |
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