CN109913781A - A kind of preparation method of ultra-thin super modeling friable plate material - Google Patents
A kind of preparation method of ultra-thin super modeling friable plate material Download PDFInfo
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- CN109913781A CN109913781A CN201910307232.4A CN201910307232A CN109913781A CN 109913781 A CN109913781 A CN 109913781A CN 201910307232 A CN201910307232 A CN 201910307232A CN 109913781 A CN109913781 A CN 109913781A
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Abstract
A kind of preparation method of ultra-thin super modeling friable plate material, is related to the preparation method of friable plate material.The invention solves aerospace Ti3The problem that Al friable plate material is difficult to and mechanical property is poor.Method: one, element foil surface preparation；Two, element foil hot pressing connects；Three, element foil reaction heat treatment.The present invention passes through the relative thickness of control element foil, realizes ultra-thin super modeling Ti3Al layers of controlledly synthesis, preparation process is pollution-free, and oxygen content is low, and material is fine and close, fine microstructures, and simple production process is easy.The present invention prepares molding field for friable plate material.
Description
Technical field
The present invention relates to the preparation methods of friable plate material.
Background technique
Ti3It is excellent that Al intermetallic compound and its alloy have that low-density, specific strength specific modulus is high, creep-resistant property is excellent etc.
Point can satisfy aerospace and hypersonic vehicle to the dual requirements of performance raising and structural weight reduction, be a kind of great
The high-temperature structural material of development potentiality, and be expected to fill up the service temperature blank of high-temperature titanium alloy and nickel-base alloy.However,
Ti3The intrinsic long-range order atomic arrangement mode of Al intermetallic compound keeps the proliferation of its dislocation and reciprocation extremely tired
Difficulty, or even processing hardening and room temperature processing performance are lost substantially.Therefore, brittleness Ti3The controllable forming of Al, which has become, limits it
The bottleneck problem of industrial application.How Ti is being promoted3There are still skills for the controllable forming of realization plate on the basis of Al mechanical property
Art challenge.
Summary of the invention
The invention solves aerospace Ti3The problem that Al friable plate material is difficult to and mechanical property is poor, and mention
A kind of preparation method of ultra-thin super modeling friable plate material is supplied.
The preparation method of the ultra-thin super modeling friable plate material of one kind of the invention is to sequentially include the following steps:
One, element foil surface preparation.Respectively corroded pure Ti foil and pure Al foil to 50 using HF solution and NaOH solution ~
500 μm and 10 ~ 100 μm, successively it is cleaned by ultrasonic and dries in acetone and ethyl alcohol.For corrosion HF acid volumetric concentration be 3% ~
The mass concentration of 20%, NaOH corrosive liquid is 3% ~ 20%;
Two, element foil hot pressing connects.It is Ti by step 1 treated pure Ti foil and pure Al foil alternative stacked, outermost layer
Layer, is placed in hot pressing connects in vacuum sintering funace.Hot pressing temperature is 300 ~ 600 DEG C, applies the pressure of 30 ~ 100MPa and pressure maintaining
0.5~5h；
Three, element foil reaction heat treatment.The Ti-Al based composite material sheet material that step 2 is obtained is 10-3~10-1The vacuum of Pa
Low temperature/high temperature two-step thermal processing is carried out in environment.Control Low Temperature Heat Treatment temperature is 550 ~ 700 DEG C first, keeps the temperature 0.1 ~ 5h, then
900 ~ 1300 DEG C of progress high-temperature heat treatments are warming up to, the pressure and 0.5 ~ 5h of pressure maintaining of 20 ~ 40MPa are applied.Prepare stratiform knot
Structure Ti-Ti3Al composite board, wherein brittleness Ti3Al layers with a thickness of 6 ~ 15 μm, along its normal direction include 1 ~ 3
Ti3Al crystal grain.
The beneficial effects of the present invention are: (1) present invention by the thickness of control aluminium element foil, realizes ultra-thin super modeling
Ti3Al layers of controlledly synthesis；(2) high performance Ti may be implemented using the present invention3The near net of Al/Ti laminar composite plate at
Shape avoids the Direct Rolling deformation to brittleness Intermatallic Ti-Al compound；(3) present invention is annealed using vacuum reaction, synthesis
Material oxygen content it is low, pollution-free, material is fine and close, fine microstructures；(4) simple production process is easy, and reaction rate is fast, synthesis
Period is short.
Detailed description of the invention
Fig. 1 is the Ti of embodiment preparation3The metallographic microstructure of Al/Ti laminar composite plate.
Fig. 2 is the Ti of embodiment preparation3The electron backscatter diffraction photo of Al/Ti laminar composite plate.
Fig. 3 is the Ti of embodiment preparation3Al/Ti laminar composite plate is loaded onto micro- under 9% macro-strain in situ
See tissue.
Fig. 4 is the Ti of embodiment preparation3Al/Ti laminar composite plate is loaded onto situ under 2.5% macro-strain
Microstrain distribution map.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment 1: the preparation method of the ultra-thin super modeling friable plate material of one kind of present embodiment is according to the following steps
It carries out:
One, element foil surface preparation.Respectively corroded pure Ti foil and pure Al foil to 50 using HF solution and NaOH solution ~
500 μm and 10 ~ 100 μm, successively it is cleaned by ultrasonic and dries in acetone and ethyl alcohol.For corrosion HF acid volumetric concentration be 3% ~
The mass concentration of 20%, NaOH corrosive liquid is 3% ~ 20%;
Two, element foil hot pressing connects.It is Ti by step 1 treated pure Ti foil and pure Al foil alternative stacked, outermost layer
Layer, is placed in hot pressing connects in vacuum sintering funace.Hot pressing temperature is 300 ~ 600 DEG C, applies the pressure of 30 ~ 100MPa and pressure maintaining
0.5~5h；
Three, element foil reaction heat treatment.The Ti-Al based composite material sheet material that step 2 is obtained is 10-3~10-1The vacuum of Pa
Low temperature/high temperature two-step thermal processing is carried out in environment.Control Low Temperature Heat Treatment temperature is 550 ~ 700 DEG C first, keeps the temperature 0.1 ~ 5h, then
900 ~ 1300 DEG C of progress high-temperature heat treatments are warming up to, the pressure and 0.5 ~ 5h of pressure maintaining of 20 ~ 40MPa are applied.Prepare stratiform knot
Structure Ti-Ti3Al composite board, wherein brittleness Ti3Al layers with a thickness of 6 ~ 15 μm, along its normal direction include 1 ~ 3
Ti3Al crystal grain.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: at surface in step 1
The HF acid volumetric concentration of reason is 10%, and the mass concentration of NaOH solution is 10%.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: through chemistry in step 1
The thickness of pure Ti foil is reduced to 300 μm after corrosion, and the thickness of pure Al foil is reduced to 50 μm.Other and specific embodiment one or two
It is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: pure in step 2
The number of plies of Ti foil is 10 layers, and the number of plies of pure Al foil is 9 layers.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: being controlled in step 2
Hot pressing temperature processed is 500 DEG C, pressure 40MPa, soaking time 1h.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: low in step 3
Warming treatment temperature is 660 DEG C, keeps the temperature 0.5h, is then warming up to 700 DEG C of heat preservation 1h, vacuum degree 10-2Pa.Other and specific reality
It is identical to apply one of mode one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: high in step 3
Warming treatment temperature is 1100 DEG C, applies the pressure and pressure maintaining 3h of 30MPa, vacuum degree 10-2Pa.Other and specific embodiment
One of one to six is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: step 3 synthesizes
Ti3Brittleness Ti in Al/Ti laminar composite3Al layers with a thickness of 13 μm, along its normal direction include 2 Ti3Al crystal grain.
It is other identical as one of specific embodiment one to seven.
Beneficial effects of the present invention are verified using following embodiment:
A kind of preparation method of ultra-thin super modeling friable plate material of the present embodiment, is specifically prepared according to the following steps:
One, element foil surface preparation.Pure Ti foil and pure Al foil are corroded to 300 μm using HF solution and NaOH solution respectively
With 50 μm, be successively cleaned by ultrasonic and dry in acetone and ethyl alcohol.HF acid volumetric concentration for corrosion is 10%, NaOH corrosion
The mass concentration of liquid is 10%;
Two, element foil hot pressing connects.By step 1 treated pure Ti foil and pure Al foil alternative stacked, Ti based composites foil
The number of plies be 10 layers, the number of plies of pure Al foil is 9 layers, and outermost layer is Ti layers, is placed in hot pressing connects in vacuum sintering funace.
Hot pressing temperature is 500 DEG C, applies the pressure and pressure maintaining 1h of 40MPa；
Three, element foil reaction heat treatment.The Ti-Al based composite material sheet material that step 2 is obtained is 10-2The vacuum environment of Pa
Middle progress low temperature/high temperature two-step thermal processing.Control Low Temperature Heat Treatment temperature is 660 DEG C first, keeps the temperature 0.5h, is then warming up to
700 DEG C of heat preservation 1h.High-temperature heat treatment is the pressure and pressure maintaining 3h for carrying out at 1100 DEG C, while applying 30MPa.Prepare layer
Shape structure Ti-Ti3Al composite board, wherein brittleness Ti3Al layers with a thickness of 13 μm, along its normal direction include 2
Ti3Al crystal grain.
Ti manufactured in the present embodiment3The microstructure of Al/Ti laminar composite is as depicted in figs. 1 and 2.Brittleness Ti3Al layers
With a thickness of 13 μm, along its normal direction include 2 Ti3Al crystal grain.In situ under tensile stress load, the ultra-thin Ti of brittleness3Al layers
It can be plastically deformed, or even not crack (Fig. 3) yet when macro-strain reaches 9%.Utilize the digitized map based on scanning electron microscope
As correlation technology, Ti observed3Plastic Flow behavior (Fig. 4) at Al layers.With casting homogeneous Ti3Al is compared, and of the invention is super
Bao Chao moulds Ti3Al shows unusual plastic deformation ability while keeping higher-strength.
Claims (8)
1. a kind of preparation method of ultra-thin super modeling friable plate material, it is characterised in that the Ti of layer structure3Al/Ti composite board
Preparation method be prepared according to the following steps:
One, the surface preparation of element foil uses HF solution and NaOH solution to corrode pure Ti foil and pure Al foil to 50 ~ 500 respectively
μm and 10 ~ 100 μm, be successively cleaned by ultrasonic and dry in acetone and ethyl alcohol, for corrosion HF acid volumetric concentration be 3% ~ 20%,
The mass concentration of NaOH corrosive liquid is 3% ~ 20%;
Two, element foil hot pressing connects: being Ti by step 1 treated pure Ti foil and pure Al foil alternative stacked, outermost layer
Layer is placed in hot pressing connects in vacuum sintering funace, and hot pressing temperature is 300 ~ 600 DEG C, applies the pressure of 30 ~ 100MPa and pressure maintaining
0.5~5h；
Three, element foil reaction heat treatment: the Ti-Al based composite material sheet material that step 2 is obtained is 10-3~10-1The vacuum of Pa
Low temperature/high temperature two-step thermal processing is carried out in environment, control Low Temperature Heat Treatment temperature is 550 ~ 700 DEG C first, 0.1 ~ 5h is kept the temperature, then
900 ~ 1300 DEG C of progress high-temperature heat treatments are warming up to, applies the pressure and 0.5 ~ 5h of pressure maintaining of 20 ~ 40MPa, that is, prepares stratiform knot
Structure Ti-Ti3Al composite board, wherein brittleness Ti3Al layers with a thickness of 6 ~ 15 μm, along its normal direction include 1 ~ 3
Ti3Al crystal grain.
2. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that used in step 1
It is 10% in the HF acid volumetric concentration of surface treatment, the mass concentration of NaOH solution is 10%.
3. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that passed through in step 1
The thickness of pure Ti foil is reduced to 300 μm after chemical attack, and the thickness of pure Al foil is reduced to 50 μm.
4. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that pure in step 2
The number of plies of Ti foil is 10 layers, and the number of plies of pure Al foil is 9 layers.
5. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that controlled in step 2
Hot pressing temperature processed is 500 DEG C, pressure 40MPa, soaking time 1h.
6. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that low in step 3
Warming treatment temperature is 660 DEG C, keeps the temperature 0.5h, is then warming up to 700 DEG C of heat preservation 1h, vacuum degree 10-2Pa。
7. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that high in step 3
Warming treatment temperature is 1100 DEG C, applies the pressure and pressure maintaining 3h of 30MPa, vacuum degree 10-2Pa。
8. the preparation method of the ultra-thin super modeling friable plate material of one kind according to claim 1, it is characterised in that step 3 synthesis
Ti3Brittleness Ti in Al/Ti laminar composite3Al layers with a thickness of 13 μm, along its normal direction include 2 Ti3Al crystal grain.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110978721A (en) * | 2019-12-18 | 2020-04-10 | 哈尔滨工程大学 | Method for controlling defects and cracking of FeAl intermetallic compound layered composite material |
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2019
- 2019-04-17 CN CN201910307232.4A patent/CN109913781A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110978721A (en) * | 2019-12-18 | 2020-04-10 | 哈尔滨工程大学 | Method for controlling defects and cracking of FeAl intermetallic compound layered composite material |
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