CN112620488A - Ti3Al laminated composite board and preparation method thereof - Google Patents

Ti3Al laminated composite board and preparation method thereof Download PDF

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Publication number
CN112620488A
CN112620488A CN202011487971.5A CN202011487971A CN112620488A CN 112620488 A CN112620488 A CN 112620488A CN 202011487971 A CN202011487971 A CN 202011487971A CN 112620488 A CN112620488 A CN 112620488A
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alloy foil
temperature
composite board
pressure
alloy
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Inventor
张桐桐
付杰
吴明
杜军旗
何永胜
王凯旋
赵小花
孙峰
刘向宏
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Western Superconducting Technologies Co Ltd
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Western Superconducting Technologies Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21DWORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D33/00Special measures in connection with working metal foils, e.g. gold foils
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21DWORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D39/00Application of procedures in order to connect objects or parts, e.g. coating with sheet metal otherwise than by plating; Tube expanders
    • B21D39/03Application of procedures in order to connect objects or parts, e.g. coating with sheet metal otherwise than by plating; Tube expanders of sheet metal otherwise than by folding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/043Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)

Abstract

The invention discloses a Ti3Al layered composite sheet, Ti3The Al laminated composite sheet comprises Ti3Al matrix presents the layered distribution characteristic of alternately arranged fine grains and coarse grains, and in-situ autogenous Ti5Si3The particle reinforcement also exhibits a lamellar distribution characteristic, said Ti5Si3The volume fraction of the particle reinforcement in the layered composite board is 2.4-9.6%, the invention also discloses Ti3The preparation method of the Al laminated composite board comprises the following steps: firstly, carrying out surface pretreatment on TC4 alloy foil and Al-Si alloy foil; II,Alternately stacking TC4 alloy foils and Al-Si alloy foils for hot-press connection; thirdly, carrying out low-temperature reaction annealing on the multilayer composite board; fourthly, the multilayer composite board is continuously subjected to high-temperature reaction annealing. The invention realizes high-performance Ti3Controllable preparation of Al-layered composite sheet, Ti3The Al layered composite sheet exhibits excellent strength and plastic matching.

Description

Ti3Al laminated composite board and preparation method thereof
Technical Field
The invention belongs to the field of preparation and utilization of alloy materials, and particularly relates to Ti3An Al laminated composite board and a preparation method thereof.
Background
Ti3The Al alloy has the advantages of low density, high specific modulus and specific strength, good creep resistance and the like, and is considered to be a light high-temperature structural material with potential application prospect in the fields of aerospace and the like. However, Ti3The poor room temperature plasticity of Al alloy causes the difficulty in forming and preparing the widely applied plates. Further, Ti3The problem of insufficient high-temperature strength of the Al alloy also seriously hinders the industrial application of the Al alloy. How to increase Ti3The technical problem of realizing the sheet forming preparation while the high-temperature performance of Al is still the technical problem, namely Ti3The key to practical use of Al. In recent years, researchers at home and abroad use Ti in a composite mode3The introduction of Al alloy into the reinforcement increases Ti to a certain extent3High temperature mechanical property of Al alloy. In addition, a great deal of research shows that the structural design (gradient, lamellar, reticular and the like) of the metal structural material can effectively improve the comprehensive mechanical property of the material, and also provides reference and reference for the design of the brittle material. Therefore, the compound and the tissue configuration are combinedThe combination of design and preparation process enables high-performance Ti3The forming preparation of the Al composite sheet becomes possible.
Disclosure of Invention
The object of the present invention is to provide a Ti3Al laminated composite sheet and its preparing process3The Al thin plate is difficult to form and prepare and has insufficient high-temperature strength.
The technical scheme adopted by the invention is as follows:
ti3Al layered composite plate of, wherein, Ti3The Al matrix is Ti in which fine grains and coarse grains are alternately arranged and distributed in a layered manner and are autogenous in situ5Si3The particle reinforcement is also distributed in layers, and the Ti is5Si3The volume fraction of the particle reinforcement in the layered composite board is 2.4-9.6%.
Ti3The preparation method of the Al laminated composite sheet comprises the following steps:
cleaning a TC4 alloy foil and an Al-Si alloy foil with the Si content of 2-8 wt.% in an HF solution and an NaOH solution respectively to obtain a TC4 alloy foil with the thickness of 70-95 mu m and an Al-Si alloy foil with the thickness of 20-40 mu m, ultrasonically cleaning in absolute ethyl alcohol for 2-5 min respectively, and drying; the thickness is adjusted to shorten the reaction annealing time, simplify the preparation process and be beneficial to thinning Ti3The grain size of the Al laminated composite sheet improves the mechanical property.
Step two, taking 15-20 layers of the TC4 alloy foil and 14-19 layers of the Al-Si alloy foil obtained in the step one, alternately laminating the two alloy foils, placing the two alloy foils in a vacuum hot pressing furnace, and placing the two alloy foils in a vacuum hot pressing furnace at 10 DEG C-3~10-1The pressure is applied to 35-50 MPa under the Pa vacuum condition and at the temperature of 510-550 ℃, and the pressure is maintained for 1-2 h; this parameter makes the thermocompression bonding between the TC4 alloy foil and the Al — Si alloy foil tighter.
Step three, the multilayer composite thin plate obtained in the step two is arranged at 10-3~10-1Carrying out low-temperature reaction annealing for 1-5 h under the vacuum condition of Pa and the non-pressure condition of 600-680 ℃; the TC4 alloy foil and the Al-Si alloy foil are subjected to solid-liquid reaction, so that the reaction annealing time is greatly shortened, and meanwhile, the reaction annealing time is greatly shortenedThe composition deviation of the laminated composite sheet caused by Al liquid loss due to overhigh temperature is avoided.
Step four, the multilayer composite thin plate obtained in the step three is arranged at 10-3~10-1Carrying out high-temperature reaction annealing for 1-4 h under the conditions that the temperature is 1250-1400 ℃ and the applied pressure is 45-50 MPa under the vacuum condition of Pa, then cooling along with the furnace, and removing the pressure when the furnace temperature is reduced to be below 800-1000 ℃, thus preparing the Ti3An Al laminated composite board. By utilizing the pressure and the temperature, the holes can be effectively closed, so that the laminated composite board is more densified.
Further, the Al-Si alloy foil described in step one has a Si content of 6 wt.%.
Furthermore, the thickness of the TC4 alloy foil in the first step is 80 μm, and the thickness of the Al-Si alloy foil is 30 μm.
And furthermore, the number of layers of the TC4 alloy foil in the step two is 16, the number of layers of the Al-Si alloy foil is 15, the number of layers of the TC4 alloy foil is one more than that of the Al-Si alloy foil, and both outermost sides of the TC4 alloy foil are TC4 alloy foils.
Further, in step two, the reaction temperature is 4 multiplied by 10-2And under the Pa vacuum condition, the hot pressing temperature is 520 ℃, the pressure is 50MPa, and the pressure maintaining time is 1 h.
Further, in the third step, the low-temperature reaction annealing temperature is 680 ℃, the temperature is kept for 1h under no pressure, and the vacuum degree is 4 multiplied by 10-2Pa。
Further, the high temperature reaction annealing temperature in the fourth step is 1250 ℃, the heat preservation is carried out for 1h under the condition of applying 50MPa pressure, and the vacuum degree is 2 multiplied by 10-2Pa, and releasing the pressure when the furnace temperature is reduced to below 1000 ℃.
The invention has the beneficial effects that:
1. the invention adopts TC4 alloy foil and Al-Si alloy foil as raw materials, and realizes that the matrix presents Ti with fine grains and coarse grains which are alternately arranged by adjusting the reaction annealing process3And (3) controllably preparing the Al laminated composite board. Due to Ti3The Al laminated composite board has the performance advantages of both fine crystal material and coarse crystal material, and in-situ synthesized Ti5Si3The particles are refined by Ti3Al matrix, increased Ti3Mechanical properties of Al laminated composite board andthe temperature is used.
2. Ti can be realized by adjusting the thickness of the raw material foil and the Si content in the Al-Si alloy foil3Controllable preparation of the thickness of the Al laminated composite plate, the thickness of a coarse crystal layer and a fine crystal layer and the content of the reinforcement. Because Si is in TiAl3The solid solubility (13.6-15 at.%) in Ti is far higher than that in Ti3Solid solubility (2.3 at.%) in Al, and Si is gradually dissolved in TiAl after low-temp reaction annealing3Then along with the TiAl matrix during high-temperature reaction annealing3Conversion to Ti3Precipitation of Ti with Al5Si3Therefore, the in-situ autogenous Ti can be prepared by adjusting the holding time of the low-temperature reaction annealing5Si3And (4) regulating and controlling the spatial distribution of the particles.
3. The invention can realize high-performance Ti3The near-net-shape preparation of the Al laminated composite board avoids the brittle intermetallic compound Ti3The processing deformation of forging, rolling and the like of Al is simple and easy to operate.
Drawings
FIG. 1 shows Ti prepared in example 1 of the present invention3Electron back scattering diffraction pattern of Al layered composite plate.
FIG. 2 shows Ti prepared in example 1 of the present invention3Scanning electron microscope image of the Al layered composite panel, a: fine crystal grain Ti3Al matrix and more Ti5Si3Particles, B: coarse grain Ti3Al matrix and small amount of Ti5Si3And (3) granules.
Detailed Description
The technical solution of the present invention is further described in detail by examples below.
Example 1
Ti3The preparation method of the Al laminated composite board comprises the following steps:
cleaning a TC4 alloy foil and an Al-Si alloy foil with the Si content of 6 wt.% in an HF solution and an NaOH solution respectively to obtain a TC4 alloy foil with the thickness of 80 mu m and an Al-Si alloy foil with the thickness of 30 mu m respectively, and then ultrasonically cleaning in absolute ethyl alcohol for 5min and drying;
secondly, the 16-layer TC4 alloy foil obtained in the step one and 15 layers of Al-Si alloy are mixedThe gold foils were alternately stacked and placed in a vacuum autoclave at 4X 10-2Carrying out pressure maintaining treatment for 1h under the conditions of Pa vacuum, hot pressing temperature of 520 ℃ and applied pressure of 50 MPa;
thirdly, the multilayer composite board obtained in the second step is processed at 4 multiplied by 10-2Carrying out low-temperature reaction annealing for 1h under the vacuum condition of Pa and the non-pressure condition of 680 ℃;
fourthly, the multilayer composite board obtained in the third step is processed at 2 multiplied by 10-2Carrying out high-temperature reaction annealing for 1h under the conditions that the temperature is 1250 ℃ and the applied pressure is 50MPa under the vacuum condition of Pa, then cooling along with the furnace, and unloading the pressure when the furnace temperature is reduced to below 1000 ℃, thus preparing the Ti3An Al laminated composite board. Wherein Ti3The Al laminated composite board matrix presents the laminated distribution characteristic of alternately arranged fine grains and coarse grains, and in-situ self-generated Ti5Si3The particle reinforcement also exhibits a lamellar distribution characteristic.
Ti of the example3Al layered composite sheet, Ti3Al matrix presents the layered distribution characteristic of alternately arranged fine grains and coarse grains, and in-situ autogenous Ti5Si3The grain reinforcement also exhibits a lamellar distribution characteristic, i.e. in fine-grained Ti3More distribution on Al matrix and coarse grain Ti3Relatively less scattered distribution on the Al matrix, the Ti5Si3The volume fraction of the particle reinforcement in the layered composite panel was 7.2%.
Example 2
The difference from example 1 is that the Si content is 2 wt.%, Ti5Si3The volume fraction of the particle reinforcement in the layered composite plate is 2.4%, and the rest is the same.
Example 3
The difference from example 1 is that the Si content is 8 wt.%, Ti5Si3The volume fraction of the particle reinforcement in the layered composite plate is 9.6%, and the rest is the same.
Example 4
The difference from example 1 is that the thickness of the TC4 alloy foil in the first step is 70 μm, the thickness of the Al-Si alloy foil is 20 μm, and the rest is the same.
Example 5
The difference from example 1 is that the thickness of the TC4 alloy foil in the first step is 95 μm, the thickness of the Al-Si alloy foil is 40 μm, and the rest is the same.
Example 6
The difference from example 1 is that the number of layers of the TC4 alloy foil in the second step is 20, the number of layers of the Al-Si alloy foil is 19, the TC4 alloy foil is one more layer than the Al-Si alloy foil, and the TC4 alloy foil is provided on both outermost sides. The rest is the same.
Example 7
The difference from the example 1 is that 10 is the difference in the second step-3And (3) under the Pa vacuum condition, the hot pressing temperature is 530 ℃, the pressure is 35MPa, and the pressure maintaining time is 2 h. The rest is the same.
Example 8
The difference from the embodiment 1 is that the low temperature reaction annealing temperature in the third step is 600 ℃, the temperature is not pressure and is kept for 5 hours, and the vacuum degree is 4 multiplied by 10-2Pa. The rest is the same.
Example 9
The difference from the embodiment 1 is that the high temperature reaction annealing temperature in the fourth step is 1400 ℃, the temperature is kept for 3 hours under the condition of applying the pressure of 45MPa, and the vacuum degree is 10-3Pa, and releasing the pressure when the furnace temperature is reduced to below 1000 ℃. The rest is the same.
Ti prepared in example 13The microstructure morphology of the Al laminated composite plate is shown in FIGS. 1 and 2. Ti3The Al laminated composite plate has compact structure without holes, and the matrix has the characteristic of laminated distribution of alternately arranged fine grains and coarse grains, wherein the coarse grains have the thickness of about 78 microns, the grains have the size of about 53 microns, the fine grains have the thickness of about 38 microns, the grains have the size of about 11 microns, and in-situ self-generated Ti5Si3The particle reinforcement also presents a layered distribution characteristic, and effectively refines the crystal grains of the matrix. Ti3The Al laminated composite board has the performance advantages of both fine-grained material and coarse-grained material, the tensile strength at 700 ℃ reaches more than 500MPa, the elongation reaches more than 10 percent, and compared with the blocky Ti prepared by a casting method3Al alloy, Ti prepared by the invention3The Al layered composite panel exhibits excellent high temperature mechanical properties.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (8)

1. Ti3Al layered composite sheet, characterized in that Ti3The Al matrix is Ti in which fine grains and coarse grains are alternately arranged and distributed in a layered manner and are autogenous in situ5Si3The particle reinforcement is also distributed in layers, and the Ti is5Si3The volume fraction of the particle reinforcement in the layered composite board is 2.4-9.6%.
2. Ti3The preparation method of the Al layered composite board is characterized by comprising the following steps:
cleaning a TC4 alloy foil and an Al-Si alloy foil with the Si content of 2-8 wt.% in an HF solution and an NaOH solution respectively to obtain a TC4 alloy foil with the thickness of 70-95 mu m and an Al-Si alloy foil with the thickness of 20-40 mu m, ultrasonically cleaning in absolute ethyl alcohol for 2-5 min respectively, and drying;
step two, taking 15-20 layers of the TC4 alloy foil and 14-19 layers of the Al-Si alloy foil obtained in the step one, alternately laminating the two alloy foils, placing the two alloy foils in a vacuum hot pressing furnace, and placing the two alloy foils in a vacuum hot pressing furnace at 10 DEG C-3~10-1The pressure is applied to 35-50 MPa under the Pa vacuum condition and at the temperature of 510-550 ℃, and the pressure is maintained for 1-2 h;
step three, the multilayer composite thin plate obtained in the step two is arranged at 10-3~10-1Carrying out low-temperature reaction annealing for 1-5 h under the vacuum condition of Pa and the non-pressure condition of 600-680 ℃;
step four, the multilayer composite thin plate obtained in the step three is arranged at 10-3~10-1Carrying out high-temperature reaction annealing for 1-4 h under the conditions that the temperature is 1250-1400 ℃ and the applied pressure is 45-50 MPa under the vacuum condition of Pa, then cooling along with the furnace, and reducing the furnace temperature to 800-1Removing pressure at a temperature of less than 000 ℃ to prepare Ti3An Al laminated composite board.
3. A Ti according to claim 23The preparation method of the Al laminated composite plate is characterized in that the Si content of the Al-Si alloy foil in the step one is 6 wt.%.
4. A Ti according to claim 23The preparation method of the Al laminated composite board is characterized in that the thickness of the TC4 alloy foil in the step one is 80 μm, and the thickness of the Al-Si alloy foil is 30 μm.
5. A Ti according to claim 23The preparation method of the Al layered composite plate is characterized in that the number of layers of the TC4 alloy foil in the step two is 16, the number of layers of the Al-Si alloy foil is 15, the number of layers of the TC4 alloy foil is one more than that of the Al-Si alloy foil, and both outermost sides of the TC4 alloy foil are TC4 alloy foils.
6. A Ti according to claim 23The preparation method of the Al laminated composite board is characterized in that in the second step, the thickness of the Al laminated composite board is 4 multiplied by 10-2And under the Pa vacuum condition, the hot pressing temperature is 520 ℃, the pressure is 50MPa, and the pressure maintaining time is 1 h.
7. A Ti according to claim 23The preparation method of the Al laminated composite board is characterized in that in the third step, the low-temperature reaction annealing temperature is 680 ℃, the temperature is kept for 1h under no pressure, and the vacuum degree is 4 multiplied by 10-2Pa。
8. A Ti according to claim 23The preparation method of the Al laminated composite board is characterized in that the high-temperature reaction annealing temperature in the fourth step is 1250 ℃, the heat preservation is carried out for 1h under the condition of applying 50MPa pressure, and the vacuum degree is 2 multiplied by 10-2Pa, and releasing the pressure when the furnace temperature is reduced to below 1000 ℃.
CN202011487971.5A 2020-12-16 2020-12-16 Ti3Al laminated composite board and preparation method thereof Pending CN112620488A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02101133A (en) * 1988-10-05 1990-04-12 Daido Steel Co Ltd Ti3al/tial composite material
JPH0437658A (en) * 1990-05-29 1992-02-07 Nhk Spring Co Ltd Combined material and its production
JPH0569158A (en) * 1991-09-13 1993-03-23 Nhk Spring Co Ltd Manufacture of complex material composed of intermetallic compound in at least a part
CN102744928A (en) * 2012-07-25 2012-10-24 哈尔滨工业大学 Preparation method for Ti3Al-TiAl laminated composite material
CN103057203A (en) * 2013-01-24 2013-04-24 哈尔滨工业大学 Laminated NiAl material and preparation method thereof
CN103805810A (en) * 2012-11-09 2014-05-21 北京航空航天大学 Titanium-aluminum alloy material and making method thereof
US20150086414A1 (en) * 2013-09-20 2015-03-26 MTU Aero Engines AG CREEP-RESISTANT TiAl ALLOY
CN106271011A (en) * 2016-09-12 2017-01-04 西北工业大学 γ TiAl alloy and the solid-state bonding process of TC17 alloy
CN111421218A (en) * 2020-04-28 2020-07-17 上海交通大学 Hydrogen-containing Ti2Low-temperature diffusion welding method for AlNb-based alloy and TC4 titanium alloy

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02101133A (en) * 1988-10-05 1990-04-12 Daido Steel Co Ltd Ti3al/tial composite material
JPH0437658A (en) * 1990-05-29 1992-02-07 Nhk Spring Co Ltd Combined material and its production
JPH0569158A (en) * 1991-09-13 1993-03-23 Nhk Spring Co Ltd Manufacture of complex material composed of intermetallic compound in at least a part
CN102744928A (en) * 2012-07-25 2012-10-24 哈尔滨工业大学 Preparation method for Ti3Al-TiAl laminated composite material
CN103805810A (en) * 2012-11-09 2014-05-21 北京航空航天大学 Titanium-aluminum alloy material and making method thereof
CN103057203A (en) * 2013-01-24 2013-04-24 哈尔滨工业大学 Laminated NiAl material and preparation method thereof
US20150086414A1 (en) * 2013-09-20 2015-03-26 MTU Aero Engines AG CREEP-RESISTANT TiAl ALLOY
CN106271011A (en) * 2016-09-12 2017-01-04 西北工业大学 γ TiAl alloy and the solid-state bonding process of TC17 alloy
CN111421218A (en) * 2020-04-28 2020-07-17 上海交通大学 Hydrogen-containing Ti2Low-temperature diffusion welding method for AlNb-based alloy and TC4 titanium alloy

Non-Patent Citations (1)

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Title
张桐桐: "(Ti5Si3-TiAl)/TiAl 层状复合板组织形成机制与高温力学及抗氧化行为", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *

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Application publication date: 20210409