CN113862587A - In-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material and preparation method thereof - Google Patents
In-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material and preparation method thereof Download PDFInfo
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- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 26
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 21
- 229910009594 Ti2AlN Inorganic materials 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000003014 reinforcing effect Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- 238000002490 spark plasma sintering Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000005245 sintering Methods 0.000 abstract description 16
- 125000004429 atom Chemical group 0.000 abstract description 11
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 6
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 150000004767 nitrides Chemical class 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- 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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- B22—CASTING; POWDER METALLURGY
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses an in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material and a preparation method thereof, wherein BN is used as a B source and an N source for synthesizing TiB2 and Ti2AlN, BN and TiAl alloy powder in a certain proportion are subjected to mechanical ball milling and mixing, then the mixed powder is subjected to discharge plasma sintering, and the dual-phase dual-scale synergistically enhanced TiAl-based composite material is obtained after cooling. The invention utilizes different diffusion paths of B atoms and N atoms in a matrix alloy to prepare the dual-phase dual-scale synergistically enhanced TiAl-based composite material. In the discharge plasma sintering process, B atoms mainly diffuse in grain boundaries and finally form TiB2 whiskers in the grain boundaries, while N atoms mainly diffuse along alpha 2/gamma laths, are dissolved in the gap positions of alpha phases and gamma phases, are cooled to form nano-scale nitride Ti2AlN, and are uniformly precipitated. The invention realizes the introduction of a dual-phase dual-scale second phase into the TiAl-based composite material, and can effectively improve the performance of the TiAl-based composite material.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to an in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material and a preparation method thereof.
Background
The TiAl-based alloy is one of novel high-temperature materials and has excellent properties of high specific strength, light weight, high temperature resistance and the like. Compared with titanium alloy and nickel-based alloy, TiAl-based alloy has greater superiority, can well meet the rapid development requirement of aviation industry, and is receiving more and more attention of domestic and foreign researchers. However, the inherent defects of poor room temperature plasticity, insufficient high temperature strength above 800 ℃, insufficient oxidation resistance and the like of the TiAl-based alloy severely limit the application of the TiAl-based alloy in engineering. Therefore, a large amount of research is carried out by scholars at home and abroad, the TiAl-based composite material containing various reinforcing phases is prepared mainly by utilizing a composite technology, and a plurality of excellent properties of the TiAl-based alloy are maintained, and meanwhile, some advantages of the reinforcing phases are maintained. The TiAl-based composite material with excellent comprehensive performance is obtained by reinforcing the TiAl-based alloy by using continuous fiber reinforcement or discontinuous short fibers, whiskers and particles through a composite material technology, and becomes a main trend of the development of the TiAl-based alloy.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for in-situ double-phase double-scale synergistic enhancement of a TiAl-based composite material aiming at the defects of the prior art. The method utilizes different diffusion paths of B atoms and N atoms in a matrix alloy to prepare the dual-phase dual-scale synergistically enhanced TiAl-based composite material. In the discharge plasma sintering process, B atoms mainly diffuse in grain boundaries and finally form TiB2 whiskers in the grain boundaries, while N atoms mainly diffuse along alpha 2/gamma laths, are dissolved in the gap positions of alpha phases and gamma phases, are cooled to form nano-scale nitride Ti2AlN, and are uniformly precipitated. The invention realizes the introduction of a dual-phase dual-scale second phase into the TiAl-based composite material, and can effectively improve the performance of the TiAl-based composite material.
In order to solve the technical problems, the invention adopts the technical scheme that:
in a first aspect, the invention provides a preparation method of an in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material, which comprises the following steps: mixing BN and TiAl alloy powder in proportion, performing mechanical ball milling mixing to obtain mixed powder, then performing spark plasma sintering on the mixed powder, and cooling to obtain the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material.
Preferably, the TiAl alloy powder comprises the following components in percentage by atom: 44-48%; nb: 2-8%; cr: 0-2%; v: 0 to 3 percent; mo: 0-2% and the balance Ti.
Preferably, the mixed powder contains 0.1 to 1 wt% of BN.
Preferably, the discharge plasma sintering temperature is 1250-1350 ℃, the heat preservation time is 5-10 min, and the pressure is 30-45 MPa.
Preferably, in the mechanical ball milling process, the ball-to-material ratio is 3: 1.
In a second aspect, the invention provides an in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material obtained by the preparation method according to any one of the first aspect, the composite material is of a full-lamellar structure, micrometer-scale TiB2 whiskers are distributed on a crystal boundary between lamellar clusters, and nanometer-scale Ti2AlN enhanced phases are distributed at alpha 2/gamma lath gaps formed by alpha 2 phases and gamma phases.
Preferably, the size of the TiB2 crystal whisker is 10-20 μm.
Preferably, the Ti2AlN reinforcing phase has a size of 100 to 200 nm. Compared with the prior art, the invention has the following advantages:
1. the invention utilizes different diffusion paths of B atoms and N atoms in BN nanosheets in the TiAl matrix alloy to prepare the dual-phase dual-scale synergistically enhanced TiAl-based composite material. In the discharge plasma sintering process, B atoms mainly diffuse in grain boundaries and finally form TiB2 whiskers in the grain boundaries, while N atoms mainly diffuse along alpha 2/gamma laths, are dissolved in the gap positions of alpha phases and gamma phases, are cooled to form nano-scale nitride Ti2AlN, and are uniformly precipitated. The invention realizes the introduction of a dual-phase dual-scale second phase into the TiAl-based composite material, and can effectively improve the performance of the TiAl-based composite material.
2. The method utilizes the discharge plasma sintering method to simultaneously precipitate the dual-phase dual-scale second phase at the crystal boundary of the TiAl-based composite material and between the alpha 2/gamma laths in situ, can effectively prevent O atoms from diffusing into the material through the crystal boundary and the gaps of the alpha 2/gamma laths at high temperature, reduces the high-temperature oxidation of the TiAl-based composite material, and prolongs the service life of the composite material.
3. The method can adjust the generation quantity and distribution of the TiB2 and the Ti2AlN by controlling the addition amount of BN and the sintering parameters, is flexible, convenient, simple and effective, has simple operation in the whole process, is easy to implement, and improves the application value of the method.
Drawings
FIG. 1 is an SEM image (200X) of a dual-phase dual-scale synergistically reinforced TiAl-based composite material prepared in example 1 of the present invention, in which Lamelale represents a lamellar layer.
FIG. 2 is an SEM image (2000X) of a dual-phase dual-scale synergistically reinforced TiAl-based composite prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
The invention provides a preparation method of an in-situ two-phase dual-scale synergistically enhanced TiAl-based composite material, which comprises the steps of taking BN as a B source and an N source for synthesizing TiB2 and Ti2AlN, carrying out mechanical ball milling and mixing on BN and TiAl alloy powder in a certain proportion to obtain mixed powder, then carrying out discharge plasma sintering on the mixed powder, and cooling to obtain the in-situ two-phase dual-scale synergistically enhanced TiAl-based composite material.
In the preparation process, by utilizing the diffusion characteristics of two atoms in BN in TiAl alloy and the characteristics of rapid heating and cooling, high densification degree, easily controlled process and the like of spark plasma sintering, B atoms are mainly diffused along grain boundaries at high temperature and are agglomerated at the grain boundaries to finally form micron-sized TiB2 pinned at the grain boundaries; n atoms mainly diffuse along the alpha 2/gamma lath, are dissolved in the gap position of the alpha phase and the gamma phase, and finally are cooled to separate out the nano-scale nitride Ti2 AlN. Therefore, the invention finally prepares the TiAl-based composite material synergistically enhanced by the micron-sized TiB2 pinned at the grain boundary and the nano-sized Ti2AlN dispersedly distributed in the alpha 2/gamma lath, and provides a new idea for the development and application of the TiAl-based composite material.
The TiAl alloy powder comprises the following components in percentage by atom: 44-48%; nb: 2-8%; cr: 0-2%; v: 0 to 3 percent; mo: 0-2% and the balance Ti. The specific TiAl alloy components can be optimized and adjusted according to the actual situation. The TiAl alloy composition is regulated, so that the alloy structure can be optimized, the composition of a second phase and a substrate is facilitated, and the TiAl-based composite material with excellent performance is obtained.
The mass fraction of the BN nanosheets in the mixed powder is 0.1-1 wt%, so that the problems that the precipitated phase is too small and uneven due to too small content and the precipitated phase is agglomerated due to the fact that the content is too large and the powder is not uniformly mixed are avoided. In the range, the content of TiB2 and Ti2AlN increases along with the increase of the mass fraction of the BN nano-sheet, so that the content of TiB2 and Ti2AlN can be regulated and controlled by controlling the mass fraction of BN in the mixed powder, and the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material with excellent performance is obtained.
In the discharge plasma sintering process, the sintering temperature is 1250-1350 ℃, the heat preservation time is 5-10 min, and the sintering pressure is 30-45 MPa. By regulating and controlling sintering parameters, abnormal growth of precipitated phase grains is avoided, a fine and dispersedly distributed dual-phase dual-scale synergistically enhanced TiAl-based composite material is obtained, and the performance of the TiAl-based composite material is further improved.
The in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material prepared by the method is of a full-lamellar structure, TiB2 whiskers are distributed at a crystal boundary, and the size of the TiB2 whiskers is usually 10-20 microns; the alpha 2/gamma lath is dispersed with nanometer Ti2AlN particles, and the size of the nanometer Ti2AlN particles is usually 100-200 nm. The two reinforcing phases have a reinforcing effect on the TiAl-based composite material, wherein TiB2 whiskers at a grain boundary prevent grains from deforming to achieve the reinforcing purpose through the pinning effect on the grain boundary, the nano-scale Ti2AlN in the alpha 2/gamma lath reinforces the TiAl-based composite material through the interaction with dislocation, and second phases with two scales and two categories are respectively precipitated at the grain boundary of the TiAl-based composite material and in the alpha 2/gamma lath, so that the performance of the TiAl-based composite material can be more effectively improved.
The following examples are provided to demonstrate specific technical effects of the present invention.
Example 1
In this embodiment, the preparation method of the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material comprises the following steps: placing 0.3gBN nanosheets and 99.7g of Ti-48Al-2Nb-2Cr alloy powder into a ball milling tank for mechanical ball milling, and performing mechanical ball milling and mixing for 360min at a ball-to-material ratio of 3:1 at 300r/min to obtain mixed powder. And (3) performing discharge plasma sintering on the mixed powder for 5min under the conditions that the temperature is 1300 ℃ and the pressure is 45MPa to obtain the in-situ dual-phase dual-scale synergistically enhanced Ti-48Al-2Nb-2 Cr-based composite material.
FIGS. 1 and 2 are SEM micrographs of 200X and 2000X, respectively, of the two-phase dual-scale synergistically reinforced Ti-48Al-2Nb-2 Cr-based composite material prepared in this example. As can be seen from FIG. 1, the composite material is a compact full-sheet structure, the size of the sheet groups is distributed in the range of 100-200 μm, and FIG. 2 is an enlarged view of the microstructure of a part of the composite material. As is apparent from fig. 1 and fig. 2, TiB2 whiskers with a length of 10-20 μm are pinned on grain boundaries between the sheet clusters of the two-phase dual-scale synergistically reinforced Ti-48Al-2Nb-2 Cr-based composite material of the present embodiment, and Ti2AlN reinforcing phases with a range of 100-200 nm are dispersedly distributed at α 2/γ lath gaps formed by the α 2 phase and the γ phase.
Example 2
In this embodiment, the preparation method of the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material comprises the following steps: placing 1gBN nanosheets and 99gTi-48Al-2Nb-2Cr alloy powder into a ball milling tank for mechanical ball milling, and performing mechanical ball milling and mixing for 360min at a ball-to-material ratio of 3:1 at a speed of 300r/min to obtain mixed powder. And (3) performing discharge plasma sintering on the mixed powder for 10min under the conditions that the temperature is 1250 ℃ and the pressure is 45MPa to obtain the in-situ dual-phase dual-scale synergistically enhanced Ti-48Al-2Nb-2 Cr-based composite material.
Similarly, micrometer-scale TiB2 whiskers are distributed on the grain boundary between the sheet clusters of the composite material with the full-sheet structure obtained in the embodiment, and nanometer-scale Ti2AlN reinforcing phases are distributed at the α 2/γ lath gaps formed by the α 2 phase and the γ phase.
Example 3
In this embodiment, the preparation method of the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material comprises the following steps: placing 0.1gBN nanosheets and 99.9g of Ti-48Al-2Nb-2Cr alloy powder into a ball milling tank for mechanical ball milling, and performing mechanical ball milling and mixing for 360min at a ball-to-material ratio of 3:1 at 300r/min to obtain mixed powder. And (3) performing discharge plasma sintering on the mixed powder for 8min under the conditions that the temperature is 1300 ℃ and the pressure is 40MPa to obtain the in-situ dual-phase dual-scale synergistically enhanced Ti-48Al-2Nb-2 Cr-based composite material.
Similarly, micrometer-scale TiB2 whiskers are distributed on the grain boundary between the sheet clusters of the composite material with the full-sheet structure obtained in the embodiment, and nanometer-scale Ti2AlN reinforcing phases are distributed at the α 2/γ lath gaps formed by the α 2 phase and the γ phase.
Example 4
In this embodiment, the preparation method of the in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material comprises the following steps: placing 0.5gBN nanosheets and 99.5g of Ti-45Al-8Nb alloy powder into a ball milling tank for mechanical ball milling, and performing mechanical ball milling and mixing for 360min at a ball-to-material ratio of 3:1 at 300r/min to obtain mixed powder. And (3) performing discharge plasma sintering on the mixed powder for 10min under the conditions that the temperature is 1350 ℃ and the pressure is 30MPa to obtain the in-situ dual-phase dual-scale synergistically enhanced Ti-45Al-8 Nb-based composite material.
Similarly, micrometer-scale TiB2 whiskers are distributed on the grain boundary between the sheet clusters of the composite material with the full-sheet structure obtained in the embodiment, and nanometer-scale Ti2AlN reinforcing phases are distributed at the α 2/γ lath gaps formed by the α 2 phase and the γ phase.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (8)
1. A preparation method of an in-situ two-phase dual-scale synergistically enhanced TiAl-based composite material is characterized by mixing BN and TiAl alloy powder in proportion, then carrying out mechanical ball milling mixing to obtain mixed powder, then carrying out spark plasma sintering on the mixed powder, and cooling to obtain the in-situ two-phase dual-scale synergistically enhanced TiAl-based composite material.
2. The production method according to claim 1, wherein the composition of the TiAl alloy powder is, in atomic percent, Al: 44-48%; nb: 2-8%; cr: 0-2%; v: 0 to 3 percent; mo: 0-2% and the balance Ti.
3. The production method according to claim 1, wherein the mixed powder contains BN in a mass fraction of 0.1 to 1 wt%.
4. The preparation method according to claim 1, wherein the spark plasma sintering temperature is 1250-1350 ℃, the holding time is 5-10 min, and the pressure is 30-45 MPa.
5. The preparation method of claim 1, wherein the ratio of balls to materials in the mechanical ball milling process is 3: 1.
6. The in-situ dual-phase dual-scale synergistically enhanced TiAl-based composite material obtained by the preparation method according to any one of claims 1 to 5 is characterized in that the composite material is of a full-lamellar structure, micron-scale TiB2 whiskers are distributed on a crystal boundary between lamellar clusters, and nano-scale Ti2AlN enhanced phases are distributed at alpha 2/gamma lath gaps formed by alpha 2 phases and gamma phases in a dispersing manner.
7. The in-situ dual-phase dual-scale synergistically reinforced TiAl-based composite material according to claim 6, wherein the size of the TiB2 whiskers is 10-20 μm.
8. The in-situ dual-phase dual-scale synergistically reinforced TiAl-based composite material according to claim 6, wherein the Ti2AlN reinforcing phase has a size of 100 to 200 nm.
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| CN116200622A (en) * | 2023-04-27 | 2023-06-02 | 西安稀有金属材料研究院有限公司 | Preparation method of superfine crystal TiAl alloy and composite material thereof |
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