CN118186253A - Core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material and preparation method thereof - Google Patents
Core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material and preparation method thereof Download PDFInfo
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- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000011258 core-shell material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000005242 forging Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000956 alloy Substances 0.000 claims description 35
- 229910045601 alloy Inorganic materials 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 17
- 239000011812 mixed powder Substances 0.000 claims description 13
- 230000009977 dual effect Effects 0.000 claims description 9
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000012071 phase Substances 0.000 description 71
- 238000009826 distribution Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910009594 Ti2AlN Inorganic materials 0.000 description 1
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000008384 inner phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
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Abstract
The invention provides a core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material and a preparation method thereof, wherein a matrix of the TiAl-based composite material comprises a gamma phase, and a core-shell structure reinforcing phase comprises an inner Ti 2 AlC phase and an outer Ti 3SiC2 phase. The composite material is prepared by ball milling, hot pressing sintering, sheath hot forging and heat treatment processes, and then furnace cooling is carried out.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to a core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material and a preparation method thereof.
Background
The TiAl-based alloy has excellent comprehensive properties such as low density (-4.0 g/cm 3), high specific strength, high specific modulus, good high-temperature oxidation resistance, creep resistance and the like, and is considered as an advanced high-temperature structural material with the most application prospect in the range of 700-1000 ℃. Although the TiAl-based alloy is preliminarily applied to engineering in the industrial fields of aeroengines and the like, for example, the American GE company is used for preparing low-pressure turbine blades of GEnx and GE9X aeroengines, a certain gap exists between the wide application range. The present situation is caused by the fact that the room temperature brittleness and the high temperature strength are difficult to be further improved and the forming performance is poor. Among them, how to further improve the high temperature strength thereof is one of the most urgent fundamental problems to be solved. Research shows that the composite material technology is one of effective ways for effectively improving the comprehensive mechanical properties of the TiAl-based alloy. The TiAl-based composite material with excellent comprehensive performance is obtained by reinforcing the TiAl-based alloy by utilizing continuous fiber reinforcement or discontinuous short fibers, whiskers and particles through a composite material technology, and has become a main trend of the development of the TiAl-based alloy.
The preparation process of the TiAl-based composite material mainly comprises smelting casting and powder metallurgy. The fusion casting method is the earliest method for preparing TiAl alloy and composite materials thereof, has the advantages of near net forming, simple process, low cost and the like, but also has the defects of coarse structure and easy generation of casting defects such as component segregation, shrinkage cavity, shrinkage porosity, cracks and the like. The powder metallurgy method can effectively avoid casting defects such as looseness, shrinkage cavity and the like, and the TiAl-based alloy and the composite material thereof prepared by the method have uniform components and fine tissues, and are favorable for obtaining more excellent mechanical properties, so the powder metallurgy method has become a very important preparation method of the TiAl alloy and the composite material. However, the ingot of the TiAl-based composite material directly prepared by adopting powder metallurgy sintering processes such as vacuum hot-pressed sintering, hot isostatic pressing, spark plasma sintering and the like often has the defects of a small number of micropores (mostly caused by powder defects), flat grain boundaries and the like, and the full play of the reinforcing effect of the reinforcing phase is affected.
The MAX phase is a ternary lamellar compound, the composition of which can be represented by M n+1AXn, M is transition metal, A is mainly IIIA and IVA groups, X is C or N, N is generally 1-3, and common compounds are Ti 2AlC、Ti2AlN、Ti3SiC2、Ti3AlC2, ti 3GeC2 and the like. The MAX has the characteristics of metal and ceramic when being the same: has metal-like thermal conductivity, electrical conductivity and machinability, and also has ceramic-like high melting point, high hardness, high modulus, high oxidation resistance and thermal stability. Therefore, the preparation of the MAX phase reinforced TiAl-based composite material can effectively improve the high-temperature strength and other performances of the TiAl alloy, and has good application prospect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material and a preparation method thereof. According to the method, the double MAX phase high Wen Jianghua TiAl-based composite material with a core-shell structure is prepared by utilizing the fact that the solubility of C atoms and Si atoms in matrix alloy is different and the solubility of alloy elements in different MAX phases is different.
In order to achieve the above object, the present invention provides a dual MAX phase high temperature reinforced TiAl based composite material of core-shell structure, wherein: the matrix of the TiAl-based composite material comprises a gamma phase, and the core-shell structure reinforcing phase comprises an internal Ti 2 AlC phase and an external Ti 3SiC2 phase.
Preferably, the size of the core-shell structure reinforcing phase is 10-50 μm, wherein the thickness of the outer layer Ti 3SiC2 phase is 0.5-3 μm.
Preferably, the raw materials of the TiAl-based composite material comprise TiAl alloy powder and SiC powder; the SiC powder accounts for 1-5wt% of the TiAl-based composite material raw material.
Preferably, in the TiAl alloy, al: 43-48%; nb: 2-10%; cr:0 to 4 percent; w:0 to 2 percent; b:0 to 0.5 percent and the balance of Ti.
The invention provides a method for preparing a core-shell structure double MAX phase high temperature reinforced TiAl-based composite material, which comprises the following steps,
Ball milling: ball milling is carried out on SiC powder and TiAl alloy powder to obtain mixed powder;
hot pressing and sintering: hot-pressing and sintering the mixed powder to obtain a TiAl-based composite material blank;
And (3) hot forging of the sheath: performing sheath hot forging on the blank;
and (3) heat treatment: and (3) carrying out annealing heat treatment on the sheath body, and then cooling in a furnace.
Preferably, the ball milling is carried out under the protection of argon, the ball-material ratio is 1:5, and the grinding balls are made of stainless steel.
Preferably, the hot-pressing sintering is performed in an argon atmosphere, the temperature is 1250-1300 ℃, the heat preservation and pressure maintaining time is 2-5 h, and the pressure is 20-50 MPa.
Preferably, the hot forging temperature of the sheath is 1250-1300 ℃, and the deformation is 30-70%.
Preferably, the heat treatment is carried out at 800-1000 ℃ for 2 hours.
The beneficial effects of the invention are as follows:
1. According to the invention, the double MAX phase high Wen Jianghua TiAl-based composite material with a core-shell structure is prepared by utilizing the fact that the solubility of C atoms and Si atoms in matrix alloy is different and the solubility of alloy elements in different MAX phases. During hot press sintering, si and C elements in the SiC particles are separated, wherein the C elements are distributed in a gradient from inside the reinforcing phase to the matrix, and the Si elements are mainly concentrated on the outer layer of the reinforcing phase. The invention realizes that the double MAX phase with the core-shell structure is introduced into the TiAl-based composite material, and can effectively improve the high temperature strength of the TiAl-based alloy.
2. The invention utilizes a hot-press sintering method to generate a double MAX phase with a core-shell structure in a TiAl alloy matrix. On the one hand, the formation of the outer Ti 3SiC2 phase effectively prevents the diffusion of elements between the TiAl matrix and the inner Ti 2 AlC phase, so that the core-shell structure has higher thermal stability compared with a single MAX phase; on the other hand, the hardness of the outer Ti 3SiC2 phase is always higher than that of the inner Ti 2 AlC phase, and the core-shell structure with the outer hardness and the inner softness has better toughness than that of a single phase, so that cracks in the loading process are restrained, and therefore, the core-shell structure has better toughening effect than that of a single MAX phase.
3. The method can adjust the generation quantity and distribution of the double MAX phases by controlling the addition quantity of SiC, hot-pressing sintering and hot forging process parameters, is flexible and convenient, has simple operation in the whole process, is easy to implement, and improves the application value of the method.
Drawings
FIG. 1 is a low-power SEM microscopic structure diagram of a dual MAX phase high temperature reinforced Ti-47.5Al-7Nb-0.4W-0.1B matrix composite;
Electron probe micro-area scanning analysis of the composite reinforcement phase prepared in fig. 2, wherein: (a) a back-scattering microstructure; (b) Ti element distribution; (c) Al element distribution; (d) Nb element distribution; (e) W element distribution; (f) B element distribution; (g) Si element distribution; (h) distribution of C elements.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present application, the present application will be further described with reference to the following specific examples.
The technical scheme adopted by the invention is as follows:
In a first aspect, the invention provides a preparation method of a core-shell structure double MAX phase high Wen Jianghua TiAl-based composite material, which comprises the following steps: mixing SiC and TiAl-based alloy powder according to a proportion, performing mechanical ball milling and mixing to obtain mixed powder, performing argon atmosphere protection hot-pressing sintering on the mixed powder to obtain a TiAl-based composite material blank, performing sheath hot forging with a certain deformation on the TiAl-based alloy composite material blank, and cooling to obtain the required double MAX phase-high Wen Jianghua TiAl-based composite material with a core-shell structure.
Preferably, the components of the TiAl alloy powder are as follows: 43-48%; nb: 2-10%; cr:0 to 4 percent; w:0 to 2 percent; b:0 to 0.5 percent and the balance of Ti.
Preferably, the mass fraction of SiC in the mixed powder is 1 to 5wt%.
Preferably, in the mechanical ball milling process, powder mixing is carried out under the protection of argon, the ball-to-material ratio is 1:5, and the grinding balls are made of stainless steel.
Preferably, the argon atmosphere protects the hot-pressing sintering temperature from 1250 to 1300 ℃, the heat preservation and pressure maintaining time is 2 to 5 hours, and the pressure is 20 to 50MPa.
Preferably, the hot forging temperature of the sheath is 1250-1300 ℃, the deformation is 30-70%, and after the hot forging is finished, the sheath body is annealed, and the specific heat treatment process is as follows: preserving heat for 2h at 800-1000 ℃, and then cooling in a furnace.
In a second aspect, the present invention provides a core-shell structure dual MAX phase high Wen Jianghua TiAl-based composite material obtained by the preparation method according to any one of the first aspects, wherein a matrix of the composite material is a near-gamma structure and mainly comprises gamma phase, and a uniformly distributed core-shell structure reinforcing phase mainly comprises an inner Ti 2 AlC phase and an outer Ti 3SiC2 phase.
Preferably, the size of the reinforcing phase having a core-shell structure is 10 to 50 μm, and the thickness of the outer layer Ti 3SiC2 phase is 0.5 to 3 μm.
Example 1
In this embodiment, the preparation method of the core-shell structure dual MAX phase high Wen Jianghua TiAl-based composite material includes: 3g of SiC powder and 97g of Ti-47.5Al-7Nb-0.4W-0.1B (at.%) alloy powder are placed in a ball milling tank of mechanical ball milling, and the mixture is subjected to mechanical ball milling and mixing for 7.5 hours at the speed of 150r/min under the condition that the ball-to-material ratio is 1:5, so as to obtain mixed powder. And carrying out argon atmosphere hot-pressing sintering on the mixed powder for 2 hours under the conditions of 1250 ℃ and 20MPa to obtain a TiAl-based composite material blank. The blank is subjected to sheath hot forging under the conditions that the temperature is 1250 ℃ and the deformation is 50%, and after the hot forging is finished, the sheath body is subjected to annealing heat treatment, wherein the specific heat treatment process comprises the following steps: and (3) preserving heat for 2 hours at 850 ℃, and then cooling in a furnace to obtain the core-shell structure double MAX phase high temperature reinforced Ti-47.5Al-7Nb-0.4W-0.1B matrix composite.
FIG. 1 is a low-magnification SEM micrograph of a core-shell structure double MAX phase high temperature reinforced Ti-47.5Al-7Nb-0.4W-0.1B matrix composite prepared in this example. From fig. 1, it can be seen that the matrix of the composite material is a near gamma tissue, the reinforcing phase presents a remarkable core-shell structure, and the size is 10-50 μm.
FIG. 2 shows the results of electron probe micro-area scanning analysis of the reinforcing phase of the composite material. As is apparent from fig. 2, three elements of Ti, al and C in the reinforcing phase of the composite material prepared in this embodiment are mainly distributed in the Ti 2 AlC phase, while other elements are mainly concentrated in the outer layer phase Ti 3SiC2 of the reinforcing phase, and the thickness of the outer layer Ti 3SiC2 phase is 0.5-3 μm.
The high temperature compression yield strength is as follows: the yield strength at 900 ℃ can reach more than 400MPa, and compared with the yield strength at 900 ℃ of the TiAl matrix alloy, the yield strength is only 370MPa; the yield strength at 1000 ℃ can reach more than 230MPa, and compared with the yield strength at 1000 ℃ of the TiAl matrix alloy, the yield strength is only 200MPa.
Example 2:
In this embodiment, the preparation method of the core-shell structure dual MAX phase high Wen Jianghua TiAl-based composite material includes: placing 1gSiC powder and 99g Ti-48Al-2Cr-2Nb alloy powder into a ball milling tank for mechanical ball milling, and carrying out mechanical ball milling and mixing for 7.5 hours at the speed of 150r/min under the condition that the ball-to-material ratio is 1:5, so as to obtain mixed powder. And carrying out argon atmosphere hot-pressing sintering on the mixed powder for 3 hours under the conditions of 1300 ℃ and 20MPa to obtain a TiAl-based composite material blank. The blank is subjected to sheath hot forging under the conditions that the temperature is 1250 ℃ and the deformation is 40%, and after the hot forging is finished, the sheath body is subjected to annealing heat treatment, wherein the specific heat treatment process comprises the following steps: and (3) preserving heat for 2 hours at 900 ℃, and then cooling in a furnace to obtain the core-shell structure double MAX phase high temperature reinforced Ti-48Al-2Cr-2Nb based composite material.
Similarly, the matrix of the composite material obtained in this embodiment is a near-gamma structure, and mainly comprises gamma phase, while the uniformly distributed core-shell structure reinforcing phase mainly comprises an inner Ti 2 AlC phase and an outer Ti 3SiC2 phase.
The high temperature compression yield strength is as follows: the yield strength at 900 ℃ can reach more than 350MPa, and compared with the yield strength at 900 ℃ of the TiAl matrix alloy, the yield strength is only 300MPa; the yield strength at 1000 ℃ can reach more than 190MPa, and compared with the yield strength at 1000 ℃ of the TiAl matrix alloy is only about 150 MPa.
Example 3:
In this embodiment, the preparation method of the core-shell structure dual MAX phase high Wen Jianghua TiAl-based composite material includes: placing 4gSiC powder and 96g Ti-48Al-2Cr-2Nb alloy powder into a ball milling tank for mechanical ball milling, and carrying out mechanical ball milling and mixing for 7.5 hours at the speed of 150r/min under the condition that the ball-to-material ratio is 1:5, so as to obtain mixed powder. And carrying out hot-pressing sintering on the mixed powder for 2.5 hours in an argon atmosphere under the conditions of the temperature of 1280 ℃ and the pressure of 30MPa to obtain a TiAl-based composite material blank. The blank is subjected to sheath hot forging under the conditions that the temperature is 1300 ℃ and the deformation is 60%, and after the hot forging is finished, the sheath body is subjected to annealing heat treatment, wherein the specific heat treatment process comprises the following steps: and (3) preserving heat for 2 hours at 950 ℃, and then cooling in a furnace to obtain the core-shell structure double MAX phase high temperature reinforced Ti-48Al-2Cr-2 Nb-based composite material.
Similarly, the matrix of the composite material obtained in this embodiment is a near-gamma structure, and mainly comprises gamma phase, while the uniformly distributed core-shell structure reinforcing phase mainly comprises an inner Ti 2 AlC phase and an outer Ti 3SiC2 phase.
The high temperature compression yield strength is as follows: the yield strength at 900 ℃ can reach more than 380MPa, and compared with the yield strength at 900 ℃ of the TiAl matrix alloy, the yield strength is only 300MPa; the yield strength at 1000 ℃ can reach more than 210MPa, and compared with the yield strength at 1000 ℃ of the TiAl matrix alloy is only about 150 MPa.
In the TiAl-based composite material of the invention, si element is mainly distributed in the outer layer phase of the core-shell structure reinforcing phase, and C element is mainly distributed in the inner phase of the core-shell structure reinforcing phase. During hot press sintering, si and C elements in the SiC particles are separated, wherein the C elements are distributed in a gradient from inside the reinforcing phase to the matrix, and the Si elements are mainly concentrated on the outer layer of the reinforcing phase. This phenomenon may be caused by two reasons: on the one hand, because the solubility of Si atoms in the TiAl matrix is very low, the Si atoms cannot be diffused into the matrix in a large scale in the hot-pressed sintering process, so that the Si atoms are enriched on the surface layer of the reinforcing phase; on the other hand, the solubility of Si element in the Ti 2 AlC phase is small, and thus, tends to be distributed outside the reinforcing phase. The invention realizes that the double MAX phase with the core-shell structure is introduced into the TiAl-based composite material, and can effectively improve the high-temperature strength of the TiAl-based alloy.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. A kind of core-shell structure double MAX phase high temperature reinforced TiAl base composite material, characterized by that: the matrix of the TiAl-based composite material comprises a gamma phase, and the core-shell structure reinforcing phase comprises an internal Ti 2 AlC phase and an external Ti 3SiC2 phase.
2. The core-shell structure dual MAX phase high temperature strengthened TiAl-based composite material of claim 1, wherein: the size of the core-shell structure reinforcing phase is 10-50 mu m, wherein the thickness of the outer layer Ti 3SiC2 phase is 0.5-3 mu m.
3. The core-shell structure dual MAX phase high temperature strengthened TiAl-based composite material of claim 1, wherein: the raw materials of the TiAl-based composite material comprise TiAl alloy powder and SiC powder, wherein the SiC accounts for 1-5wt% of the raw materials of the TiAl-based composite material.
4. The core-shell structure dual MAX phase high temperature strengthened TiAl-based composite of claim 3, wherein: the TiAl alloy comprises the following components in percentage by atom: 43-48%; nb: 2-10%; cr:0 to 4 percent; w:0 to 2 percent; b:0 to 0.5 percent and the balance of Ti.
5. A method for preparing the core-shell structure double MAX phase high temperature reinforced TiAl-based composite material of any one of claims 1-4, characterized in that: comprises the steps of,
Ball milling: ball milling is carried out on SiC and TiAl alloy to obtain mixed powder;
hot pressing and sintering: hot-pressing and sintering the mixed powder to obtain a TiAl-based composite material blank;
And (3) hot forging of the sheath: performing sheath hot forging on the blank;
and (3) heat treatment: and (3) carrying out annealing heat treatment on the sheath body, and then cooling in a furnace.
6. The method according to claim 5, wherein: the ball milling is carried out under the protection of argon, the ball-material ratio is 1:5, and the grinding ball is made of stainless steel.
7. The method according to claim 5, wherein: the hot-pressing sintering is performed in an argon atmosphere, the temperature is 1250-1300 ℃, the heat preservation and pressure maintaining time is 2-5 h, and the pressure is 20-50 MPa.
8. The method according to claim 5, wherein: the hot forging temperature of the sheath is 1250-1300 ℃, and the deformation is 30-70%.
9. The method according to claim 5, wherein: the heat treatment is to keep the temperature at 800-1000 ℃ for 2h.
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