CN115354182A - TiAl in-situ growth 3 Texture of the skeleton Ti 3 AlC 2 Preparation method of reinforced aluminum-based composite material - Google Patents
TiAl in-situ growth 3 Texture of the skeleton Ti 3 AlC 2 Preparation method of reinforced aluminum-based composite material Download PDFInfo
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 44
- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 39
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 80
- 238000000498 ball milling Methods 0.000 claims abstract description 65
- 239000002245 particle Substances 0.000 claims abstract description 38
- 239000011159 matrix material Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims description 91
- 239000000463 material Substances 0.000 claims description 22
- 229910045601 alloy Inorganic materials 0.000 claims description 20
- 239000000956 alloy Substances 0.000 claims description 20
- 235000021355 Stearic acid Nutrition 0.000 claims description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 13
- 239000008117 stearic acid Substances 0.000 claims description 13
- 239000002923 metal particle Substances 0.000 claims description 12
- 238000002490 spark plasma sintering Methods 0.000 claims description 10
- 229910017818 Cu—Mg Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004886 process control Methods 0.000 claims description 6
- 229910021364 Al-Si alloy Inorganic materials 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910018594 Si-Cu Inorganic materials 0.000 claims description 4
- 229910008465 Si—Cu Inorganic materials 0.000 claims description 4
- 229910007565 Zn—Cu Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 229910018569 Al—Zn—Mg—Cu Inorganic materials 0.000 claims description 2
- 229910019086 Mg-Cu Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 238000000713 high-energy ball milling Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 229910009818 Ti3AlC2 Inorganic materials 0.000 abstract description 2
- 229910010039 TiAl3 Inorganic materials 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 11
- 239000011156 metal matrix composite Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003014 reinforcing effect 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
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- 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
- 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
- B22F3/02—Compacting only
-
- 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
- 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
-
- 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
- C22C21/00—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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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
- 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
-
- 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
- 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
Abstract
A preparation method of a texture Ti3AlC2 reinforced aluminum matrix composite with a TiAl3 framework grown in situ relates to a preparation method of an aluminum matrix composite. To solve the problem of low temperature and high efficiencyTi 3 AlC 2 Ti in oriented arrangement in Al composite material 3 AlC 2 And in situ autogenous TiAl 3 To (3) is described. The method comprises the following steps: with Ti of large particle size 3 AlC 2 The powder and aluminum metal powder are used as raw materials, and Ti with very small thickness/length ratio is prepared by high-energy ball milling 3 AlC 2 Sheet and aluminum sheet metal; then mixing the two flaky powders by low-energy ball milling, and finally sintering by combining cold pressing and discharge plasma to ensure that the flaky Ti in the composite material 3 AlC 2 And (4) texturing and arranging the particles. The invention can effectively reduce the reaction temperature and the reaction time, the composite material has higher room temperature and high temperature strength, and TiAl can be regulated and controlled 3 The generation amount of the composite material is reduced, so that the effective regulation and control of the composite material tissue can be realized.
Description
Technical Field
The invention relates to a preparation method of an aluminum matrix composite.
Background
The Metal Matrix Composites (MMCs) have excellent comprehensive mechanical properties and are widely applied to the fields of aerospace and the like. Conventional hard ceramics such as SiC and Al 2 O 3 Etc. as reinforcement typically results in low plasticity, which limits the use of MMCs. The MAX phase is a novel ceramic, has a nano-layered structure, can generate deformation modes such as basal plane slippage, kinking and the like under the action of external force, and has pseudoplasticity and high fracture toughness. In recent years, researchers have attempted to use a deformable MAX phase as a metallic reinforcement,to increase the ductility of the MMCs. As a typical MAX phase, ti 3 AlC 2 Low cost and good comprehensive mechanical property, and is an ideal reinforcement of a metal matrix.
However, the deformable nature of the MAX phase tends to result in limited strengthening effects. In order to fully exploit the strengthening power of the MAX phase, more advanced technical routes are needed to optimize the material preparation. It is reported that the deformation behavior of the MAX phase is significantly affected by the grain orientation, and that the directionally arranged flaky MAX phase particles improve toughness through grain pullout and crack bridging. Thus, the strength and toughness of the MAX phase and its composite can be improved by texturing. Further, as Ti 3 Important interface reaction products of AlC2 and Al systems, tiAl 3 The high-strength high-hardness high-strength composite material has ultrahigh hardness and excellent high-temperature strength, and can remarkably strengthen the composite material and improve the high-temperature performance of the composite material. Thus, in the texture Ti 3 AlC 2 Considerable TiAl is generated in situ in particle reinforced aluminum-based composite material 3 Is ideal for increasing Ti 3 AlC 2 A method for preparing the Al composite material. However, at present, various MAX phase reinforced metal matrix composite materials can be prepared at home and abroad. However, in Ti 3 AlC 2 In-situ generation of TiAl in the Al system 3 Higher sintering temperatures are generally required. In addition, obtaining textured MAX phases in composite materials often requires secondary processing means such as hot deformation, which is inefficient. The difficulty at present is how to realize the low-temperature and high-efficiency Ti 3 AlC 2 Ti in oriented arrangement is simultaneously obtained in the Al composite material 3 AlC 2 And in situ autogenous TiAl 3 。
Disclosure of Invention
The invention aims to solve the problem of how to efficiently and at low temperature in Ti 3 AlC 2 Ti in oriented arrangement is simultaneously obtained in the Al composite material 3 AlC 2 And in situ autogenous TiAl 3 To provide an in-situ grown TiAl 3 Texture of the skeleton Ti 3 AlC 2 A preparation method of a reinforced aluminum matrix composite.
The invention grows TiAl in situ 3 Texture Ti of skeleton 3 AlC 2 Reinforced aluminiumThe preparation method of the base composite material comprises the following steps:
1. weighing material
Weighing 5-30% of Ti by volume fraction 3 AlC 2 Powder and 95 to 70 percent of aluminum metal powder;
the average diameter of the aluminum metal powder is 1-20 mu m;
the Ti 3 AlC 2 The average grain diameter of the powder is 15-60 mu m;
2. ti 3 AlC 2 Breaking and sheet ball milling of powder
Ti weighed in the step one 3 AlC 2 Putting the powder into a ball milling tank for ball milling; the ball-material ratio is (8-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-20 h; by ball milling of Ti 3 AlC 2 Opening cluster, breaking particles, and stripping interlayer to obtain sheet Ti with thickness of 0.1-2 μm and diameter of 0.3-5 μm 3 AlC 2 A particle;
3. sheet ball mill for aluminum metal powder
Putting the aluminum metal powder weighed in the step one into a ball milling tank for ball milling; the ball-material ratio is (5-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-30 h; deforming the spherical aluminum metal particles by ball milling to obtain sheet aluminum metal particles with the thickness of 0.2-1.6 mu m and the diameter of 8-15 mu m;
4. flake Ti 3 AlC 2 Ball milling and mixing of powder and aluminum flake metal powder
The sheet Ti obtained in the second step 3 AlC 2 Putting the particles and the sheet aluminum metal particles obtained in the step three into a ball milling tank for ball milling and mixing; low-energy ball milling is adopted, the ball material ratio is (1-2): 1, the rotating speed is 150 rpm-200 rpm, the ball milling time is 1.5 h-3 h, the two particles are fully mixed, and finally the temperature is kept for 10 h-20 h in a vacuum furnace or protective atmosphere at 200 ℃ -300 ℃ to obtain the sheet Ti 3 AlC 2 And a composite powder of sheet aluminum metal;
5. ti 3 AlC 2 Filling die of composite powder of aluminum and metal
The sheet Ti obtained in the step four 3 AlC 2 Uniformly pouring the composite powder of the flaky aluminum metal into a mold, fully vibrating the filled mold to ensure that the interior of the powder is uniform and the surface of the powder is smooth, and then carrying out cold pressing on the powder; in the cold pressing process, the pressurizing speed is 0.1 mm/min-3 mm/min, the pressure is increased to 4 MPa-20 MPa, and the pressure is maintained for 5 min-10 min, so that the directionally arranged Ti is obtained 3 AlC 2 And aluminum metal;
6. low temperature spark plasma sintering
Moving the composite preform obtained in the fifth step and the mold to a sintering chamber of a discharge plasma sintering furnace, assembling the mold by using an upper clamp and a lower clamp, and adjusting the interior of the furnace to be a vacuum environment;
firstly, preheating a prefabricated body to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-620 ℃ within 1-5 min;
then adjusting the temperature to 450-640 ℃ and keeping the temperature for 10-20 min under the condition that the pressure is 20-300 MPa, so that the preform is fully densified;
finally cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Texture of the skeleton Ti 3 AlC 2 A reinforced aluminum matrix composite.
The invention has the following beneficial effects:
1. ti of large particle size in the invention 3 AlC 2 The powder and aluminum metal powder are used as raw materials, and Ti with very small thickness/length ratio is prepared by high-energy ball milling respectively 3 AlC 2 Sheet and aluminum sheet metal; then fully mixing the two flaky powder bodies by low-energy ball milling; finally, cold pressing and spark plasma sintering are combined to ensure that the flaky Ti in the composite material 3 AlC 2 And (4) texturing and arranging the particles.
2. The invention provides an in-situ grown TiAl 3 Texture of the skeleton Ti 3 AlC 2 Method for producing reinforced aluminum matrix composite material, ti 3 AlC 2 The particle size and thickness of the sheet and aluminum sheet metal are very small, the surface energy is high, and may beThe reaction temperature and the reaction time are effectively reduced; by adopting spark plasma sintering, the Al matrix does not need to be heated to a liquid phase, and Ti can be generated in a very short time 3 AlC 2 TiAl with interpenetrated particles 3 A framework; tiAl with uniform structure and generated in situ of composite material 3 The composite material has good interface combination with a matrix, and the composite material has higher room temperature and high temperature strength.
3. The invention can regulate and control Ti by changing the ball-milling process including ball-material ratio, rotating speed, time and the like 3 AlC 2 Thickness and particle size of the flakes and Al flakes; tiAl can be regulated and controlled by changing SPS process including sintering temperature, holding time and the like 3 The amount of production of (c). Therefore, the effective regulation and control of the composite material tissue can be realized.
4. The TiAl prepared by the invention grows in situ 3 Texture of the skeleton Ti 3 AlC 2 In reinforced Al-based composites, tiAl 3 The volume fraction of (A) is 10-40%, and the density is 2.78g/cm 3 ～3.24g/cm 3 The compactness is more than 98 percent, the tensile strength is between 180 and 540MPa, and the elongation is between 0.2 and 4.5 percent.
Drawings
FIG. 1 example one resulting in-situ grown TiAl 3 Texture of the skeleton Ti 3 AlC 2 Microstructure photograph of the reinforced aluminum matrix composite.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first specific implementation way is as follows: this embodiment grows TiAl in situ 3 Texture of the skeleton Ti 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material comprises the following steps:
1. weighing material
Weighing 5-30% of Ti according to volume fraction 3 AlC 2 Powder and 95 to 70 percent of aluminum metal powder;
the average diameter of the aluminum metal powder is 1-20 mu m;
the Ti 3 AlC 2 The average grain diameter of the powder is 15-60 mu m;
2. ti (titanium) 3 AlC 2 Breaking and sheet ball milling of powder
Ti weighed in the step one 3 AlC 2 Putting the powder into a ball milling tank for ball milling; the ball-material ratio is (8-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-20 h; by ball milling of Ti 3 AlC 2 Opening clusters, crushing particles and carrying out interlayer stripping to obtain sheet Ti with the thickness of 0.1-2 mu m and the diameter of 0.3-5 mu m 3 AlC 2 Particles;
3. sheet ball mill for aluminum metal powder
Putting the aluminum metal powder weighed in the step one into a ball milling tank for ball milling; the ball-material ratio is (5-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-30 h; deforming the spherical aluminum metal particles by ball milling to obtain sheet aluminum metal particles with the thickness of 0.2-1.6 mu m and the diameter of 8-15 mu m;
4. flake Ti 3 AlC 2 Ball milling and mixing of powder and aluminum flake metal powder
The sheet Ti obtained in the second step 3 AlC 2 Putting the particles and the sheet aluminum metal particles obtained in the step three into a ball milling tank for ball milling and mixing; low-energy ball milling is adopted, the ball-material ratio is (1-2): 1, the rotating speed is 150 rpm-200 rpm, the ball milling time is 1.5 h-3 h, the two particles are fully mixed, and finally the temperature is kept for 10 h-20 h in a vacuum furnace or a protective atmosphere at 200 ℃ to 300 ℃ to obtain the flaky Ti 3 AlC 2 And a composite powder of sheet aluminum metal;
5. ti 3 AlC 2 Filling die of composite powder of aluminum and metal
The sheet Ti obtained in the fourth step 3 AlC 2 Uniformly pouring the composite powder of the flaky aluminum metal into a mold, fully vibrating the filled mold to ensure that the interior of the powder is uniform and the surface of the powder is smooth, and then cold pressing the powder; in the cold pressing process, the pressurizing speed is 0.1 mm/min-3 mm/min, the pressure is increased to 4 MPa-20 MPa, and the pressure is maintained for 5 min-10 min, so that the directionally arranged Ti is obtained 3 AlC 2 And aluminumA composite preform of metal;
6. low temperature spark plasma sintering
Moving the composite preform obtained in the fifth step and the mold to a sintering chamber of a discharge plasma sintering furnace, assembling the mold by using an upper fixture and a lower fixture, and adjusting the interior of the furnace to be in a vacuum environment;
firstly, preheating a prefabricated body to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-620 ℃ within 1-5 min;
then adjusting the temperature to 450-640 ℃ and keeping the temperature for 10-20 min under the condition of the pressure of 20-300 MPa, so that the preform is fully densified;
finally cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Texture of the skeleton Ti 3 AlC 2 A reinforced aluminum matrix composite.
The embodiment has the following beneficial effects:
1. in the present embodiment, ti having a large particle diameter is used 3 AlC 2 The powder and aluminum metal powder are used as raw materials, and Ti with very small thickness/length ratio is prepared by high-energy ball milling respectively 3 AlC 2 Sheet and aluminum sheet metal; then fully mixing the two flaky powder bodies by low-energy ball milling; finally, cold pressing and spark plasma sintering are combined to ensure that the flaky Ti in the composite material 3 AlC 2 And (4) texturing and arranging the particles.
2. The embodiment provides an in-situ growth TiAl 3 Texture of the skeleton Ti 3 AlC 2 Method for producing reinforced aluminum matrix composite, ti 3 AlC 2 The particle size and thickness of the sheet and the aluminum sheet are very small, the surface energy is high, and the reaction temperature and the reaction time can be effectively reduced; by adopting spark plasma sintering, ti can be generated in a very short time without heating the Al matrix to a liquid phase 3 AlC 2 TiAl with interpenetrated particles 3 A framework; the composite material has uniform tissue and TiAl generated in situ 3 The composite material has good interface combination with a matrix, and the composite material has higher room temperature and high temperature strength.
3. In the embodiment, ti can be regulated and controlled by changing the ball milling process including ball-material ratio, rotating speed, time and the like 3 AlC 2 Thickness and particle size of the flakes and Al flakes; tiAl can be regulated and controlled by changing SPS process including sintering temperature, holding time and the like 3 The amount of production of (c). Therefore, the effective regulation and control of the composite material tissue can be realized.
4. In-situ grown TiAl prepared by the embodiment 3 Texture of the skeleton Ti 3 AlC 2 In reinforced Al-based composites, tiAl 3 The volume fraction of (A) is 10-40%, and the density is 2.78g/cm 3 ～3.24g/cm 3 The compactness is more than 98 percent, the tensile strength is between 180 and 540MPa, and the elongation is between 0.2 and 4.5 percent.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the aluminum metal is pure aluminum or aluminum alloy.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the aluminum metal is one or a combination of more of Al-Si alloy, al-Si-Cu alloy, al-Cu-Mg alloy, al-Zn-Cu alloy, al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the mass fraction of Si in the Al-Si alloy is 2-25%; the mass fraction of Si in the Al-Si-Cu alloy is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Zn in the Al-Zn-Cu alloy is 0.5-55%, and the mass fraction of Cu is 0.5-53%; in the Al-Zn-Mg-Cu alloy, the mass fraction of Zn is 0.5-55%, the mass fraction of Mg is 0.5-38%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Cu-Mg alloy is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%.
The fifth concrete implementation mode is as follows: the difference between this embodiment and one of the first to fourth embodiments is: the Ti in the step one 3 AlC 2 The purity of (A) is more than 95%.
The sixth specific implementation mode is as follows: the difference between this embodiment and one of the first to fifth embodiments is: in the second step, stearic acid is used as a process control agent in the ball milling process, and the stearic acid is Ti 3 AlC 2 0.1 to 0.3 percent of the powder mass.
The seventh concrete implementation mode: the difference between this embodiment and one of the first to sixth embodiments is: in the ball milling process in the second step, the materials of the used milling pot and the milling ball are stainless steel, zirconia or tungsten carbide.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and step three, stearic acid is used as a process control agent in the ball milling process, and the stearic acid accounts for 0.25-0.5 percent of the mass of the aluminum metal powder.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and the diameter of the inner wall of the die in the fifth step is 40-120 mm.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is that: the protective atmosphere in the fourth step is one of nitrogen, argon, helium and the like; the pressure of the protective gas is 0.1MPa to 10MPa.
The following examples were employed to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: example in situ growth of TiAl 3 Texture of the skeleton Ti 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is completed according to the following steps:
1. weighing material
Weighing 20% by volume of Ti 3 AlC 2 Powder and 80% aluminum metal powder; the Ti 3 AlC 2 The purity of the powder is 99%; ti 3 AlC 2 The particle size range of the powder is 10-20 mu m, and the average particle size is 14.8 mu m; the aluminum metal is pure Al; the particle size range of the aluminum metal is 3-10.6 mu m, and the average particle size is 4.5 mu m;
2. ti 3 AlC 2 Breaking and sheet ball milling of powder
Ti weighed in the step one 3 AlC 2 Putting the powder into a zirconia ball-milling tank for ball milling; stearic acid is used as a process control agent, and the stearic acid is Ti 3 AlC 2 0.25% of the powder mass; the ball-material ratio is 10; by ball milling of Ti 3 AlC 2 Opening clusters, crushing particles and carrying out interlayer stripping to obtain sheet Ti with the thickness of 0.3-2 mu m and the diameter of 0.8-5 mu m 3 AlC 2 Particles;
3. sheet ball mill for aluminum metal powder
Putting the aluminum metal powder weighed in the step one into a ball milling tank for ball milling; stearic acid is used as a process control agent, and the stearic acid accounts for 0.4 percent of the mass of the aluminum metal powder; the ball-material ratio is 10; deforming the spherical aluminum metal particles by ball milling to obtain sheet aluminum metal particles with the thickness of 0.8-2.5 microns and the diameter of 8-12 microns;
4. flake Ti 3 AlC 2 Ball milling and mixing of powder and aluminum flake metal powder
The flaky Ti obtained in the step two 3 AlC 2 Putting the particles and the sheet aluminum metal particles obtained in the step three into a ball milling tank for ball milling and mixing; and (2) performing low-energy ball milling for 3 hours at a ball-material ratio of 2 to 200rpm in a vacuum furnace, fully mixing the two particles, and finally, preserving heat for 10 hours in the vacuum furnace at 250 ℃ to fully remove stearic acid on the surface of the powder to obtain the flaky Ti 3 AlC 2 And a composite powder of sheet aluminum metal;
5. ti 3 AlC 2 Filling die of composite powder of aluminum and metal
The sheet Ti obtained in the step four 3 AlC 2 Uniformly pouring the composite powder of the flaky aluminum metal and the flaky aluminum metal into a mold, wherein the diameter of the inner wall of the mold is 60mm; fully vibrating the filled die to ensure that the interior of the powder is uniform and the surface of the powder is smooth, and then carrying out cold pressing on the powder; in the cold pressing process, the pressurizing speed is 0.5mm/min, the pressure is increased to 5MPa and maintained for 5min, and the Ti in directional arrangement is obtained 3 AlC 2 And aluminum metal;
6. low temperature spark plasma sintering
Moving the composite preform obtained in the fifth step and the mold to a sintering chamber of a discharge plasma sintering furnace, assembling the mold by using an upper clamp and a lower clamp, and adjusting the interior of the furnace to be a vacuum environment;
the preform was first preheated to 400 ℃ at a pressure of 20MPa, and then the sample was heated to 620 ℃ over 2 min;
then adjusting the temperature to 640 ℃ and keeping the temperature for 20min under the condition that the pressure is 40MPa, so that the preform is fully densified;
finally cooling at the speed of 20 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Texture of the skeleton Ti 3 AlC 2 A reinforced aluminum matrix composite.
FIG. 1 shows in-situ growth of TiAl obtained in example I 3 Texture Ti of skeleton 3 AlC 2 Microstructure photograph of the reinforced aluminum matrix composite. Wherein the bright color region is Ti 3 AlC 2 Particles, dark areas are Al matrix, gray areas are in-situ grown TiAl 3 The skeleton can be seen from the figure that the composite material has good compactness and only a small number of holes; in addition, ti 3 AlC 2 The particles are distributed in the composite material more uniformly without obvious agglomeration. The Ti3AlC2 particles are in the form of flat strips in the composite material and are oriented with the basal plane perpendicular to the sintering direction. TiAl3 and sheet Ti generated in situ 3 AlC 2 And mutually penetrate to form a skeleton structure. TiAl 3 The framework bonds well to the matrix and reinforcing phase.
EXAMPLE one resulting in-situ grown TiAl 3 Texture Ti of skeleton 3 AlC 2 The density of the particle reinforced aluminum-based composite material is 2.99g/cm 3 The compactness is 99.8 percent, the compressive yield strength is 355.7MPa, the compressive strength is 572.1MPa, and the tensile strength is 340.9MPa.
Claims (10)
1. In-situ growth TiAl 3 Texture of the skeleton Ti 3 AlC 2 Preparation method of reinforced aluminum-based composite materialThe method is characterized in that: growing TiAl in situ 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material comprises the following steps:
1. weighing material
Weighing 5-30% of Ti according to volume fraction 3 AlC 2 Powder and 95-70% aluminum metal powder;
the average diameter of the aluminum metal powder is 1-20 mu m;
the Ti 3 AlC 2 The average grain diameter of the powder is 15-60 mu m;
2. ti (titanium) 3 AlC 2 Breaking and sheet ball milling of powder
Ti weighed in the step one 3 AlC 2 Putting the powder into a ball milling tank for ball milling; the ball-material ratio is (8-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-20 h; by ball milling of Ti 3 AlC 2 Opening clusters, crushing particles and carrying out interlayer stripping to obtain sheet Ti with the thickness of 0.1-2 mu m and the diameter of 0.3-5 mu m 3 AlC 2 Particles;
3. sheet ball milling of aluminum metal powder
Putting the aluminum metal powder weighed in the step one into a ball milling tank for ball milling; the ball-material ratio is (5-15) to 1, the rotating speed is 300-450 rpm, and the ball milling time is 10-30 h; deforming the spherical aluminum metal particles by ball milling to obtain sheet aluminum metal particles with the thickness of 0.2-1.6 mu m and the diameter of 8-15 mu m;
4. flake Ti 3 AlC 2 Ball milling and mixing of powder and aluminum flake metal powder
The sheet Ti obtained in the second step 3 AlC 2 Putting the particles and the sheet aluminum metal particles obtained in the step three into a ball milling tank for ball milling and mixing; low-energy ball milling is adopted, the ball material ratio is (1-2): 1, the rotating speed is 150 rpm-200 rpm, the ball milling time is 1.5 h-3 h, the two particles are fully mixed, and finally the temperature is kept for 10 h-20 h in a vacuum furnace or protective atmosphere at 200 ℃ -300 ℃ to obtain the sheet Ti 3 AlC 2 And a composite powder of sheet aluminum metal;
5. ti (titanium) 3 AlC 2 Filling die of composite powder of aluminum and metal
The sheet Ti obtained in the step four 3 AlC 2 Uniformly pouring the composite powder of the flaky aluminum metal into a mold, fully vibrating the filled mold to ensure that the interior of the powder is uniform and the surface of the powder is smooth, and then cold pressing the powder; in the cold pressing process, the pressurizing speed is 0.1 mm/min-3 mm/min, the pressure is increased to 4 MPa-20 MPa, and the pressure is maintained for 5 min-10 min, so that the Ti with directional arrangement is obtained 3 AlC 2 And aluminum metal;
6. low temperature spark plasma sintering
Moving the composite preform obtained in the fifth step and the mold to a sintering chamber of a discharge plasma sintering furnace, assembling the mold by using an upper fixture and a lower fixture, and adjusting the interior of the furnace to be in a vacuum environment;
firstly, preheating a prefabricated body to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-620 ℃ within 1-5 min;
then adjusting the temperature to 450-640 ℃ and keeping the temperature for 10-20 min under the condition of the pressure of 20-300 MPa, so that the preform is fully densified;
finally cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Texture of the skeleton Ti 3 AlC 2 A reinforced aluminum matrix composite.
2. The in-situ grown TiAl of claim 1 3 Texture of the skeleton Ti 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: in the first step, the aluminum metal is pure aluminum or aluminum alloy.
3. The in-situ grown TiAl of claim 1 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: step one, the aluminum metal is one or a combination of more of Al-Si alloy, al-Si-Cu alloy, al-Cu-Mg alloy, al-Zn-Cu alloy, al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy.
4. The in-situ grown TiAl of claim 3 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: the mass fraction of Si in the Al-Si alloy is 2-25%; the mass fraction of Si in the Al-Si-Cu alloy is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Zn in the Al-Zn-Cu alloy is 0.5-55%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Zn in the Al-Zn-Mg-Cu alloy is 0.5-55%, the mass fraction of Mg is 0.5-38%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Cu-Mg alloy is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%.
5. The in-situ grown TiAl of claim 1 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: the Ti in the step one 3 AlC 2 The purity of (A) is more than 95%.
6. The in-situ grown TiAl of claim 1 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: stearic acid is used as a process control agent in the ball milling process in the second step, and the stearic acid is Ti 3 AlC 2 0.1 to 0.3 percent of the powder mass.
7. The in-situ grown TiAl of claim 1 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: in the ball milling process in the second step, the materials of the used milling pot and the milling ball are stainless steel, zirconia or tungsten carbide.
8. The in-situ grown TiAl of claim 1 3 SkeletonTexture Ti of 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: and step three, stearic acid is used as a process control agent in the ball milling process, and the stearic acid accounts for 0.25-0.5 percent of the mass of the aluminum metal powder.
9. The in-situ grown TiAl of claim 1 3 Texture of the skeleton Ti 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: and fifthly, the diameter of the inner wall of the die is 40-120 mm.
10. The in-situ grown TiAl of claim 1 3 Texture Ti of skeleton 3 AlC 2 The preparation method of the reinforced aluminum matrix composite material is characterized by comprising the following steps: the protective atmosphere in the fourth step is one of nitrogen, argon and helium; the pressure of the protective gas is 0.1MPa to 10MPa.
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