CN115386813A - In-situ growth TiAl 3 Ti of whisker 3 AlC 2 Preparation method of particle reinforced aluminum-based composite material - Google Patents
In-situ growth TiAl 3 Ti of whisker 3 AlC 2 Preparation method of particle 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 113
- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 60
- 239000002245 particle Substances 0.000 title claims abstract description 54
- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 46
- 239000011159 matrix material Substances 0.000 claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 15
- 239000010936 titanium Substances 0.000 claims description 106
- 239000000843 powder Substances 0.000 claims description 87
- 229910045601 alloy Inorganic materials 0.000 claims description 32
- 239000000956 alloy Substances 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 238000003825 pressing Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 229910017818 Cu—Mg Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- 229910001148 Al-Li alloy Inorganic materials 0.000 claims description 4
- 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
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910007565 Zn—Cu Inorganic materials 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 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
- 229910018134 Al-Mg Inorganic materials 0.000 claims description 2
- 229910018167 Al—Be Inorganic materials 0.000 claims description 2
- 229910018182 Al—Cu Inorganic materials 0.000 claims description 2
- 229910018467 Al—Mg Inorganic materials 0.000 claims description 2
- 229910018566 Al—Si—Mg Inorganic materials 0.000 claims description 2
- 229910018569 Al—Zn—Mg—Cu Inorganic materials 0.000 claims description 2
- 229910000952 Be alloy Inorganic materials 0.000 claims description 2
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 229910019086 Mg-Cu Inorganic materials 0.000 claims description 2
- 229910007981 Si-Mg Inorganic materials 0.000 claims description 2
- 229910008316 Si—Mg Inorganic materials 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 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
- 239000010959 steel Substances 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000011812 mixed powder Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 abstract 1
- 229910010039 TiAl3 Inorganic materials 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- KVFIJIWMDBAGDP-UHFFFAOYSA-N ethylpyrazine Chemical compound CCC1=CN=CC=N1 KVFIJIWMDBAGDP-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- C22C49/04—Light metals
- C22C49/06—Aluminium
-
- 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
Abstract
A preparation method of Ti3AlC2 particle reinforced aluminum matrix composite material with TiAl3 crystal whiskers growing in situ relates to a preparation method of aluminum matrix composite material. In order to solve the problem that the existing preparation process is difficult to ensure Ti simultaneously 3 AlC 2 The strength and the plasticity of the aluminum matrix composite material are enhanced. The invention uses Ti 3 AlC 2 Particles and aluminum metal are used as raw materials, and Ti is prepared by ball milling 3 AlC 2 Mixed powder of Ti and aluminum metal, and then sintering Ti by spark plasma 3 AlC 2 The particles are compounded with aluminum to finally prepare Ti 3 AlC 2 A particle-reinforced aluminum-based composite material; the reaction time is short, only 5 min-20 min, and the Al matrix does not need to be heated to liquid by adopting the spark plasma sintering methodPhase, therefore TiAl 3 The content of the phase is controllable; and the composite material has high preparation efficiency, good reliability and excellent comprehensive mechanical property. Effectively generating TiAl with different sizes and contents at the interface 3 The composite material prepared by the whisker has the characteristics of good interface bonding, good mechanical property, particularly plasticity, easy mechanical processing and the like.
Description
Technical Field
The invention relates to a preparation method of an aluminum matrix composite.
Background
The MAX phase is a ternary nano-layered compound, and the micro-layered structure endows the MAX phase with high damage tolerance, conductivity, excellent machinability, high modulus and high hardness, so that extensive research is obtained in recent years. In order to achieve high strength and high toughness of MAX phase reinforced aluminum matrix composites, good interfacial bonding between the MAX phase and the aluminum matrix is required. However, studies have shown that the reaction of the MAX phase with Al is difficult to control. Although the conventional solid phase method can inhibit the reaction of MAX phase and Al, the low temperature is not favorable for interface bonding, which can lead to the performance reduction of the composite material. Although the liquid phase method preparation is beneficial to interface reaction combination, the molten Al liquid reacts with MAX phase to generate a large amount of brittle phase, and the plasticity of the composite material is seriously reduced. Therefore, in order to obtain a MAX phase reinforced aluminum matrix composite material having high strength and high plasticity, it is necessary to promote interfacial bonding between the MAX phase and Al, and to suppress the generation of a large amount of brittle phase.
As a typicalMAX phase ceramics of Ti 3 AlC 2 Has excellent friction and wear resistance and high temperature oxidation resistance, and can be used as an ideal reinforcement of an aluminum matrix. At present, ti is used 3 AlC 2 The literature on reinforced aluminum matrix composites is also relatively rare. Wang et al prepared 40% volume fraction Ti using hot isostatic pressing 3 AlC 2 A reinforced pure aluminum composite material. When the sintering temperature exceeds 700 ℃, the composite material system can react to generate a large amount of TiAl 3 、Al 4 C 3 And TiC, the density of the composite material is only 96-98%. Wang et al prepared 20-30% volume fraction of Ti at 780 ℃ by hot pressing sintering 3 AlC 2 -TiAl 3 A reinforced pure aluminum composite material. TiAl 3 The in-situ generation of (A) enables the room temperature compressive strength of the composite material to be as high as 404MPa, but the compressive strain is only 12%. In the current literature reports, to increase Ti 3 AlC 2 Interfacial bonding with aluminum substrates, the preparation temperature is generally selected to be above the melting point of aluminum to form TiAl in situ 3 And (4) phase. But the high temperature causes TiAl 3 Resulting in a sharp decrease in the plasticity of the composite material.
Disclosure of Invention
The invention aims to solve the problem that the existing preparation process is difficult to ensure Ti 3 AlC 2 The problem of enhancing the strength and the plasticity of the aluminum-based composite material is solved, and the TiAl in-situ growth is provided 3 Ti of whisker 3 AlC 2 A preparation method of a particle reinforced aluminum matrix composite.
The invention grows TiAl in situ 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material comprises the following steps:
1. weighing material
Weighing 10-40% of Ti by volume fraction 3 AlC 2 Powder and 90-60% aluminum metal powder;
2. ti 3 AlC 2 Grading ball milling of powder and aluminum metal powder
Ti weighed in the step one 3 AlC 2 The powder and aluminum metal powder are filled into a ball milling tankPerforming ball milling; firstly, ball milling at a low rotating speed, wherein the ball-material ratio is (1-2) to 1, the rotating speed is 150-200 rpm, and the ball milling time is 1.5-3 h, so that the two kinds of powder are fully mixed; then ball milling is carried out at a high rotating speed, the ball-material ratio is (3-5): 1, the rotating speed is 250-400 rpm, the ball milling time is 1.5-3 h, so that Ti is obtained 3 AlC 2 Fully opening large particles or clusters under the action of ball milling; by means of ball milling 3 AlC 2 The powder and the aluminum metal powder are uniformly mixed and fully contacted to obtain Ti 3 AlC 2 And aluminum metal;
3. preparation of preforms
Ti obtained in the second step 3 AlC 2 Putting the composite powder of the aluminum metal and the titanium alloy into a die for cold pressing, wherein in the process of cold pressing, the pressing speed is 0.1-3 mm/min, the pressure is increased to 4-20 MPa, and the pressure is maintained for 5-10 min to obtain Ti 3 AlC 2 And aluminum metal;
4. spark plasma sintering
Ti obtained in the third step 3 AlC 2 And moving the composite prefabricated body of the aluminum metal and the die to a sintering chamber of a discharge plasma sintering furnace, assembling the die by using an upper clamp and a lower clamp, and in SPS sintering equipment under the protective atmosphere or vacuum condition:
firstly, preheating a preform to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-640 ℃ under the pressure of 20-300 MPa within 1-10 min;
then keeping the temperature at 450-640 ℃ and the pressure at 20-300 MPa for 5-20 min; fully densifying the preform;
finally, cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Ti of whisker 3 AlC 2 A particulate reinforced aluminum matrix composite.
The invention has the following beneficial effects:
1. the invention uses Ti 3 AlC 2 Particles and aluminum metal are used as raw materials, and Ti is prepared by ball milling 3 AlC 2 Mixed powder of Ti and aluminum metal, and then sintering Ti by spark plasma 3 AlC 2 The particles are compounded with aluminum to finally prepare Ti 3 AlC 2 A particle-reinforced aluminum-based composite material; the reaction time is short, only 5-20 min, and the Al substrate does not need to be heated to a liquid phase by adopting the spark plasma sintering method, so that TiAl 3 The content of the phase is controllable; and the composite material has high preparation efficiency, good reliability and excellent comprehensive mechanical property.
2. The invention provides an in-situ grown TiAl 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum-based composite material can realize Ti by controlling the heating rate, temperature and heat preservation time of spark plasma sintering 3 AlC 2 The reinforced aluminum-based composite material is fully densified in a short time, the interface reaction degree can be effectively controlled, and Ti is enabled to be reacted at a high temperature 3 AlC 2 And the elements of the Al matrix interdiffuse. Ti 3 AlC 2 The Ti element in the crystal is dislocated and diffused into the Al matrix. Because of the high Al concentration of the substrate, tiAl is generated by the reaction with Al 3 . With the diffusion of Ti element, tiAl 3 Gradually grows into an Al matrix, and TiAl with different sizes and contents is effectively generated at the interface 3 The composite material prepared by the whisker has the characteristics of good interface bonding, good mechanical property, particularly plasticity, easy mechanical processing and the like.
3. The TiAl prepared by the invention grows in situ 3 Ti of whisker 3 AlC 2 Ti in particle reinforced aluminum-based composite material 3 AlC 2 The content of the particles is 10 to 40 percent, and TiAl 3 The diameter of the whisker is 40 nm-1000 nm; the density of the composite material is 2.84g/cm 3 ～3.32g/cm 3 The density is more than 98 percent, the elastic modulus is between 80GPa and 150GPa, the bending strength is between 400MPa and 800MPa, the yield strength is between 60MPa and 300MPa, the tensile strength is between 120MPa and 400MPa, and the elongation is between 1 percent and 20 percent.
4. The invention provides a method for preparing Ti rapidly and efficiently 3 AlC 2 The mode of reinforcing the aluminum matrix composite material has simple preparation method, safety and easy operation,Easy control of the process, low density and high compactness of the composite material, ti 3 AlC 2 The particles are uniformly distributed, and the industrial production and application are favorably realized.
Drawings
FIG. 1 shows the in-situ grown TiAl obtained in example one 3 Ti of whisker 3 AlC 2 A microstructure photograph of the particle-reinforced aluminum-based composite material;
FIG. 2 shows in-situ growth of TiAl obtained in example I 3 Ti of whisker 3 AlC 2 Interface TiAl of particle reinforced aluminum-based composite material 3 Transmission pictures of whiskers.
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 embodiment is as follows: the embodiment grows TiAl in situ 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material comprises the following steps:
1. weighing material
Weighing 10-40% of Ti according to volume fraction 3 AlC 2 Powder and 90-60% aluminum metal powder;
2. ti 3 AlC 2 Grading ball milling of powder and aluminum metal powder
Ti weighed in the step one 3 AlC 2 Putting the powder and aluminum metal powder into a ball milling tank for ball milling; firstly, ball milling at a low rotating speed, wherein the ball-material ratio is (1-2) to 1, the rotating speed is 150-200 rpm, and the ball milling time is 1.5-3 h, so that the two kinds of powder are fully mixed; then ball milling is carried out at a high rotating speed, the ball-material ratio is (3-5): 1, the rotating speed is 250-400 rpm, the ball milling time is 1.5-3 h, so that Ti is obtained 3 AlC 2 Fully opening large particles or clusters under the action of ball milling; by means of ball milling 3 AlC 2 The powder and aluminum metal powder are uniformly mixed and fully contacted to obtain Ti 3 AlC 2 And aluminum metal;
3. preparation of preforms
Ti obtained in the second step 3 AlC 2 Putting the composite powder with the aluminum metal into a die for cold pressing, wherein in the process of cold pressing, the pressing speed is 0.1-3 mm/min, the pressure is increased to 4-20 MPa, and the pressure is maintained for 5-10 min to obtain Ti 3 AlC 2 And aluminum metal;
4. spark plasma sintering
Ti obtained in the third step 3 AlC 2 And moving the composite prefabricated body of the aluminum metal and the die to a sintering chamber of a discharge plasma sintering furnace, assembling the die by using an upper clamp and a lower clamp, and in SPS sintering equipment under the condition of protective atmosphere or vacuum:
firstly, preheating a preform to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-640 ℃ under the pressure of 20-300 MPa within 1-10 min;
then keeping the temperature at 450-640 ℃ and the pressure at 20-300 MPa for 5-20 min; fully densifying the preform;
finally, cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Ti of whisker 3 AlC 2 A particulate reinforced aluminum matrix composite.
The embodiment has the following beneficial effects:
1. the present embodiment uses Ti 3 AlC 2 Particles and aluminum metal are used as raw materials, and Ti is prepared by ball milling 3 AlC 2 Mixed powder of Ti and aluminum metal, and then sintering Ti by spark plasma 3 AlC 2 The particles are compounded with aluminum to finally prepare Ti 3 AlC 2 A particle-reinforced aluminum-based composite material; the reaction time is short, only 5-20 min, and the Al substrate does not need to be heated to a liquid phase by adopting the spark plasma sintering method, so that TiAl 3 The content of the phase is controllable; and the composite material has high preparation efficiency, good reliability and excellent comprehensive mechanical property.
2. The embodiment provides an in-situ growth TiAl 3 Ti of whisker 3 AlC 2 Particle reinforcementThe preparation method of the aluminum-based composite material not only can realize Ti through controlling the heating rate, the temperature and the heat preservation time of the spark plasma sintering 3 AlC 2 The reinforced aluminum-based composite material is fully densified in a short time, the interface reaction degree can be effectively controlled, and Ti is enabled to be reacted at a high temperature 3 AlC 2 And the elements of the Al matrix are diffused mutually. Ti (titanium) 3 AlC 2 The Ti element in the crystal is dislocated and diffused into the Al matrix. Because the Al concentration of the substrate is very high, tiAl is generated by the reaction with Al 3 . With the diffusion of Ti element, tiAl 3 Gradually grows into an Al matrix, and TiAl with different sizes and contents is effectively generated at an interface 3 The composite material prepared by the whisker has the characteristics of good interface bonding, good mechanical property, particularly plasticity, easy mechanical processing and the like.
3. In-situ grown TiAl prepared by the embodiment 3 Ti of whisker 3 AlC 2 Ti in particle reinforced aluminum-based composite material 3 AlC 2 The content of the particles is 10 to 40 percent, and TiAl 3 The diameter of the whisker is 40 nm-1000 nm; the density of the composite material is 2.84g/cm 3 ～3.32g/cm 3 The compactness is more than 98 percent, the elastic modulus is between 80GPa and 150GPa, the bending strength is between 400MPa and 800MPa, the yield strength is between 60MPa and 300MPa, the tensile strength is between 120MPa and 400MPa, and the elongation is between 1 percent and 20 percent.
4. The embodiment provides a method for preparing Ti rapidly and efficiently 3 AlC 2 The mode of reinforcing the aluminum-based composite material has the advantages of simple preparation method, safety, easy operation, easy control of process, low density and high density of the composite material, and Ti 3 AlC 2 The particles are uniformly distributed, and the industrialized production and application are favorably realized.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the Ti in the step one 3 AlC 2 The purity of (2) is more than 95%; the Ti 3 AlC 2 The average particle diameter of the powder is 0.2-40 μm.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the average diameter of the aluminum metal powder in the first step is 1-30 μm.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is: in the first step, the aluminum metal powder is pure aluminum or aluminum alloy powder.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the aluminum alloy powder is one or a combination of more of Al-Si alloy, al-Cu alloy, al-Mg alloy, al-Si-Cu alloy, al-Si-Mg alloy, al-Cu-Mg alloy, al-Zn-Cu alloy, al-Zn-Mg-Cu alloy, al-Be alloy, al-Li alloy and Al-Si-Cu-Mg alloy; the mass fraction of Si in the Al-Si alloy powder is 0.5-25%; the mass fraction of Cu in the Al-Cu alloy powder is 0.5-53%; the mass fraction of Mg in the Al-Mg alloy powder is 0.5-38%; the mass fraction of Si in the Al-Si-Cu alloy powder is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Mg alloy powder is 0.5-25%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Cu in the Al-Cu-Mg alloy powder 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 powder 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 powder 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 Be in the Al-Be alloy powder is 0.5-20%; the mass fraction of Li in the Al-Li alloy powder is 0.5-35%; the mass fraction of Al-Si-Cu-Mg alloy Si is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%.
The sixth specific implementation mode is as follows: the difference between this embodiment and one of the first to fifth embodiments is: and the material of the grinding pot and the grinding ball used in the ball milling process in the step two is alumina, zirconia or tungsten carbide.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the diameter of the inner wall of the die in the third step is 40 mm-120 mm.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the mould in the third step is a graphite mould or a steel mould.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the protective atmosphere in the fourth step is one of nitrogen, argon, helium and the like.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: in the fourth step, the pressure of the protective atmosphere is 0.1 MPa-10 MPa.
The first embodiment is as follows: example an in situ grown TiAl 3 Ti of whisker 3 AlC 2 The preparation method of the particle 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 95%; ti 3 AlC 2 The particle size range of the powder is 1-36 mu m, and the average particle size is 9.6 mu m; the aluminum metal powder is pure Al; the particle size range of the aluminum metal powder is 3-10.6 mu m, and the average particle size is 4.5 mu m;
2. ti 3 AlC 2 Homogenization of powder and aluminum metal powder
Ti weighed in the step one 3 AlC 2 Putting the powder and aluminum metal powder into a ball milling tank for ball milling; firstly, ball milling at a low rotation speed, wherein the ball-material ratio is 1; then ball milling is carried out at a high rotating speed, the ball-material ratio is 3, the rotating speed is 300rpm, and the ball milling time is 1.5h, so that Ti 3 AlC 2 Large particles or clusters are fully opened under the action of ball milling; by means of ball milling 3 AlC 2 The powder and the aluminum metal powder are uniformly mixed and fully contacted to obtain Ti 3 AlC 2 And aluminum metal; the material of the grinding pot and the grinding ball used in the ball milling process is alumina;
3. preparation of the preform
Ti obtained in the second step 3 AlC 2 Graphite is filled with composite powder of aluminum metalCold pressing is carried out in the die, and the diameter of the inner wall of the graphite die is 100mm; in the cold pressing process, the pressurizing speed is 0.5mm/min, the pressure is increased to 5MPa and maintained for 5min, and Ti is obtained 3 AlC 2 And aluminum metal;
4. spark plasma sintering
Ti obtained in the third step 3 AlC 2 And moving the composite prefabricated body of the aluminum metal and the die to a sintering chamber of a discharge plasma sintering furnace, assembling the die by using an upper clamp and a lower clamp, and in SPS sintering equipment under the vacuum condition:
first, the preform was preheated to 400 ℃ at a pressure of 40MPa, then the sample was heated to 620 ℃ at a pressure of 40MPa and within 1.5 min;
then, the preform is kept for 10min at the temperature of 620 ℃ and the pressure of 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 the TiAl in-situ growth 3 Ti of whisker 3 AlC 2 A particle-reinforced aluminum-based composite material;
FIG. 1 shows the in-situ grown TiAl obtained in example one 3 Ti of whisker 3 AlC 2 A microstructure photograph of the particle reinforced aluminum matrix composite; as can be seen from FIG. 1, the composite material has good compactness and only a few holes; in addition, ti 3 AlC 2 The particles are distributed in the composite material more uniformly without obvious agglomeration; FIG. 2 shows in-situ growth of TiAl obtained in example I 3 Ti of whisker 3 AlC 2 TiAl at interface of particle reinforced aluminum-based composite material 3 Transmission pictures of whiskers; from FIG. 2, it can be seen that TiAl 3 The diameter of the whisker of (2) is 78nm; tiAl 3 The combination of the whisker, the matrix and the reinforcing phase is good; EXAMPLE one resulting in situ grown TiAl 3 Ti of whisker 3 AlC 2 The density of the particle reinforced aluminum-based composite material is 3.02g/cm 3 The compactness is 100 percent, the elastic modulus is 92GPa, the yield strength is 104MPa, the tensile strength is 180MPa, and the elongation is 17.5 percent.
The second embodiment:
example an in situ grown TiAl 3 Ti of whisker 3 AlC 2 The preparation method of the particle 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 95%; ti (titanium) 3 AlC 2 The particle size range of the powder is 10-36 mu m, and the average particle size is 14.5 mu m; the aluminum metal powder is Al-Cu-Mg alloy; the mass fraction of Cu in the Al-Cu-Mg alloy is 4.2%, and the mass fraction of Mg is 1.6%; the particle size range of the aluminum metal powder is 10-25 mu m, and the average particle size is 16.8 mu m;
2. ti 3 AlC 2 Homogenization of powder and aluminum metal powder
Ti weighed in the step one 3 AlC 2 Putting the powder and aluminum metal powder into a ball milling tank for ball milling; firstly, adopting low rotation speed, the ball-material ratio of 1 to 1, the rotation speed of 150rpm and the ball milling time of 1.5h to fully mix the two kinds of powder; then, adopting a high rotating speed, a ball-material ratio of 5 to 1, a rotating speed of 250rpm and ball milling time of 3.5h to ensure that Ti 3 AlC 2 Large particles or clusters are fully opened under the action of ball milling; by means of ball milling 3 AlC 2 The powder and aluminum metal powder are uniformly mixed and fully contacted to obtain Ti 3 AlC 2 And aluminum metal; the material of the grinding pot and the grinding ball used in the ball milling process is alumina;
3. preparation of preforms
Ti obtained in the second step 3 AlC 2 Putting the composite powder of the aluminum metal and the graphite mould into the graphite mould for cold pressing, wherein the diameter of the inner wall of the graphite mould is 60mm; in the cold pressing process, the pressurizing speed is 0.5mm/min, the pressure is increased to 5MPa and maintained for 5min, and Ti is obtained 3 AlC 2 And aluminum metal;
4. spark plasma sintering
Ti obtained in the third step 3 AlC 2 And the composite preform of aluminum metal is moved to the place together with the moldIn a sintering chamber of an electric plasma sintering furnace, a mould is assembled by an upper fixture and a lower fixture, and in SPS sintering equipment under the vacuum condition:
first, the preform was preheated to 400 ℃ at a pressure of 40MPa, followed by heating the sample to 500 ℃ at a pressure of 40MPa and within 2 min;
then, the preform is kept for 10min at the temperature of 500 ℃ and the pressure of 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 the TiAl in-situ growth 3 Ti of whisker 3 AlC 2 A particulate reinforced aluminum matrix composite.
Example two in situ growth of TiAl 3 Ti of whisker 3 AlC 2 The density of the particle reinforced aluminum-based composite material is 3.05g/cm 3 The compactness is 100 percent, the elastic modulus is 108GPa, the yield strength is 216MPa, the tensile strength is 382MPa, and the elongation is 8.2 percent.
Claims (10)
1. TiAl in-situ growth 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: growing TiAl in situ 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material comprises the following steps:
1. weighing material
Weighing 10-40% of Ti by volume fraction 3 AlC 2 Powder and 90-60% aluminum metal powder;
2. ti (titanium) 3 AlC 2 Grading ball milling of powder and aluminum metal powder
Ti weighed in the step one 3 AlC 2 Putting the powder and aluminum metal powder into a ball milling tank for ball milling; firstly, ball milling at a low rotating speed, wherein the ball-material ratio is (1-2) to 1, the rotating speed is 150-200 rpm, and the ball milling time is 1.5-3 h, so that the two kinds of powder are fully mixed; then ball milling is carried out at a high rotating speed, the ball-material ratio is (3-5): 1, the rotating speed is 250-400 rpm, the ball milling time is 1.5-3 h, so that Ti is obtained 3 AlC 2 Large particles or clusters under the action of ball millingFully opening; by means of ball milling 3 AlC 2 The powder and aluminum metal powder are uniformly mixed and fully contacted to obtain Ti 3 AlC 2 And aluminum metal;
3. preparation of the preform
Ti obtained in the second step 3 AlC 2 Putting the composite powder with the aluminum metal into a die for cold pressing, wherein in the process of cold pressing, the pressing speed is 0.1-3 mm/min, the pressure is increased to 4-20 MPa, and the pressure is maintained for 5-10 min to obtain Ti 3 AlC 2 And aluminum metal;
4. spark plasma sintering
Ti obtained in the third step 3 AlC 2 And moving the composite prefabricated body of the aluminum metal and the die to a sintering chamber of a discharge plasma sintering furnace, assembling the die by using an upper clamp and a lower clamp, and in SPS sintering equipment under the condition of protective atmosphere or vacuum:
firstly, preheating a prefabricated body to 300-400 ℃ under the pressure of 20-300 MPa, and then heating a sample to 450-640 ℃ under the pressure of 20-300 MPa within 1-10 min;
then keeping the temperature at 450-640 ℃ and the pressure at 20-300 MPa for 5-20 min; fully densifying the preform;
finally, cooling at the speed of 20-40 ℃/min, demoulding after cooling to obtain a sintered block, namely growing TiAl in situ 3 Ti of whisker 3 AlC 2 A particulate reinforced aluminum matrix composite.
2. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the Ti in the step one 3 AlC 2 The purity of (2) is more than 95%; the Ti 3 AlC 2 The average particle diameter of the powder is 0.2-40 μm.
3. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: in the first step, the average diameter of the aluminum metal powder is 1-30 μm.
4. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: in the first step, the aluminum metal powder is pure aluminum or aluminum alloy powder.
5. The in-situ grown TiAl of claim 4 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the aluminum alloy powder is one or a combination of more of Al-Si alloy, al-Cu alloy, al-Mg alloy, al-Si-Cu alloy, al-Si-Mg alloy, al-Cu-Mg alloy, al-Zn-Cu alloy, al-Zn-Mg-Cu alloy, al-Be alloy, al-Li alloy and Al-Si-Cu-Mg alloy; the mass fraction of Si in the Al-Si alloy powder is 0.5-25%; the mass fraction of Cu in the Al-Cu alloy powder is 0.5-53%; the mass fraction of Mg in the Al-Mg alloy powder is 0.5-38%; the mass fraction of Si in the Al-Si-Cu alloy powder is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Mg alloy powder is 0.5-25%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Cu in the Al-Cu-Mg alloy powder 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 powder 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 powder 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 Be in the Al-Be alloy powder is 0.5-20%; the mass fraction of Li in the Al-Li alloy powder is 0.5-35%; the mass fraction of Al-Si-Cu-Mg alloy Si is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%.
6. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: and the material of the grinding pot and the grinding ball used in the ball milling process in the step two is alumina, zirconia or tungsten carbide.
7. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the diameter of the inner wall of the die in the third step is 40 mm-120 mm.
8. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the mould in the third step is a graphite mould or a steel mould.
9. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the protective atmosphere in the fourth step is one of nitrogen, argon, helium and the like.
10. The in-situ grown TiAl of claim 1 3 Ti of whisker 3 AlC 2 The preparation method of the particle reinforced aluminum matrix composite material is characterized by comprising the following steps: the pressure of the protective atmosphere in the fourth step is 0.1 MPa-10 MPa.
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| CN115679229A (en) * | 2022-12-12 | 2023-02-03 | 西安稀有金属材料研究院有限公司 | Potassium titanate whisker reinforced aluminum matrix composite material and preparation method thereof |
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| WO2009072834A2 (en) * | 2007-12-07 | 2009-06-11 | Korea Institute Of Science And Technology | Ti3alc2 composite materials with high strength and method of manufacturing the same |
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| CN115679229A (en) * | 2022-12-12 | 2023-02-03 | 西安稀有金属材料研究院有限公司 | Potassium titanate whisker reinforced aluminum matrix composite material and preparation method thereof |
| CN115679229B (en) * | 2022-12-12 | 2023-11-17 | 西安稀有金属材料研究院有限公司 | Potassium titanate whisker reinforced aluminum matrix composite material and preparation method thereof |
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