CN117512378A - Ultrahigh-toughness aluminum-based composite material and preparation method thereof - Google Patents
Ultrahigh-toughness aluminum-based composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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Abstract
The invention discloses an ultrahigh-toughness aluminum-based composite material and a preparation method thereof, wherein the method comprises the following steps: s1, preparing aluminum-based alloy powder A with partial amorphization by adopting an ultrasonic gas atomization method; s2, mixing pure metal powder and boron powder according to the atomic percentage of the AlNiTiZr aluminum-based amorphous alloy, adding a dispersing agent, and preparing powder B by adopting a mechanical alloying method; s3, uniformly mixing the powder A, B obtained in the steps S1 and S2, and then performing spark plasma sintering; s4, carrying out hot extrusion forming and heat treatment on the sintered material to obtain the ultrahigh-strength and high-toughness aluminum-based composite material; s1, the cooling speed is more than or equal to 10 5 K/s. The ultrahigh-strength and high-toughness aluminum-based composite material has the yield strength of about 700-800 MPa and the tensile strength of about 800-900 MPaThe elongation is 5-12%, and the toughness is far better than that of the existing high-toughness aluminum alloy material.
Description
Technical Field
The invention belongs to the field of aluminum-based composite materials, and particularly relates to an ultrahigh-toughness aluminum-based composite material and a preparation method thereof.
Background
With the promotion of strategic targets of carbon peak reaching, carbon neutralization energy conservation and emission reduction, the new high-specific strength and ultrahigh-strength and high-toughness aluminum-based composite material is in an industry burst period. Aluminum is used for replacing steel, and aluminum is used for replacing titanium to form an important development direction of high-performance aluminum alloy and aluminum-based composite materials. The aluminum-based composite material is prepared by adding ceramic reinforcing phase (SiC, al) into aluminum matrix by stirring casting, powder metallurgy and other methods 2 O 3 Etc.), has more outstanding specific strength, specific rigidity, wear resistance and other characteristics than the traditional aluminum alloy, and is widely applied to aerospace, traffic, weapons and other equipment. For example, countries such as America, japanese, english, etc. developed SiC/Al, B/Al and Al 2 O 3 Al-based composite material, and can be applied to the parts of engine pistons, aircraft bodies, wings, rudders, skins and the like. However, because of adverse reaction of a matrix-reinforced phase interface, difficult regulation and control of the content and uniform distribution of the reinforced phase and the like, the strength of the aluminum-based composite material is still limited, the strength is about 500MPa, the aluminum-based composite material is equivalent to 7000 series precipitation hardening aluminum alloy, the cost is high, and the toughness of the material is difficult to be compatible.
In the existing method, although the in-situ endogenetic precipitation strengthening phase obtained by the stirring casting method solves the problems of uniform dispersion, tissue refinement and the like of the strengthening phase, the strengthening and toughening level of the aluminum-based composite material reaches a higher degree, but the content of the ceramic phase can still be controlled at a lower level, the high content is easy to agglomerate, the material performance is reduced, and the fact that the prepared aluminum-based composite material reaches the strength limit is determined, and the further improvement is difficult. Although the powder metallurgy method is convenient for designing powder components, the problems of interface adverse reaction, coarsening of crystal structure, insufficient sintering density and the like often exist, and the matrix materials are mostly conventional gas atomization or water atomization aluminum alloy powder, so that the surface oxygen content is high, and the formation of sintering necks in the powder metallurgy is not facilitated.
Therefore, the preparation of aluminum-based composite materials with higher strength and toughness is one of the bottleneck problems in industry development. How to obtain the design and the preparation of the ultrahigh-strength and high-toughness aluminum-based composite material with the tensile strength exceeding 800MPa and the elongation rate still kept 10 percent, the realization of low-cost and light-weight manufacturing of important equipment by replacing steel with aluminum and replacing titanium with aluminum is truly realized, and the further exploration and the research are needed.
Disclosure of Invention
Based on the technical problems, the invention provides the ultrahigh-toughness aluminum-based composite material and the preparation method thereof on the basis of the existing powder metallurgy technology, and the ultrahigh-toughness aluminum-based composite material with the tensile strength exceeding 800MPa and the elongation percentage kept about 10% can be obtained.
The specific scheme of the invention is as follows:
the invention aims at providing a preparation method of the ultrahigh-toughness aluminum-based composite material, which comprises the following steps: s1, preparing aluminum-based alloy powder A with partial amorphization by adopting an ultrasonic gas atomization method; s2, mixing pure metal powder and boron powder according to the atomic percentage of the AlNiTiZr aluminum-based amorphous alloy, adding a dispersing agent, and preparing powder B by adopting a mechanical alloying method; s3, uniformly mixing the powder A, B obtained in the steps S1 and S2, and then performing spark plasma sintering; s4, carrying out hot extrusion forming and heat treatment on the sintered material to obtain the ultrahigh-strength and high-toughness aluminum-based composite material; s1, the cooling speed is more than or equal to 10 5 K/s。
Preferably, in S1, the aluminum-based alloy is 7000-series aluminum alloy; more preferably, the aluminum-based alloy is selected from any one of 7075 aluminum alloy, 7055 aluminum alloy, al-10Zn-3.5Mg-1.5 Cu.
Preferably, in S1, the partially amorphized aluminum-based alloy powder A contains a surface oxide layer having a thickness of 1-5 nm.
The method is suitable for any aluminum-based alloy, and the toughness can be greatly improved by taking any aluminum alloy as a base material by adopting the method. The 7000-series aluminum alloy is preferable in the present invention because 7000-series aluminum alloy itself is more excellent in performance, and on this basis, an ultrahigh strength and toughness aluminum-based composite material having a tensile strength of 800MPa or more and an elongation of about 10% can be obtained.
The invention adopts the ultrasonic gas atomization method, and the cooling speed is more than or equal to 10 5 The partially amorphous aluminum-based alloy powder A can be prepared under the K/s (ultra-fast cooling) condition, the surface of the powder A is provided with an extremely thin oxide film, the activity is high, the components are not segregated, and the amorphous content in the powder A can be regulated and controlled by controlling the cooling speed.
Preferably, in S2, the boron powder is added in an amount of 1:2-3 by mole of Ti in the AlNiTiZr-based aluminum-based amorphous alloy.
Preferably, in S2, the dispersant is stearic acid or sodium stearate; the addition amount of the dispersing agent is 1-3wt.% of the total amount of the pure metal powder and the boron powder.
Preferably, in S2, the mechanical alloying method is a ball milling method, specifically, ball milling is carried out under inert atmosphere, the ball-to-material ratio is 10-20:1, the ball milling rotating speed is 300-600r/min, and the ball milling time is 50-80h.
The AlNiTiZr-series aluminum-based amorphous alloy has a wide supercooled liquid phase region, and a certain amount of boron powder is added in the step S2, and the AlNiTiZr-series aluminum-based amorphous alloy has the function of being capable of reacting with Ti in the aluminum-based amorphous alloy in situ to generate endogenous TiB 2 The nanophase further serves as reinforcement.
Preferably, in S3, powder B is added in an amount of 1-40wt.% of the total amount of powder A, B.
Preferably, in S3, powder A, B is mixed by a low-energy ball milling method, wherein the ball milling rotating speed is 100-300r/min, and the ball milling time is 100-300min.
Preferably, in S3, the spark plasma sintering process includes: adding A, B mixed powder into a graphite mold, slowly applying pressure to 25MPa on the graphite mold under vacuum and room temperature conditions, and maintaining the pressure for 5min; heating to 200 ℃, synchronously applying pressure to 50MPa, and preserving heat and pressure for 5min; heating to 400 ℃, maintaining the pressure at 50MPa, and preserving heat and pressure for 3min; heating to 450 ℃, maintaining the pressure at 50MPa, and preserving heat and pressure for 5min; finally, the temperature is raised to 500 ℃, the pressure is maintained at 50MPa, and the temperature and pressure are maintained for 5min.
The step S3 of the invention adopts a spark plasma sintering process, and the sintering process can play the combined roles of particle discharge, conductive heating and pressurization. Besides the two factors of heating and pressurizing for promoting sintering, the plasma generated by the pulse current can enable particles in the sintering body to generate Joule heat, so that the surface is locally melted and surface substances are peeled off, and sputtering and discharging impact of high-temperature plasma clearly enable impurities and adsorbed gas on the surface of powder particles, so that diffusion is promoted, low-temperature rapid sintering is realized, and the density of the powder particles is improved. The invention adopts a spark plasma sintering process, and can obtain ultrafine crystals by sintering at low temperature, thereby obtaining the ultrahigh strength and toughness aluminum-based composite material.
Preferably, in S4, the hot extrusion temperature is 400-500 ℃, the extrusion ratio is 4-16:1, and the extrusion speed is 0.1-5mm/S; the heat treatment is a T6 heat treatment process.
The second object of the invention is to provide an ultrahigh-toughness aluminum-based composite material, which is prepared by adopting any one of the methods.
The invention has the beneficial effects that:
the invention combines the high activity, high uniformity and partial amorphization characteristics of the ultra-fast cooling aluminum alloy powder, combines the in-situ reaction strengthening of powder metallurgy, realizes the multi-dimensional composite strengthening of amorphous/nanocrystalline/endogenous precipitation in the sintering process by controlling the alloy components and the spark plasma sintering process and the hot extrusion and heat treatment technology, and can obtain the light structural material of the standard titanium alloy and the high-strength steel. The yield strength of the ultrahigh-strength high-toughness aluminum-based composite material is about 700-800 MPa, the tensile strength is about 800-900 MPa, the elongation is 5-12%, and the toughness is far better than that of the existing high-strength high-toughness aluminum alloy material.
Drawings
Fig. 1 is an SEM image of the partially amorphized aluminum alloy powder a obtained in example 1 at different magnification:
FIG. 2 is a micrograph of powder B obtained in example 1, wherein (a) is the SEAD profile; (b) is a TEM image;
FIG. 3 is an EBSD of the ultra high strength and toughness aluminum matrix composite obtained in example 1;
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
An ultrahigh-toughness aluminum-based composite material, the preparation method of which comprises the following steps:
s1, preparing aluminum-based alloy powder A with partial amorphization
Ultrasonic gas atomization equipment is adopted, and the cooling speed is controlled to be more than or equal to 10 5 K/s, after melting 7055 aluminum alloy, guiding the melted 7055 aluminum alloy to the inner wall of a tubular resonator excited by ultrasonic frequency, and breaking the melted 7055 aluminum alloy by vibration tension wave atomization; meanwhile, nitrogen is introduced to generate unsteady shock waves, and pressure pulses further break up droplets atomized by tension waves to obtain a part of amorphous aluminum alloy powder A with a surface oxide layer of 2 nm;
SEM images of the partially amorphized aluminum-based alloy powder a obtained in this example S1 at different times are shown in fig. 1, and it can be seen from fig. 1 (a) that the powder a is a spherical powder; FIG. 1 (b) shows that the powder A has an extremely thin oxide layer of 2-3nm on the surface;
s2, preparing powder B
According to the atomic percentage of Al76Ni8Ti8Zr4Y4 aluminum alloy, mixing pure Al powder, ni powder, ti powder, zr powder and Y powder with boron powder, adding dispersing agent sodium stearate accounting for 2wt.% of the total amount of pure metal powder and boron powder, and preparing powder B by adopting a ball milling method; wherein, the adding amount of the boron powder is calculated by the mole amount of Ti in Al76Ni8Ti8Zr4Y4 aluminum alloy, and the mole ratio of Ti to B is 1:2. The ball milling method specifically comprises the following steps:
selecting GCr15 bearing steel balls, controlling the ball-material ratio to be 10:1, and mixing and lapping four grinding balls with diameters of 20mm, 12mm, 10mm and 5mm, wherein the number ratio of the grinding balls is 1:5:38:10; the rotation speed of the ball mill is 400r/min, under the protection of argon, the ball mill is stopped for 30min every 2h to prevent powder from overheating, and the ball milling time is 80h;
the micrograph of powder B obtained in this example S2 is shown in FIG. 2;
s3, SPS sintering
Uniformly mixing powder B obtained by powder A, S2 obtained by the step S1 by adopting a low-energy ball milling method, wherein the addition amount of the powder B is 5wt.% of the total amount of the powder A, B; the mixed powder is put into a graphite die for SPS sintering, and the specific sintering process is as follows:
(1) slowly applying pressure to 25MPa on the graphite mold under the conditions of vacuum and room temperature, and maintaining the pressure for 5min;
(2) heating to 200 ℃, synchronously applying pressure to 50MPa, and preserving heat and pressure for 5min;
(3) heating to 400 ℃, maintaining the pressure at 50MPa, and preserving heat and pressure for 3min;
(4) heating to 450 ℃, maintaining the pressure at 50MPa, and preserving heat and pressure for 5min;
(5) finally, heating to 500 ℃, maintaining the pressure at 50MPa, and preserving heat and pressure for 5min;
s4, hot extrusion forming and heat treatment
Controlling the hot extrusion temperature at 420 ℃, the extrusion ratio at 9:1, and the extrusion speed at 0.5mm/s; and then adopting a T6 heat treatment method, namely carrying out solution treatment on the hot extrusion sample after heat preservation for 120min at 470 ℃, and then carrying out aging treatment at 120 ℃/24h to obtain the ultrahigh-strength and high-toughness aluminum-based composite material.
The EBSD diagram of the ultrahigh-toughness aluminum-based composite material finally obtained in the embodiment is shown in figure 3.
Example 2
An ultrahigh-toughness aluminum-based composite material, the preparation method of which comprises the following steps:
s1, preparing aluminum-based alloy powder A with partial amorphization
Ultrasonic gas atomization equipment is adopted, and the cooling speed is controlled to be more than or equal to 10 5 K/s, after Al-10Zn-3.5Mg-1.5Cu aluminum alloy is melted, guiding the melted Al-10Zn-3.5Mg-1.5Cu aluminum alloy to the inner wall of the tubular resonator excited by ultrasonic frequency, and breaking the melted Al-10Zn-3.5Mg-1.5Cu aluminum alloy by vibration tension wave atomization; at the same time, nitrogen is introduced to generate unsteady shock wave, and pressure pulse further breaks up tension wave fogMelting to obtain aluminum alloy powder A with a surface oxide layer of 2nm and partial amorphization;
s2, preparing powder B
According to the atomic percentage of Al70Ni10Ti10Zr5Ta5 aluminum alloy, mixing pure Al powder, ni powder, ti powder, zr powder, ta powder and boron powder, adding dispersing agent sodium stearate accounting for 2wt.% of the total amount of pure metal powder and boron powder, and preparing powder B by adopting a ball milling method; wherein, the adding amount of the boron powder is calculated by the mole amount of Ti in Al70Ni10Ti10Zr5Ta5 aluminum alloy, and the mole ratio of Ti to B is 1:2. The specific parameters of the ball milling method are the same as those of the example 1;
s3, SPS sintering
Uniformly mixing powder B obtained by powder A, S2 obtained by the step S1 by adopting a low-energy ball milling method, wherein the addition amount of the powder B is controlled to be 5wt.% of the total amount of the powder A, B; placing the mixed powder into a graphite mold for SPS sintering, wherein the specific sintering process is the same as that of the embodiment 1;
s4, hot extrusion forming and heat treatment
Controlling the hot extrusion temperature at 450 ℃, the extrusion ratio at 9:1 and the extrusion speed at 0.3mm/s; and then adopting a T6 heat treatment method, namely carrying out solution treatment on the hot extrusion sample after heat preservation for 120min at 500 ℃, and then carrying out aging treatment at 120 ℃/24h to obtain the ultrahigh-strength and high-toughness aluminum-based composite material.
Comparative example 1
An aluminum-based composite material, the preparation method of which comprises the following steps:
(1) Preparing amorphous aluminum-based alloy powder A: the same as S1 of example 1;
(2) Preparation of powder B: the same as S2 of example 1;
(3) Uniformly mixing powder A and powder B by adopting a low-energy ball milling method, wherein the addition amount of the powder B is controlled to be 5 wt%; sequentially performing hot extrusion and heat treatment on the mixed powder; specifically, the hot extrusion temperature is controlled at 420 ℃, the extrusion ratio is 9:1, and the extrusion speed is 0.5mm/s; and then adopting a T6 heat treatment method, namely carrying out solution treatment on the hot extrusion sample after heat preservation for 120min at 470 ℃, and then carrying out aging treatment at 120 ℃/24h to obtain the product.
Comparative example 2
An aluminum-based composite material, the preparation method of which comprises the following steps:
(1) 7055 aluminum alloy powder is prepared by adopting a conventional gas atomization method;
(2) Preparation of powder B: the same as S2 of example 1;
(3) SPS sintering: the same as S3 of example 1;
(4) Hot extrusion and heat treatment: the same as S4 of example 1.
The properties of the aluminum-based composite materials obtained in the above examples and comparative examples were tested, and the test results are shown in table 1 below:
TABLE 1 Properties of aluminum-based composite materials
| Yield strength/MPa | Tensile strength/MPa | Elongation/% | |
| Example 1 | 793 | 825 | 10.2 |
| Example 2 | 824 | 861 | 8.4 |
| Comparative example 1 | 645 | 706 | 7.5 |
| Comparative example 2 | 612 | 680 | 9.6 |
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the ultrahigh-strength and high-toughness aluminum-based composite material is characterized by comprising the following steps of: s1, preparing aluminum-based alloy powder A with partial amorphization by adopting an ultrasonic gas atomization method; s2, mixing pure metal powder and boron powder according to the atomic percentage of the AlNiTiZr aluminum-based amorphous alloy, adding a dispersing agent, and preparing powder B by adopting a mechanical alloying method; s3, uniformly mixing the powder A, B obtained in the steps S1 and S2, and then performing spark plasma sintering; s4, carrying out hot extrusion forming and heat treatment on the sintered material to obtain the ultrahigh-strength and high-toughness aluminum-based composite material;
s1, the cooling speed is more than or equal to 10 5 K/s。
2. The method for producing an ultrahigh-strength and high-toughness aluminum-based composite material according to claim 1, wherein in S1, the aluminum-based alloy is 7000 series aluminum alloy; preferably, the aluminum-based alloy is selected from any one of 7075 aluminum alloy, 7055 aluminum alloy, al-10Zn-3.5Mg-1.5 Cu.
3. The method for producing an ultrahigh-strength and toughness aluminum-based composite according to claim 1 or 2, wherein in S1, the partially amorphized aluminum-based alloy powder a contains a surface oxide layer having a thickness of 1 to 5 nm.
4. The method for producing an ultrahigh-strength and toughness aluminum-based composite material according to any one of claims 1 to 3, wherein in S2, the boron powder is added in a molar ratio of Ti to B of 1:2 to 3 based on the molar amount of Ti in the AlNiTiZr-based aluminum-based amorphous alloy.
5. The method for preparing an ultrahigh-toughness aluminum-based composite material according to any one of claims 1 to 4, wherein in S2, the dispersant is stearic acid or sodium stearate; the addition amount of the dispersing agent is 1-3wt.% of the total amount of the pure metal powder and the boron powder.
6. The method for preparing an ultrahigh-toughness aluminum-based composite material according to any one of claims 1 to 5, wherein in S2, the mechanical alloying method is a ball milling method, specifically, ball milling is performed under an inert atmosphere, the ball-to-material ratio is 10-20:1, the ball milling rotation speed is 300-600r/min, and the ball milling time is 50-80h.
7. The method of producing an ultrahigh-toughness aluminum-based composite according to any one of claims 1 to 6, wherein in S3, the amount of powder B added is 1 to 40wt.% of the total amount of powder A, B.
8. The method for preparing an ultrahigh-toughness aluminum-based composite material according to any one of claims 1 to 7, wherein in S3, powder A, B is mixed by a low-energy ball milling method, wherein the ball milling speed is 100-300r/min, and the ball milling time is 100-300min.
9. The method for producing an ultrahigh-strength and toughness aluminum-based composite material according to any one of claims 1 to 8, wherein in S4, the hot extrusion temperature is 400 to 500 ℃, the extrusion ratio is 4 to 16:1, and the extrusion speed is 0.1 to 5mm/S; the heat treatment is a T6 heat treatment process.
10. An ultrahigh-toughness aluminum-based composite material, which is characterized by being prepared by the method of any one of claims 1-9.
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