CN117344170A - High-strength and high-toughness graphene reinforced bimodal aluminum-based composite material and preparation method and application thereof - Google Patents
High-strength and high-toughness graphene reinforced bimodal aluminum-based composite material and preparation method and application thereof Download PDFInfo
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 132
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 83
- 230000002902 bimodal effect Effects 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 61
- 239000011812 mixed powder Substances 0.000 claims abstract description 42
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000005204 segregation Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910000838 Al alloy Inorganic materials 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 29
- 230000008569 process Effects 0.000 abstract description 9
- 238000003892 spreading Methods 0.000 abstract description 7
- 230000007480 spreading Effects 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 238000002156 mixing Methods 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
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- 238000010907 mechanical stirring Methods 0.000 description 4
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- 230000005540 biological transmission Effects 0.000 description 3
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- 230000002787 reinforcement Effects 0.000 description 3
- 238000005482 strain hardening Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
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- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003856 thermoforming Methods 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002159 nanocrystal Substances 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
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- 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
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
-
- 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
- C22C32/0084—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 carbon or graphite as the main non-metallic constituent
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/25—Process efficiency
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Abstract
The invention discloses a high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material, and a preparation method and application thereof. The preparation method comprises the following steps: carrying out mixed ball milling treatment on the micron crystal aluminum-based powder I and pure magnesium powder to realize the segregation of magnesium atoms at an aluminum crystal boundary to obtain nanometer crystal mixed powder I; the mass fraction of the pure magnesium powder is 5-10wt% of the total mass of the micron crystal aluminum-based powder I and the pure magnesium powder; mechanically stirring the nanocrystalline mixed powder I, the nanocrystalline aluminum-based powder II and the graphene powder in an organic solvent, and sequentially drying, pressing and extrusion molding the obtained mixed solution to obtain the nano-crystalline aluminum-based powder II. The preparation method provided by the invention has the advantages that the damage to graphene in the process of dispersing and spreading is avoided, the solid solution of magnesium atoms in an aluminum matrix and the offset polymerization of aluminum grain boundaries are realized, the tissue thermal stability of the material in a thermal environment is improved, and the obtained composite material has high strength and high toughness.
Description
Technical Field
The invention relates to the technical field of aluminum-based composite materials, in particular to a high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material, and a preparation method and application thereof.
Background
The information disclosed in the background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an admission or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The high-strength high-toughness performance of the graphene reinforced aluminum-based composite material is a target which is always pursued by material researchers, and researches show that when the content of graphene exceeds a critical value, the strong plasticity of the material is reduced because the spreading and dispersion distribution of the graphene cannot be completely realized, and the partially polymerized graphene forms a crack source in the plastic deformation process.
The finer the grains of the material, the higher the strength thereof, and this rule is established when the grain size is higher than a certain critical size (about 10-15 nm), which is also the main driving force for ultra-fine grain material research. The prior publications, such as CN 103993192A, CN 104073674A, CN 106513621A and CN 107675028A, focus on improving the strength of the graphene reinforced aluminum-based composite material, and realizing the refinement of aluminum matrix grains and the uniform distribution of graphene in the aluminum matrix through mechanical ball milling and severe plastic deformation, however, the method still has the following defects: (1) The refinement of aluminum matrix grains and the dispersion of graphene are synchronously carried out, so that the structure regulation and control are difficult; (2) The flaky graphene is damaged in the mechanical ball milling and severe plastic deformation process, and the increase of defects affects the mechanical property and physical property of the material; (3) The superfine crystal aluminum matrix structure has poor stability, and the crystal grains are easy to grow up in a thermal environment, so that the material performance is reduced; (4) The dispersion efficiency of the graphene is low by mechanical ball milling and severe plastic deformation, and the requirement of industrial production is difficult to meet.
Disclosure of Invention
In view of the above, the invention provides a high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material, and a preparation method and application thereof, wherein the preparation method can prevent the flaky graphene structure from being damaged and the crystal grains from growing in the thermoforming process, and meanwhile, the refinement of aluminum-based matrix crystal grains and the dispersion of graphene are separately carried out, so that the prepared composite material has high strength and high toughness.
In a first aspect, the invention provides a preparation method of a high-strength and toughness graphene reinforced bimodal aluminum-based composite material, which comprises the following steps:
step S1: carrying out mixed ball milling treatment on the micron crystal aluminum-based powder I and pure magnesium powder to realize the segregation of magnesium atoms at an aluminum crystal boundary to obtain nanometer crystal mixed powder I; the mass fraction of the pure magnesium powder is 5-10wt% of the total mass of the micron crystal aluminum-based powder I and the pure magnesium powder;
step S2: mechanically stirring the nanocrystalline mixed powder I, the nanocrystalline aluminum-based powder II and the graphene powder in an organic solvent to obtain a mixed solution;
step S3: drying the mixed solution obtained in the step S2 to obtain mixed powder II;
step S4: and (3) sequentially pressing and extruding the mixed powder II obtained in the step (S3) to obtain the product.
In a second aspect, the invention provides the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material prepared by the preparation method.
In a third aspect, the invention provides application of the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in aluminum alloy parts.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the nanocrystalline aluminum matrix powder is prepared by ball milling, and then the mechanical stirring is adopted to realize the uniform mixing of the nanocrystalline aluminum matrix powder, the microcrystalline aluminum matrix powder and the graphene, so that the damage of the graphene in the process of dispersing and spreading is avoided, and the improvement of the mechanical and physical properties of the graphene on the aluminum matrix is facilitated;
(2) According to the invention, magnesium atoms are solid-solved in an aluminum matrix and are partially polymerized at an aluminum crystal boundary through mixing and ball milling of pure magnesium powder and aluminum-based powder, and under the coupling action of a pinning effect and a dragging effect, the tissue thermal stability of the graphene reinforced bimodal aluminum-based composite material with an ultrafine grain structure in a thermal environment (thermal processing and thermal treatment) can be improved, and the product stability of the composite material is improved;
(3) According to the invention, ball-milled aluminum-based powder (nanocrystalline) and unground aluminum-based powder (microcrystalline) are mixed, the grain size of an aluminum matrix shows bimodal distribution, and the strength and plasticity of the graphene reinforced aluminum-based composite material are improved simultaneously based on grain boundary reinforcement, back stress reinforcement and work hardening, wherein the yield strength is more than 254MPa, and the elongation is more than 12%;
(4) The graphene reinforced aluminum-based composite material with high strength and high toughness can be obtained by mechanical mixing, complicated chemical modification is not needed, the process flow is simple, the cost is low, the equipment requirement is low, the production efficiency is high, the repeatability is good, and the method is suitable for industrial production and has wide application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. It will be obvious to those skilled in the art that other figures may be obtained from these figures without the inventive effort.
FIG. 1 is a scanning electron microscope image of a mixed powder II of example 1 of the present invention;
FIG. 2 is a scanning electron microscope picture of a high strength and toughness graphene-reinforced bimodal aluminum-based composite of example 1 of the present invention;
fig. 3 is a transmission electron microscope picture of the high strength and toughness graphene reinforced bimodal aluminum-based composite material of example 1 of the present invention.
Fig. 4 is a transmission electron microscope picture of the high strength and toughness graphene reinforced bimodal aluminum-based composite of comparative example 3 of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
As described in the background art of the invention, in the preparation process of the graphene reinforced aluminum matrix composite material in the prior art, the flaky graphene is easily damaged in the mechanical ball milling or severe plastic deformation process, so that the mechanical property and the physical property are deteriorated, and meanwhile, the growth of superfine grains is easily generated in a thermal environment, so that the performance of the material is influenced. Therefore, the invention provides a preparation method of a high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material, which comprises the following steps:
step S1: carrying out mixed ball milling treatment on the micron crystal aluminum-based powder I and pure magnesium powder to realize the segregation of magnesium atoms at an aluminum crystal boundary to obtain nanometer crystal mixed powder I; the mass fraction of the pure magnesium powder is 5-10wt% of the total mass of the micron crystal aluminum-based powder I and the pure magnesium powder;
step S2: mechanically stirring the nanocrystalline mixed powder I, the nanocrystalline aluminum-based powder II and the graphene powder in an organic solvent to obtain a mixed solution;
step S3: drying the mixed solution obtained in the step S2 to obtain mixed powder II;
step S4: and (3) sequentially pressing and extruding the mixed powder II obtained in the step (S3) to obtain the product.
According to the invention, the nanocrystallization of an aluminum matrix and the segregation of magnesium atoms in an aluminum grain boundary are realized by adopting a mixed ball mill, and then the uniform mixing of nanocrystalline aluminum-based powder, graphene powder and microcrystalline aluminum-based powder, the spreading of graphene and the uniform dispersion distribution of graphene in the aluminum-based powder are realized by mechanical mixing.
The finer the grains of the material, the higher the strength thereof, and this rule holds when the grain size is higher than a certain critical size (about 10-15 nm), however, as the grains are refined, the grain size of the ultra-fine grain aluminum alloy is close to or smaller than the size range of the plastic deformation mechanism dominant by the dislocation in the metal, the starting of the dislocation source and the dislocation movement in the grains are both inhibited, meanwhile, the newly generated dislocation distance is extremely small, the interaction is easy to occur and annihilate at the grain boundary, the work hardening potential of the material is seriously weakened, and the fracture caused by plastic instability is easy to occur. According to the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material provided by the invention, the grain sizes of the aluminum matrix are in bimodal distribution (namely the nanocrystalline aluminum matrix and the microcrystalline aluminum matrix), the work hardening capacity brought by storage dislocation can be recovered, the expansion of local non-uniform deformation is restrained, and the strength and the plasticity of the composite material are improved at the same time.
In the prior art, mechanical ball milling or severe plastic deformation treatment is often carried out on graphene, and uniform dispersion and spreading of graphene are realized through welding damage process or coordinated plastic deformation of powder particles, however, structural damage of flaky graphene is unavoidable to achieve good effect. According to the invention, the dispersion of graphene is realized only through mechanical stirring, the spreading of agglomerated graphene and the uniform distribution of the agglomerated graphene in aluminum powder are realized through the action of centrifugal force and the action of shearing force between aluminum powder, the aluminum powder can avoid re-agglomeration of graphene after mechanical stirring is finished (in a standing state), the dispersion process is free from damage of graphene, and meanwhile, the preparation process is simplified; the intact graphene is uniformly spread in the aluminum matrix, so that the physical properties of the aluminum matrix composite material are improved, and the mechanical properties of the composite material are improved through bearing reinforcement.
The superfine crystal aluminum matrix in the prior art has poor tissue stability, and grains are easy to grow up in a thermal environment, so that the performance of the material is reduced. According to the invention, through mixing and ball milling, on the premise of meeting the material strength-plasticity requirement, the grain growth of the nanocrystalline aluminum matrix is avoided, and the addition amount of the pure magnesium powder is limited, so that magnesium atoms are biased to gather at the aluminum grain boundary, the tissue heat stability of the aluminum matrix composite material with an ultrafine grain structure in a heat environment (heat processing and heat treatment) can be improved, and the product stability of the composite material is improved. When the addition amount of the pure magnesium powder is less than 5 weight percent, the nanocrystalline aluminum matrix is easy to grow greatly, which is not beneficial to the improvement of the strength; when the addition amount of the pure magnesium powder is more than 10 weight percent, the obtained aluminum-based composite material has poor plasticity.
The first and second micro-crystalline aluminum-based powder can be pure aluminum or aluminum alloy powder, and in order to efficiently obtain the first nano-crystalline mixed powder, the high-strength and toughness graphene reinforced dual-mode aluminum-based composite material has the performance customizable property, the average grain size of the first micro-crystalline aluminum-based powder is 1-20 mu m, and the average grain size of the second micro-crystalline aluminum-based powder is 1-100 mu m.
In an exemplary embodiment of the present invention, in step S1, the pure magnesium powder is selected to have an average particle size of 10 to 100. Mu.m.
In a typical embodiment of the invention, in the step S1, the rotation speed of the ball mill is 300-500 rpm, the ball-material ratio is 50-70:1, and the ball milling time is 5-20 h. The ball milling treatment ensures that the micro-crystal aluminum-based powder is converted into a nano-crystal aluminum matrix. Preferably, the average grain size of the aluminum matrix in the first nanocrystalline mixed powder is 50-80 nm.
The graphene used in the invention is the same as the graphene commonly used in the field, and is obtained by a physical method. In the step S2, the mass fraction of the graphene powder is 0.1-1wt% of the total amount of the nanocrystalline mixed powder I, the microcrystalline aluminum-based powder II and the graphene powder. Too little graphene powder cannot play a reinforcing effect, and too much graphene powder can agglomerate to reduce mechanical properties. In order to fully exert the reinforcing effect of graphene, the number of graphene layers of the present invention is preferably 1 to 20.
In a typical embodiment of the present invention, in step S2, the mass fraction of the second microcrystalline aluminum-based powder is 10-90 wt% of the total mass of the first nanocrystalline mixed powder, the second microcrystalline aluminum-based powder, and the graphene powder. By controlling the proportion of the aluminum-based powder with different sizes, the requirements on mechanical properties, physical properties and material cost diversification can be met.
In a typical embodiment of the present invention, in step S2, the organic solvent is preferably ethanol or acetone, and more preferably ethanol. And a proper organic solvent can ensure the spreading of graphene on the premise of quick drying.
In a typical embodiment of the present invention, in step S3, in order to improve the drying efficiency while avoiding oxidation of the aluminum powder, the drying mode of the present invention is vacuum drying at a temperature of 50 to 100 ℃ for a time of 1 to 5 hours.
In an exemplary embodiment of the present invention, in the step S4, the pressing pressure is 500MPa or more, and the extrusion molding temperature is 200 to 400 ℃. Pressing is to obtain a blank with a certain shape; the subsequent extrusion is performed to enhance the bond strength between the mixed powders, to make the composite more dense, and to eliminate the adverse effect of air voids in the powder-molded composite on its material properties.
The invention also provides the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material prepared by the preparation method, preferably the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material has the yield strength of more than 280MPa and the elongation rate of more than 12%.
The invention also provides application of the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in aluminum alloy parts.
The technical scheme of the invention is further described below by combining specific embodiments.
Example 1
The embodiment provides a preparation method of a high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material, which comprises the following steps:
(1) Mixing and ball milling pure aluminum powder with the average particle size of 10 mu m and pure magnesium powder with the average particle size of 10 mu m to obtain nanocrystalline mixed powder I; wherein the mass fraction of the pure magnesium powder is 10wt%, the ball milling rotation speed is 300rpm, the ball material ratio is 60:1, and the ball milling time is 16 hours.
(2) Mechanically stirring the nanocrystalline mixed powder I, pure aluminum powder with the average particle size of 1 mu m and graphene powder with the layer number of 10 in ethanol to obtain mixed liquid; wherein the mass fraction of the first nanocrystalline mixed powder is 9wt%, the mass fraction of the pure aluminum powder with the average particle size of 1 μm is 90wt%, and the mass fraction of the graphene powder is 1wt%.
(3) And (3) drying the mixed solution in vacuum at 80 ℃ for 1h to realize solid-liquid separation, thereby obtaining mixed powder II.
(4) Pressing the mixed powder II, wherein the pressing pressure is 600MPa; and then carrying out extrusion molding at 400 ℃ to obtain the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material.
The second mixed powder obtained in step (3) of example 1 was observed by a scanning electron microscope, and the result is shown in FIG. 1. As can be seen from the figure, the graphene is fully spread.
The high strength and toughness graphene reinforced bimodal aluminum-based composite material in the step (4) of the embodiment 1 is observed by adopting a scanning electron microscope, and the result is shown in fig. 2. As can be seen from the figure, the graphene is uniformly distributed in the aluminum matrix.
The high strength and toughness graphene reinforced bimodal aluminum-based composite material in the step (4) of the example 1 is observed by adopting a transmission electron microscope, and the result is shown in fig. 3. From the figure, it can be seen that the aluminum matrix grain size exhibits a bimodal distribution, the ultra-fine grain aluminum matrix average grain size is 80nm, and the micro-grain aluminum matrix average grain size is 1 μm.
And (3) carrying out mechanical property test on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the step (4) of the embodiment 1, wherein the yield strength of the composite material is 280MPa, and the elongation is 18%.
Example 2
The difference from example 1 is that: in the step (2), the mass fraction of the first nanocrystalline mixed powder was 80wt%, and the mass fraction of the pure aluminum powder having an average particle diameter of 1 μm was 19wt%.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 2, wherein the yield strength of the composite material is 340MPa, and the elongation is 12%.
Example 3
The difference from example 1 is that: in the step (2), the mass fraction of the nanocrystalline mixed powder I was 50% by weight, and the mass fraction of the pure aluminum powder having an average particle diameter of 1 μm was 49% by weight.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material of the embodiment 3, the yield strength of the composite material is 300MPa, and the elongation is 16%.
Example 4
The difference from example 1 is that:
the step (1) is as follows: mixing and ball milling pure aluminum powder with the average particle size of 20 mu m and pure magnesium powder with the average particle size of 10 mu m to obtain nanocrystalline mixed powder I; wherein the mass fraction of the pure magnesium powder is 10wt%, the ball milling rotation speed is 500rpm, the ball material ratio is 70:1, and the ball milling time is 20 hours.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 4, the yield strength of the composite material is 272MPa, and the elongation is 20%.
Example 5
The difference from example 1 is that:
the step (1) is as follows: mixing and ball milling pure aluminum powder with the average particle size of 1 mu m and pure magnesium powder with the average particle size of 10 mu m to obtain nanocrystalline mixed powder I; wherein the mass fraction of the pure magnesium powder is 10wt%, the ball milling rotation speed is 300rpm, the ball material ratio is 50:1, and the ball milling time is 6 hours.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 5, the yield strength of the composite material is 286MPa, and the elongation is 17%.
Example 6
The difference from example 1 is that: the pure aluminum powder in the step (1) and the step (2) is 6061 alloy powder, wherein the mass fraction of aluminum element is 97.9wt%.
After aging the high-strength and high-toughness graphene-reinforced bimodal aluminum-based composite material of the embodiment 6 for 4 hours at the temperature of 180 ℃, carrying out mechanical property test on the composite material, wherein the yield strength of the composite material is 336MPa, and the elongation is 15%.
Example 7
The difference from example 1 is that: in the step (1), the mass fraction of the pure magnesium powder is 5wt%.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 7, the yield strength of the composite material is 254MPa, and the elongation percentage is 21%.
Example 8
The difference from example 1 is that: the temperature during extrusion was 200 ℃.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 8, the yield strength of the composite material is 300MPa, and the elongation is 15%.
Example 9
The difference from example 1 is that: the average particle diameter of the pure aluminum powder in the step (2) was 100. Mu.m.
Mechanical property test is carried out on the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material in the embodiment 9, the yield strength of the composite material is 256MPa, and the elongation is 20%.
Comparative example 1
This comparative example provides a method for preparing a graphene-reinforced coarse-grain aluminum-based composite material, which is different from example 1 in that no nanocrystalline mixed powder one is added. The method comprises the following specific steps:
(1) Mechanically stirring pure aluminum powder with the average particle size of 1 mu m and graphene powder with the layer number of 10 in ethanol to obtain mixed solution; wherein the mass fraction of the pure aluminum powder with the average particle diameter of 1 μm is 99wt% and the mass fraction of the graphene powder is 1wt%.
(2) And (3) drying the mixed solution in vacuum at 80 ℃ for 1h to realize solid-liquid separation, thereby obtaining mixed powder.
(3) Pressing the mixed powder, wherein the pressing pressure is 600MPa; and then carrying out extrusion molding at 400 ℃ to obtain the graphene reinforced coarse-grain aluminum-based composite material.
And (3) carrying out mechanical property test on the graphene reinforced coarse-grain aluminum-based composite material, wherein the yield strength of the composite material is 220MPa, and the elongation is 14%. It can be seen that the graphene reinforced coarse-grain aluminum-based composite material has better plasticity, but lower strength.
Comparative example 2
The comparative example provides a preparation method of a graphene reinforced ultra-fine grain aluminum-based composite material, which is different from example 1 in that pure aluminum powder with an average particle diameter of 1 μm is not added in step (2) to perform mechanical stirring. The method comprises the following specific steps:
(1) Mixing and ball milling pure aluminum powder with the average particle size of 10 mu m and pure magnesium powder with the average particle size of 10 mu m to obtain nanocrystalline mixed powder I; ball milling rotation speed is 300rpm, ball material ratio is 60:1, and ball milling time is 16h.
(2) Mechanically stirring the nanocrystalline mixed powder I and graphene powder with the layer number of 10 in ethanol to obtain mixed liquid; wherein the mass fraction of the first nanocrystalline mixed powder is 99wt%, and the mass fraction of the graphene powder is 1wt%.
(3) And (3) drying the mixed solution in vacuum at 80 ℃ for 1h to realize solid-liquid separation, thereby obtaining mixed powder II.
(4) Pressing the mixed powder II, wherein the pressing pressure is 600MPa; and then carrying out extrusion molding at 400 ℃ to obtain the graphene reinforced superfine crystal aluminum-based composite material.
The mechanical property test is carried out on the graphene reinforced superfine crystal aluminum-based composite material, the yield strength of the composite material is 350MPa, the elongation is 5%, and the graphene reinforced superfine crystal aluminum-based composite material has higher strength but poorer plasticity.
Comparative example 3
The comparative example provides a preparation method of a graphene-reinforced bimodal aluminum-based composite material, which is different from example 1 in that pure magnesium powder is not added in step (1). The method comprises the following specific steps:
(1) Ball milling is carried out on pure aluminum powder with the average particle size of 10 mu m to obtain nanocrystalline pure aluminum powder, the ball milling rotation speed is 300rpm, the ball-material ratio is 60:1, and the ball milling time is 16h.
(2) Mechanically stirring nanocrystalline pure aluminum powder, pure aluminum powder with an average particle size of 1 mu m and graphene powder with a layer number of 10 in ethanol to obtain a mixed solution; wherein the mass fraction of the nanocrystalline pure aluminum powder is 9wt%, the mass fraction of the pure aluminum powder with the average particle size of 1 μm is 90wt%, and the mass fraction of the graphene powder is 1wt%.
(3) And (3) drying the mixed solution in vacuum at 80 ℃ for 1h to realize solid-liquid separation, thereby obtaining mixed powder.
(4) Pressing the mixed powder, wherein the pressing pressure is 600MPa; and then carrying out extrusion molding at 400 ℃ to obtain the graphene reinforced bimodal aluminum-based composite material.
Mechanical property tests are carried out on the graphene reinforced bimodal aluminum-based composite material, the yield strength of the composite material is 230MPa, the elongation is 14%, and the material strength is low, which is attributed to the fact that pure magnesium powder is not added in the ball milling process, the heat stability of nanocrystalline aluminum-based material is poor, crystal grain growth occurs in the thermoforming process, as shown in fig. 4, the maximum crystal grain size of the nanocrystalline reaches more than 500nm, and the crystal boundary strengthening effect is weakened.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-strength and high-toughness graphene reinforced bimodal aluminum-based composite material is characterized by comprising the following steps of:
step S1: carrying out mixed ball milling treatment on the micron crystal aluminum-based powder I and pure magnesium powder to realize the segregation of magnesium atoms at an aluminum crystal boundary to obtain nanometer crystal mixed powder I; the mass fraction of the pure magnesium powder is 5-10wt% of the total mass of the micron crystal aluminum-based powder I and the pure magnesium powder;
step S2: mechanically stirring the nanocrystalline mixed powder I, the nanocrystalline aluminum-based powder II and the graphene powder in an organic solvent to obtain a mixed solution;
step S3: drying the mixed solution obtained in the step S2 to obtain mixed powder II;
step S4: and (3) sequentially pressing and extruding the mixed powder II obtained in the step (S3) to obtain the product.
2. The method for preparing the high-strength and high-toughness graphene-reinforced bimodal aluminum-based composite material according to claim 1, wherein the first and second microcrystalline aluminum-based powders are pure aluminum or aluminum alloy powders; preferably, the average particle diameter of the first micron crystal aluminum-based powder is 1-20 mu m, and the average particle diameter of the second micron crystal aluminum-based powder is 1-100 mu m.
3. The method for preparing the high-strength and toughness graphene-reinforced bimodal aluminum-based composite material according to claim 1, wherein in the step S1, the average particle size of pure magnesium powder is 10-100 μm.
4. The method for preparing the high-strength and toughness graphene reinforced bimodal aluminum-based composite material according to claim 1, wherein in the step S1, the rotation speed of ball milling is 300-500 rpm, the ball-material ratio is 50-70:1, and the ball milling time is 5-20 h.
5. The preparation method of the high-strength and toughness graphene-reinforced bimodal aluminum-based composite material according to claim 1, wherein in the step S2, the mass fraction of graphene powder is 0.1-1 wt% of the total mass of nanocrystalline mixed powder I, nanocrystalline aluminum-based powder II and graphene powder; the mass fraction of the second microcrystalline aluminum-based powder is 10-90 wt% of the total mass of the first nanocrystalline mixed powder, the second microcrystalline aluminum-based powder and the graphene powder.
6. The method for preparing the high-strength and toughness graphene-reinforced bimodal aluminum-based composite material according to claim 5, wherein in the step S2, the number of graphene layers is 1-20; preferably, the organic solvent comprises ethanol or acetone, more preferably ethanol.
7. The method for preparing the high-strength and toughness graphene-reinforced bimodal aluminum-based composite material according to claim 1, wherein the drying is vacuum drying, the drying temperature is 50-100 ℃, and the drying time is 1-5 h; preferably, the pressing pressure is more than 500MPa, and the extrusion molding temperature is 200-400 ℃.
8. A high strength and toughness graphene-reinforced bimodal aluminum-based composite material prepared by the preparation method according to any one of claims 1 to 7.
9. The high strength and toughness graphene-reinforced bimodal aluminum-based composite material according to claim 8, wherein the yield strength of the high strength and toughness graphene-reinforced bimodal aluminum-based composite material is above 254MPa and the elongation is above 12%.
10. The use of the high-strength and toughness graphene-reinforced bimodal aluminum-based composite material as claimed in claim 8 or 9 in aluminum alloy parts.
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