CN108950281B - Preparation method of polyethylene glycol-repaired graphene-reinforced aluminum-based composite material - Google Patents
Preparation method of polyethylene glycol-repaired graphene-reinforced aluminum-based composite material Download PDFInfo
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- 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
Abstract
A preparation method of a polyethylene glycol-repaired graphene-reinforced aluminum-based composite material relates to a preparation method of a graphene-reinforced aluminum-based composite material. The method aims to solve the problem that grinding aids are remained in an aluminum alloy matrix and realize graphene self-repairing. Preparation: weighing graphene, polyethylene glycol and aluminum metal powder, putting the graphene, polyethylene glycol and aluminum metal powder into a ball milling tank for ball milling, cold pressing, and preparing the composite material after cold pressing. The grinding aid polyethylene glycol is thermally decomposed to generate active C atoms, the active C atoms are adsorbed at the defects of the graphene, so that the structural integrity of the graphene is greatly improved, good interface connection is formed, the overall performance of the material is greatly improved, the polyethylene glycol is beneficial to the flaking of aluminum metal powder, the problem of high dispersion difficulty of single-layer or few-layer graphene in the aluminum-based composite material is solved, cold welding among the aluminum metal powder is reduced, the removal is easy, and the prepared few-layer graphene reinforced aluminum-based composite material has excellent comprehensive performance. The method is suitable for preparing the graphene reinforced aluminum matrix composite.
Description
The technical field is as follows:
the invention relates to a preparation method of a graphene reinforced aluminum matrix composite.
Background art:
graphene has a tensile strength of up to 125GPa, an elastic modulus of 1TPa and a thermal conductivity of 5000W/(m.K), and is undoubtedly an almost ideal reinforcement with excellent comprehensive performance. The graphene can be divided into single-layer graphene, double-layer graphene, few-layer graphene (3-10 layers) and multi-layer graphene (the number of layers is more than 10, and the total thickness is less than 10nm) according to the number of layers. At present, researches on improving the performance of resin and ceramic by using graphene are the most active, and researches on reinforcing a metal matrix, especially on reinforcing an aluminum matrix composite material by using graphene are relatively few. The preparation process mainly comprises a solid phase method and a liquid phase method, wherein the solid phase method comprises various powder metallurgy methods, friction stir welding, the latest Spark Plasma Sintering (SPS) method and the like, and the liquid phase method comprises a pressure infiltration method and the like.
The graphene reinforced aluminum-based composite material has a wide application prospect, the theoretical tensile strength of the graphene reinforced aluminum-based composite material is up to 1.5GPa when calculated by utilizing a shear hysteresis model, but the actual research finds that the high performance of the graphene reinforced aluminum-based composite material is only partially reflected when a very small amount of graphene (less than 0.5-1 wt.%) is added, and the actual strength of the graphene reinforced aluminum-based composite material is rapidly reduced in the process of adding the high-content graphene and is far away from the theoretical calculated strength. The common aluminum powder in the current research is spherical, the specific surface area of the spherical aluminum powder is low, the content of graphene adsorbed on the surface is low, the graphene reinforced aluminum-based composite material with high volume fraction is difficult to prepare, and the flake aluminum powder has higher theoretical packing density, so that the porosity is reduced, and the comprehensive performance of the material is improved; the high-content graphene is extremely easy to agglomerate, and agglomerates in the composite material to form holes, so that the strength of the matrix is reduced; the single-layer graphene is expensive in manufacturing cost and difficult to use on a large scale, most of graphene used in the current research is few-layer graphene micro-sheets with 10-50 layers, van der waals force between graphene layers is weaker than that of covalent bond combination, and if interlayer slippage occurs during fracture, the graphene is difficult to play a role in reinforcement, so that the graphene is hopefully opened in a ball milling mode; ball milling is beneficial to dispersion and opening of graphene, but common grinding aids, such as silane coupling agents, ionic surfactants, stearic acid and the like, are difficult to decompose or decompose to generate impurities such as Si, Na and the like, and the impurities can remain in an aluminum alloy matrix, so that the aluminum alloy components can be changed, the product performance can be reduced, and the influence on subsequent processing and use can be generated.
The invention content is as follows:
the invention provides a preparation method of a polyethylene glycol-repaired graphene-reinforced aluminum matrix composite, aiming at solving the problem that a grinding aid adopted in the dispersion and opening processes of graphene is difficult to decompose or generates residues in an aluminum alloy matrix.
The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material is carried out according to the following steps:
weighing materials
Weighing 0.5-4% of graphene, 2-50% of polyethylene glycol and the balance of aluminum metal powder as raw materials according to mass fraction; the graphene is few-layer graphene, the average sheet diameter is 200 nm-15 mu m, and the average thickness is 1-30 nm; the average particle size of the aluminum metal powder is 1-30 μm;
the aluminum metal powder is aluminum alloy; the aluminum alloy is one or a combination of more of Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy;
the mass fraction of Si in the Al-Si alloy is 2-25%; the mass fraction of Si in the Al-Si-Cu alloy is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Zn in the Al-Zn-Cu alloy is 0.5-55%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Zn in the Al-Zn-Mg-Cu alloy is 0.5-55%, the mass fraction of Mg is 0.5-38%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Cu-Mg alloy is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%;
second, graphene dispersion and precast block molding
Putting the graphene, polyethylene glycol and aluminum metal powder weighed in the step one into a ball milling tank, ball milling for 0.5-7 h at the rotating speed of 100-250 rpm to obtain mixed powder, and putting the mixed powder obtained after ball milling into a cold pressing die for cold pressing to obtain a polyethylene glycol-graphene/aluminum prefabricated body;
the cold pressing comprises the following specific steps: pressurizing the mixed powder to 4-8 MPa at a pressurizing speed of 0.1-30 mm/min, and maintaining the pressure for 5-20 min; the ball-material ratio in the ball milling tank is (5-20): 1;
third, prefabricated section heat preservation
Putting the polyethylene glycol-graphene/aluminum preform obtained in the step two into a vacuum furnace, heating to 350-380 ℃, preserving heat for 2-2.5 hours, heating to 450-490 ℃, and preserving heat for 1-1.2 hours to obtain a polyethylene glycol-repaired graphene/aluminum preform;
the polyethylene glycol is cracked at 350-380 ℃, the cracked polyethylene glycol generates a large number of free oxygen functional groups, has extremely strong reaction activity, is diffused to the surface of graphene at high temperature for adsorption and combination, and forms unique bridging oxygen connection at the defect position of the graphene, so that the damage degree of the graphene is greatly reduced, and the graphene can be prevented from being further damaged; completely decomposing residual polyethylene glycol at 450-490 ℃, diffusing to the surface of the preform and removing to obtain a residue-free polyethylene glycol-repaired graphene/aluminum preform;
fourthly, preparing the polyethylene glycol repaired graphene/aluminum prefabricated body obtained in the third step into the polyethylene glycol repaired graphene reinforced aluminum-based composite material through a pressure infiltration method, a non-pressure infiltration method, a powder metallurgy method or a discharge plasma sintering method, and then completing the preparation.
The invention has the following beneficial effects:
1. the grinding aid polyethylene glycol selected by the invention has moderate viscosity, oxidation resistance, small volatility and no corrosion to metal, is decomposed to generate a large amount of free oxygen functional groups in the heat treatment process, the oxygen functional groups are combined with carbon atoms of defective graphene to form bridge oxygen bonds, and different defective carbons are repaired and connected through the bridge oxygen bonds, so that the damage degree of the graphene is greatly reduced, the load bearing capacity of the graphene is improved, and the further damage of the graphene is also prevented. And the polyethylene glycol pyrolysis product is pollution-free and can be easily removed in a vacuum or atmosphere environment, so that the reduction of the elastic modulus, the bending strength, the yield strength and the tensile strength caused by the grinding aid residue is avoided, and the polyethylene glycol repair graphene reinforced aluminum matrix composite without the grinding aid residue can be prepared.
2. The method takes few-layer graphene, aluminum metal and polyethylene glycol as raw materials, the polyethylene glycol is taken as a ball milling grinding aid, and aluminum metal particles are formed into sheets by utilizing the grinding, shearing and impacting effects of a grinding medium generated in the rotation of a cylinder in the ball milling process; the polyethylene glycol is coated on the surface of the aluminum metal powder, so that the impact behavior of the ball milling medium and the aluminum metal powder is changed, the shearing force in impact is easier to act on the surface of the aluminum metal powder, the aluminum metal powder is favorably flaked, the flaky aluminum powder is favorably separated from the surface of the ball milling medium, and the subsequent operation is convenient.
3. According to the invention, the flake aluminum powder prepared by ball milling graphene, polyethylene glycol and aluminum metal powder has uniform diameter, large diameter-thickness ratio, diameter of 20-50 μm, thickness of 0.5-1 μm and large diameter-thickness ratio, so that the graphene is effectively and uniformly adsorbed on the surface of the flake aluminum powder, the agglomeration of the graphene in a composite material is reduced, the problem of high dispersion difficulty of single-layer or few-layer graphene in the aluminum-based composite material is solved, the polyethylene glycol is coated on the surface of the flake aluminum powder, the direct contact of a new interface generated after ball milling is prevented, and the reduction of cold welding among aluminum metal powder is facilitated; the content of few-layer graphene in the graphene reinforced aluminum-based composite material prepared by the invention can reach 4 wt.% at most, and is far higher than the content (less than 1 wt.%) of few-layer graphene which is taken as a direct raw material at present;
5. the polyethylene glycol generates active C atoms after thermal decomposition, and has extremely high reduction activity after being adsorbed at the graphene defect, so that the graphene oxidation defect is repaired greatly, the integrity of the layered structure is improved, the complete layered graphene structure is more favorable for uniformly dispersing load and transferring stress, the local stress concentration is reduced, the composite material is favorable for bearing larger external force, and the comprehensive performance of the composite material is improved;
6. the polyethylene glycol is used as a grinding aid, has good water solubility, is volatile and easy to decompose, can be removed by various methods such as vacuum filtration, filter pressing, heat treatment, vacuum drying and the like, does not damage the morphology of the flaky aluminum powder in the removal process, and does not influence the components and subsequent application of the aluminum alloy;
7. the graphene reinforced aluminum-based composite material prepared by the invention has excellent comprehensive performance, the elastic modulus exceeds 82GPa, the bending strength is more than 700MPa, the yield strength exceeds 450MPa, the tensile strength exceeds 550MPa, and the elongation rate exceeds 9%.
Description of the drawings:
FIG. 1 is a metallographic representation photograph of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite obtained in example 1;
the specific implementation mode is as follows:
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 preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material is carried out according to the following steps:
weighing materials
Weighing 0.5-4% of graphene, 2-50% of polyethylene glycol and the balance of aluminum metal powder as raw materials according to mass fraction;
second, graphene dispersion and precast block molding
Putting the graphene, polyethylene glycol and aluminum metal powder weighed in the step one into a ball milling tank, ball milling for 0.5-7 h at the rotating speed of 100-250 rpm to obtain mixed powder, and putting the mixed powder obtained after ball milling into a cold pressing die for cold pressing to obtain a polyethylene glycol-graphene/aluminum prefabricated body;
third, prefabricated section heat preservation
Putting the polyethylene glycol-graphene/aluminum preform obtained in the step two into a vacuum furnace, heating to 350-380 ℃, preserving heat for 2-2.5 hours, heating to 450-490 ℃, and preserving heat for 1-1.2 hours to obtain a polyethylene glycol-repaired graphene/aluminum preform;
fourthly, preparing the polyethylene glycol repaired graphene/aluminum prefabricated body obtained in the third step into the polyethylene glycol repaired graphene reinforced aluminum-based composite material through a pressure infiltration method, a non-pressure infiltration method, a powder metallurgy method or a discharge plasma sintering method, and then completing the preparation.
The embodiment has the following beneficial effects:
1. the grinding aid polyethylene glycol selected by the embodiment has moderate viscosity, is antioxidant, has small volatility, does not corrode metal, decomposes to generate a large amount of free oxygen functional groups in the heat treatment process, combines the oxygen functional groups with carbon atoms of defective graphene to form a bridge oxygen bond, repairs and connects different defective carbons through the bridge oxygen bond, reduces the damage degree of the graphene to a great extent, improves the load bearing capacity of the graphene, and prevents the further damage of the graphene. And the polyethylene glycol pyrolysis product is pollution-free and can be easily removed in a vacuum or atmosphere environment, so that the reduction of the elastic modulus, the bending strength, the yield strength and the tensile strength caused by the grinding aid residue is avoided, and the polyethylene glycol repair graphene reinforced aluminum matrix composite without the grinding aid residue can be prepared.
2. In the embodiment, few-layer graphene, aluminum metal and polyethylene glycol are used as raw materials, the polyethylene glycol is used as a ball milling grinding aid, and aluminum metal particles are formed into sheets by utilizing the grinding, shearing and impacting effects of a grinding medium generated in the rotation of a cylinder in the ball milling process; the polyethylene glycol is coated on the surface of the aluminum metal powder, so that the impact behavior of the ball milling medium and the aluminum metal powder is changed, the shearing force in impact is easier to act on the surface of the aluminum metal powder, the aluminum metal powder is favorably flaked, the flaky aluminum powder is favorably separated from the surface of the ball milling medium, and the subsequent operation is convenient.
3. According to the embodiment, the flake aluminum powder prepared by ball milling of graphene, polyethylene glycol and aluminum metal powder is uniform in sheet diameter, large in diameter-thickness ratio, 20-50 microns in diameter, 0.5-1 micron in thickness and large in diameter-thickness ratio, so that the graphene is effectively and uniformly adsorbed on the surface of the flake aluminum powder, the agglomeration of the graphene in a composite material is reduced, the problem of high dispersion difficulty of single-layer or few-layer graphene in the aluminum-based composite material is solved, the polyethylene glycol is coated on the surface of the flake aluminum powder, a new interface generated after ball milling is prevented from being in direct contact, and the reduction of cold welding among aluminum metal powder is facilitated; the content of the few-layer graphene in the graphene reinforced aluminum-based composite material prepared by the embodiment can reach 4 wt.% at most, and is far higher than the content (less than 1 wt.%) of the few-layer graphene which is taken as a direct raw material at present;
5. the polyethylene glycol generates active C atoms after thermal decomposition, and has extremely high reduction activity after being adsorbed at the graphene defect, so that the graphene oxidation defect is repaired greatly, the integrity of the layered structure is improved, the complete layered graphene structure is more favorable for uniformly dispersing load and transferring stress, the local stress concentration is reduced, the composite material is favorable for bearing larger external force, and the comprehensive performance of the composite material is improved;
6. the embodiment takes the polyethylene glycol as a grinding aid, the polyethylene glycol has good water solubility, is volatile and easy to decompose, can be removed by various methods such as vacuum filtration, filter pressing, heat treatment, vacuum drying and the like, does not damage the morphology of the flaky aluminum powder in the removal process, and does not influence the components and subsequent application of the aluminum alloy;
7. the graphene reinforced aluminum matrix composite material prepared by the embodiment has excellent comprehensive performance, the elastic modulus exceeds 82GPa, the bending strength is greater than 700MPa, the yield strength exceeds 450MPa, the tensile strength exceeds 550MPa, and the elongation rate exceeds 9%.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the graphene is few-layer graphene, the average sheet diameter is 200 nm-15 mu m, and the average thickness is 1-30 nm. Other steps and parameters are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the first step, the average particle size of the aluminum metal powder is 1-30 μm. Other steps and parameters are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: step one, the aluminum metal powder is aluminum alloy. Other steps and parameters are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the aluminum alloy in the first step is one or a combination of more of Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy. Other steps and parameters are the same as in embodiment four.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the mass fraction of Si in the Al-Si alloy is 2-25%; the mass fraction of Si in the Al-Si-Cu alloy is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Zn in the Al-Zn-Cu alloy is 0.5-55%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Zn in the Al-Zn-Mg-Cu alloy is 0.5-55%, the mass fraction of Mg is 0.5-38%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Cu-Mg alloy is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%. Other steps and parameters are the same as in one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: step two, the cold pressing comprises the following specific steps: pressurizing the mixed powder to 4-8 MPa at a pressurizing speed of 0.1-30 mm/min, and maintaining the pressure for 5-20 min. Other steps and parameters are the same as in one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and the ball-material ratio in the ball-milling tank in the second step is (5-20): 1. other steps and parameters are the same as in one of the first to seventh embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum matrix composite material comprises the following steps:
weighing materials
Weighing 4% of graphene, 50% of polyethylene glycol and the balance of aluminum metal powder as raw materials according to mass fraction; the graphene is few-layer graphene, the average sheet diameter is 200nm, and the average thickness is 1 nm; the average particle size of the aluminum metal powder is 1 μm;
the aluminum metal powder is aluminum alloy; the aluminum alloy is Al-Si alloy, and the mass fraction of Si in the Al-Si alloy is 2-25%;
second, graphene dispersion and precast block molding
Putting the graphene, polyethylene glycol and aluminum metal powder weighed in the step one into a ball milling tank, ball milling the mixed powder obtained by 0.5 at the rotating speed of 250rpm, putting the mixed powder obtained after ball milling into a cold pressing die, and carrying out cold pressing to obtain a polyethylene glycol-graphene/aluminum prefabricated body;
the cold pressing comprises the following specific steps: pressurizing the mixed powder to 8MPa at a pressurizing speed of 0.1mm/min, and maintaining the pressure for 5 min; the ball-material ratio in the ball-milling tank is 5: 1;
third, prefabricated section heat preservation
Putting the polyethylene glycol-graphene/aluminum preform obtained in the step two into a vacuum furnace, heating to 360 ℃, preserving heat for 2 hours, then heating to 470 ℃, and preserving heat for 1 hour to obtain a polyethylene glycol repaired graphene/aluminum preform;
the polyethylene glycol is cracked at 350-380 ℃, the cracked polyethylene glycol generates a large number of free oxygen functional groups, has extremely strong reaction activity, is diffused to the surface of graphene at high temperature for adsorption and combination, and forms unique bridging oxygen connection at the defect position of the graphene, so that the damage degree of the graphene is greatly reduced, and the graphene can be prevented from being further damaged; completely decomposing residual polyethylene glycol at 450-490 ℃, diffusing to the surface of the preform and removing to obtain a residue-free polyethylene glycol-repaired graphene/aluminum preform;
fourthly, preparing the polyethylene glycol repaired graphene/aluminum prefabricated body obtained in the third step into the polyethylene glycol repaired graphene reinforced aluminum-based composite material through a pressure infiltration method, a non-pressure infiltration method, a powder metallurgy method or a discharge plasma sintering method, and then completing the preparation.
The pressure infiltration method comprises the following specific processes: putting the polyethylene glycol-repaired graphene/aluminum prefabricated part into a vacuum air pressure infiltration furnace, putting the pure aluminum block into a graphite mold at the bottom of a furnace chamber of the vacuum air pressure infiltration furnace, putting the polyethylene glycol-repaired graphene/aluminum prefabricated part on the upper part of the furnace chamber of the vacuum air pressure infiltration furnace, sealing the vacuum air pressure infiltration furnace, and vacuumizing until the vacuum degree is less than 10-4MPa, heating a vacuum air pressure infiltration furnace, and preheating the polyethylene glycol repaired graphene/aluminum preform to 400 ℃ under vacuum; heating an industrial pure aluminum block to 760 ℃ and preserving heat for 0.5h to obtain molten aluminum metal; immersing the preheated polyethylene glycol-repaired graphene/aluminum preform into molten aluminum metal, stopping heating, introducing protective gas into the vacuum pressure infiltration furnace, and naturally cooling the furnace temperature of the vacuum pressure infiltration furnace to room temperature to obtain a high-density graphene-reinforced aluminum-based composite ingot; the protective gas is nitrogen; the pressure of the protective gas is 0.1 MPa;
fig. 1 is a metallographic representation photograph of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material obtained in example 1, and it can be seen from the photograph that graphene nanoplatelets are uniformly distributed, large agglomerates are not generated, the overall density of the material is high, and the porosity is low. In the embodiment, the flake aluminum powder prepared by ball milling graphene, polyethylene glycol and aluminum metal powder has uniform diameter, large diameter-thickness ratio, diameter of 30-50 μm, thickness of 0.7-1 μm and large diameter-thickness ratio, so that the uniform adsorption of graphene on the surface of the flake aluminum powder is effectively realized, the agglomeration of graphene in a composite material is favorably reduced, the problem of high dispersion difficulty of single-layer or few-layer graphene in the aluminum-based composite material is solved, and the content of the few-layer graphene in the composite material can reach 4 wt% at most; the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material prepared by the embodiment has excellent comprehensive performance, the elastic modulus is 82GPa, the bending strength is 800MPa, the yield strength is 550MPa, the tensile strength is 650MPa, and the elongation is 10%.
Example 2:
the preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum matrix composite material comprises the following steps:
weighing materials
Weighing 4% of graphene, 2% of polyethylene glycol and the balance of aluminum metal powder as raw materials according to mass fraction; the graphene is few-layer graphene, the average sheet diameter is 15 micrometers, and the average thickness is 30 nm; the average particle size of the aluminum metal powder is 30 μm;
the aluminum metal powder is aluminum alloy; in the Al-Cu-Mg alloy, the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%;
second, graphene dispersion and precast block molding
Putting the graphene, polyethylene glycol and aluminum metal powder weighed in the step one into a ball milling tank, ball milling the mixed powder obtained by 0.5 at the rotating speed of 250rpm, putting the mixed powder obtained after ball milling into a cold pressing die, and carrying out cold pressing to obtain a polyethylene glycol-graphene/aluminum prefabricated body;
the cold pressing comprises the following specific steps: pressurizing the mixed powder to 4MPa at a pressurizing speed of 30mm/min, and maintaining the pressure for 10 min; the ball-material ratio in the ball milling tank is 10: 1;
third, prefabricated section heat preservation
Putting the polyethylene glycol-graphene/aluminum preform obtained in the step two into a vacuum furnace, heating to 360 ℃, preserving heat for 2 hours, then heating to 470 ℃, and preserving heat for 1 hour to obtain a polyethylene glycol repaired graphene/aluminum preform;
fourthly, preparing the polyethylene glycol repaired graphene/aluminum prefabricated body obtained in the third step into the polyethylene glycol repaired graphene reinforced aluminum-based composite material through a pressure infiltration method, a non-pressure infiltration method, a powder metallurgy method or a discharge plasma sintering method, and then completing the preparation.
The pressure infiltration method comprises the following specific processes: putting the polyethylene glycol repaired graphene/aluminum prefabricated body into a vacuum pressure infiltration furnace, and putting the pure aluminum block body into graphite at the bottom of a furnace chamber of the vacuum pressure infiltration furnaceIn the mold, the polyethylene glycol repaired graphene/aluminum prefabricated part is placed on the upper part of a furnace chamber of a vacuum air pressure infiltration furnace, the vacuum air pressure infiltration furnace is sealed and vacuumized until the vacuum degree is less than 10-4MPa, heating a vacuum air pressure infiltration furnace, and preheating the polyethylene glycol repaired graphene/aluminum preform to 400 ℃ under vacuum; heating an industrial pure aluminum block to 760 ℃ and preserving heat for 0.5h to obtain molten aluminum metal; immersing the preheated polyethylene glycol-repaired graphene/aluminum preform into molten aluminum metal, stopping heating, introducing protective gas into the vacuum pressure infiltration furnace, and naturally cooling the furnace temperature of the vacuum pressure infiltration furnace to room temperature to obtain a high-density graphene-reinforced aluminum-based composite ingot; the protective gas is nitrogen; the pressure of the protective gas is 0.1 MPa;
in the embodiment, the flake aluminum powder prepared by ball milling graphene, polyethylene glycol and aluminum metal powder has uniform diameter, large diameter-thickness ratio, diameter of 10-20 microns, thickness of 0.5-0.8 microns and large diameter-thickness ratio, so that the uniform adsorption of graphene on the surface of the flake aluminum powder is effectively realized, the agglomeration of graphene in a composite material is favorably reduced, the problem of high dispersion difficulty of single-layer or few-layer graphene in the aluminum-based composite material is solved, and the content of the few-layer graphene in the composite material can reach 4 wt% at most; the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material prepared by the embodiment has excellent comprehensive performance, the elastic modulus is 92GPa, the bending strength is 710MPa, the yield strength is 460MPa, the tensile strength is 560MPa, and the elongation is 10%.
Claims (8)
1. A preparation method of a polyethylene glycol-repaired graphene-reinforced aluminum-based composite material is characterized by comprising the following steps: the method comprises the following steps:
weighing materials
Weighing 0.5-4% of graphene, 2-50% of polyethylene glycol and the balance of aluminum metal powder as raw materials according to mass fraction;
second, graphene dispersion and precast block molding
Putting the graphene, polyethylene glycol and aluminum metal powder weighed in the step one into a ball milling tank, ball milling for 0.5-7 h at the rotating speed of 100-250 rpm to obtain mixed powder, and putting the mixed powder obtained after ball milling into a cold pressing die for cold pressing to obtain a polyethylene glycol-graphene/aluminum prefabricated body;
third, prefabricated section heat preservation
Putting the polyethylene glycol-graphene/aluminum preform obtained in the step two into a vacuum furnace, heating to 350-380 ℃, preserving heat for 2-2.5 hours, heating to 450-490 ℃, and preserving heat for 1-1.2 hours to obtain a polyethylene glycol-repaired graphene/aluminum preform;
fourthly, preparing the polyethylene glycol repaired graphene/aluminum prefabricated body obtained in the third step into the polyethylene glycol repaired graphene reinforced aluminum-based composite material through a pressure infiltration method, a non-pressure infiltration method or a powder metallurgy method, and then completing the preparation.
2. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 1, characterized in that: the graphene is few-layer graphene, the average sheet diameter is 200 nm-15 mu m, and the average thickness is 1-30 nm.
3. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 1 or 2, characterized in that: in the first step, the average particle size of the aluminum metal powder is 1-30 μm.
4. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 3, characterized in that: step one, the aluminum metal powder is aluminum alloy.
5. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 4, characterized in that: the aluminum alloy is one or a combination of more of Al-Si alloy, Al-Si-Cu alloy, Al-Cu-Mg alloy, Al-Zn-Cu alloy, Al-Zn-Mg-Cu alloy and Al-Si-Cu-Mg alloy.
6. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 5, characterized in that: the mass fraction of Si in the Al-Si alloy is 2-25%; the mass fraction of Si in the Al-Si-Cu alloy is 0.5-25%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Cu in the Al-Cu-Mg alloy is 0.5-53%, and the mass fraction of Mg is 0.5-38%; the mass fraction of Zn in the Al-Zn-Cu alloy is 0.5-55%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Zn in the Al-Zn-Mg-Cu alloy is 0.5-55%, the mass fraction of Mg is 0.5-38%, and the mass fraction of Cu is 0.5-53%; the mass fraction of Si in the Al-Si-Cu-Mg alloy is 0.5-25%, the mass fraction of Cu is 0.5-53%, and the mass fraction of Mg is 0.5-38%.
7. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 6, characterized in that: step two, the cold pressing comprises the following specific steps: pressurizing the mixed powder to 4-8 MPa at a pressurizing speed of 0.1-30 mm/min, and maintaining the pressure for 5-20 min.
8. The preparation method of the polyethylene glycol-repaired graphene-reinforced aluminum-based composite material according to claim 6, characterized in that: and the ball-material ratio in the ball-milling tank in the second step is (5-20): 1.
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