CN111321314B - Preparation method of graphene reinforced aluminum matrix composite with strong interface bonding strength - Google Patents
Preparation method of graphene reinforced aluminum matrix composite with strong interface bonding strength Download PDFInfo
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- CN111321314B CN111321314B CN202010130219.9A CN202010130219A CN111321314B CN 111321314 B CN111321314 B CN 111321314B CN 202010130219 A CN202010130219 A CN 202010130219A CN 111321314 B CN111321314 B CN 111321314B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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Abstract
The invention discloses a preparation method of a graphene reinforced aluminum-based composite material with strong interface bonding, and belongs to the field of composite material preparation. The composite material is characterized in that: the interface of the graphene and the aluminum matrix presents an interface with periodically and regularly arranged C atoms and Al atoms, and the interface presents periodically distributed molar stripes under the representation of a transmission electron microscope. The method comprises the following steps: the method comprises the following steps of 1, uniformly dispersing and mixing graphene and aluminum powder by adopting ultrasonic stirring combined with mechanical stirring based on an electrostatic adsorption principle, 2, wrapping the uniformly dispersed composite material powder with an aluminum foil 3, placing the aluminum foil wrapped with the powder in a vacuum arc melting furnace, forming covalent bond combination of graphene atoms and aluminum atoms under high-density current density, and forming a composite material block with high interface bonding strength in a specific orientation during cooling. The composite material prepared by the process has high interface bonding strength, and the process flow is simple, so that large-scale preparation is easy to realize.
Description
Technical Field
The invention relates to the technical field of composite material preparation, and particularly provides a composite material with strong interface bonding prepared by a vacuum arc melting technology.
Background
The graphene has excellent mechanical properties and is an excellent reinforcement for various composite materials; the aluminum and the aluminum alloy have excellent specific strength and wide application prospect in the automobile and aviation industries, so that the graphene reinforced aluminum matrix composite becomes a hot point for research.
As a composite material, the graphene aluminum-based composite material is of great importance in fully utilizing the bearing effect of graphene. The interface is used as a carrier of a load transfer effect, and the strength of interface combination directly determines the enhancement effect of the graphene. The powder metallurgy and the improved powder metallurgy method have certain advantages in the dispersion of graphene and are widely applied to the graphene aluminum-based composite material, however, the oxidation of the aluminum surface is difficult to avoid in the process of preparing the composite material by adopting the powder metallurgy, and amorphous Al is easily introduced into the interface between the graphene and the aluminum2O3Decrease ofThe load transfer effect of the graphene is good, so that the enhancement efficiency of the graphene is reduced, and the load bearing effect of the graphene is not good for full play; researchers such as Li utilize the fact that chemical reaction is easy to occur between graphene and aluminum, and annealing graphene aluminum-based composite materials forms proper Al on the interface between graphene and aluminum4C3The interface reaction layer enhances the interface bonding force between the graphene and the aluminum substrate, so that the bearing effect of the graphene is enhanced, but the annealing process condition is not easy to control and is greatly influenced by a sample, the interface reaction layer is easily too thick, and the graphene enhancing effect is reduced. Therefore, the development of the composite material with simple process and high interface bonding strength is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method of a strong interface bonding graphene reinforced aluminum matrix composite. The composite material is characterized in that: the interface of the graphene and the aluminum matrix presents a coherent interface combined by covalent bonds, so that the graphene enhancement efficiency is high and the enhancement effect is good. The coherent interface forming principle is as follows: under the action of high current density between an electrode and a sample, graphene is ionized, part of ionized graphene is combined with aluminum in the cooling process, part of ionized graphene is combined with aluminum and forms a structure with Al atoms and C atoms regularly arranged periodically in a specific orientation, and meanwhile Al is avoided4C3The interface bonding force is improved, and therefore the mechanical property of the composite material is improved.
The method adopted by the invention comprises the following steps:
1. pre-dispersing graphene and aluminum powder to obtain composite material powder
2. Wrapping the composite material powder obtained in the step 1 by using aluminum foil and placing the composite material powder in a vacuum arc melting furnace
3. And (3) applying electric arc to the composite material, dispersing the sample under the action of electromagnetic stirring, and cooling to obtain the graphene reinforced aluminum matrix composite material.
The graphene and the aluminum powder are pre-dispersed through an electrostatic adsorption mechanism.
The specific process of the pre-dispersion process for the graphene and the aluminum powder comprises the following steps: carrying out ultrasonic dispersion on graphene in 100ml of alcohol solution for 30-60 minutes, adding 10ml of deionized water, then gradually adding aluminum powder, stirring the obtained suspension for 20-30 minutes under the action of mechanical stirring and ultrasonic dispersion to obtain a mixed solution, carrying out suction filtration on the mixed solution, and drying to obtain composite material powder.
The environment for preparing the composite material is high-purity Ar with the pressure of 0.5-0.6Pa, and the electric arc melting furnace is firstly vacuumized to 5 x 10 before the high-purity Ar is introduced-3And removing the gas in the furnace under Pa.
The preparation conditions in the preparation process of the composite material are as follows: the smelting voltage is 18V, and the current is 150A; the smelting time is 5 minutes, and the steps are repeated after the sample is turned over.
The electromagnetic stirring current is 0.5-0.9A in the preparation process of the composite material.
The added graphene nanosheets account for 0-3% of the composite material powder by weight.
The method has the beneficial effects that the interface bonding strength of the graphene and the aluminum matrix can be improved, the graphene reinforcing effect is improved, and the mechanical property of the composite material is improved.
Drawings
FIG. 1 is a high-resolution transmission electron microscope photograph of an interface part of a graphene aluminum-based composite material
FIG. 2 is a photograph showing the evolution of mechanical properties of graphene aluminum-based composite material
FIG. 3 XRD pattern of graphene aluminum matrix composite
The invention is further described in detail with reference to the drawings and the embodiments given by the inventor.
Detailed Description
In the present invention, the raw materials and equipment used are commercially available or commonly used in the art, if not specified. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1
Placing 0.075g of graphene nanosheet in 100ml of absolute ethyl alcohol solution for ultrasonic dispersion for 30 minutes, adding 10ml of deionized water, adding 14.925g of aluminum powder to obtain a suspension, stirring for 20 minutes under the action of mechanical stirring and ultrasonic dispersion to obtain a mixed solution, and carrying out suction filtration and drying on the mixed solution to obtain graphene/aluminum mixed powder.
Wrapping the graphene/aluminum mixed powder by using an aluminum foil, and placing the wrapped graphene/aluminum mixed powder in a vacuum arc melting furnace.
Starting a mechanical pump to pump the air pressure in the furnace to 50Pa, then starting a molecular pump to pump the air pressure in the furnace to 5 × 10-3And Pa, introducing high-purity Ar with the air pressure of 0.5-0.6Pa into the furnace, applying direct current of 10V and 150A to the composite material powder wrapped by the aluminum foil in the atmosphere of the high-purity Ar for arc melting, electromagnetically stirring for 5 minutes while melting, turning over the sample by using a mechanical arm, continuing melting for 5 minutes under the parameters, and naturally cooling to room temperature to obtain a composite material block with the graphene mass percent of 0.5%.
Tensile testing of the composites was carried out at room temperature with a strain rate of 3 x 10-3And/s, comparing the strength of pure aluminum without graphene and the strength of the graphene aluminum-based composite material added with 0.5 wt% by adopting the same preparation process, wherein the tensile strength of the pure aluminum is 113.13MPa, the tensile strength of the graphene aluminum-based composite material added with 0.5 wt% is 145.48MPa, the strength is improved by 28.61%, and better reinforcing efficiency is shown.
Example 2
Placing 0.15g of graphene in 100ml of absolute ethyl alcohol solution for ultrasonic dispersion for 40 minutes, adding 10ml of deionized water, then adding 14.85g of aluminum powder to obtain suspension, stirring for 25 minutes under the action of mechanical stirring and ultrasonic dispersion to obtain mixed liquor, carrying out suction filtration on the mixed liquor, and drying to obtain graphene/aluminum mixed powder.
Wrapping the graphene/aluminum mixed powder by using an aluminum foil, and placing the wrapped graphene/aluminum mixed powder in a vacuum arc melting furnace.
Pumping the gas pressure in the furnace to 50Pa by using a mechanical pump, then starting a molecular pump, and pumping the gas pressure in the furnace to 5 × 10-3And Pa, introducing high-purity Ar with the air pressure of 0.5-0.6Pa into the furnace, applying direct current of 10V and 150A to the composite material powder wrapped by the aluminum foil in the atmosphere of the high-purity Ar for arc melting, electromagnetically stirring for 5 minutes while melting, turning over the sample by using a mechanical arm, continuing melting for 5 minutes under the parameters, and naturally cooling to room temperature to obtain a composite material block with the graphene mass percent of 1%.
Tensile testing of the composites was carried out at room temperature with a strain rate of 3 x 10-3And/s, comparing the strength of pure aluminum without graphene and the strength of the graphene aluminum-based composite material added with 1 wt% by adopting the same preparation process, wherein the tensile strength of the pure aluminum is 113.13MPa, the tensile strength of the graphene aluminum-based composite material added with 1 wt% is 184.49MPa, the strength is improved by 63.09%, and better reinforcing efficiency is shown.
Fig. 1 is a comparison of mechanical properties of pure aluminum prepared by the same process and composite materials with different mass percentages, and it can be seen from the figure that the tensile strength of the composite material is improved after graphene is added, and the strength of the composite material is improved by 28.6% and 63.1% respectively after 0.5% and 1% of graphene are added. And the second figure is a TEM (transmission electron microscope) of the interface structure of the composite material prepared by the process flow, and the TEM shows that the graphene and aluminum interface has periodically distributed molar stripes, so that the periodic regular arrangement of C atoms and Al atoms is proved, and the interface is tightly combined. FIG. three is the XRD results of pure aluminum prepared using the same procedure and composite materials of different mass percentages, which shows that there is no Al in the composite material4C3And (4) generating.
The above shows that the method of the present invention can prepare the graphene aluminum-based composite material with the interface of graphene and aluminum being coherent and without Al4C3, and the mechanical properties of the composite material are greatly improved.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (3)
1. A preparation method of a graphene reinforced aluminum matrix composite with strong interface bonding strength is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing graphene/aluminum mixed powder: ultrasonically dispersing graphene nano sheets with the weight percentage of less than 3% and the thickness of 1-10nm in 50-150 ml of alcohol solution for 30-60 minutes, adding 5-15 ml of deionized water, gradually adding aluminum powder with the average particle size of 10-100 microns to obtain suspension, stirring the suspension for 20-30 minutes under the action of mechanical stirring and ultrasonic dispersion to obtain mixed liquid, and performing suction filtration and drying on the mixed liquid to obtain graphene/aluminum mixed powder;
(2) preparing a composite material: wrapping the graphene pre-dispersion powder obtained in the step (1) by using an aluminum foil, placing the wrapped graphene pre-dispersion powder in a vacuum arc melting furnace, and ensuring that the vacuum degree of the arc melting furnace is lower than 5 x 10 by adopting multi-stage vacuum equipment-3Pa, then introducing high-purity Ar with the air pressure of 0.5-0.6Pa into the furnace, adding direct current to carry out arc melting in the atmosphere of the high-purity Ar, electromagnetically stirring for 3-7 minutes while melting, then continuing to melt for 3-7 minutes after turning over the sample by using a mechanical arm, and naturally cooling to room temperature to obtain the composite material block.
2. The preparation method of the graphene reinforced aluminum matrix composite material with the strong interface bonding strength according to claim 1, wherein the electromagnetic stirring current is 0.5-0.9A.
3. The preparation method of the graphene reinforced aluminum matrix composite material with the strong interface bonding strength as claimed in claim 1, wherein during arc melting, the melting voltage is greater than 15V, and the current is greater than 150A.
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