CN115478187A - Preparation method of graphene reinforced aluminum alloy base composite material - Google Patents
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Abstract
The invention discloses a preparation method of a graphene reinforced aluminum alloy matrix composite material. The method is simple and easy to implement, and the prepared composite material has the characteristics of uniform graphene distribution and good performance consistency.
Description
Technical Field
The invention relates to a preparation method of an aluminum alloy base composite material, in particular to a preparation method of a graphene/aluminum alloy composite material.
Background
Graphene is an sp discovered in recent years 2 Hybrid carbon atom close packingThe formed novel two-dimensional planar nano material has huge specific surface area (2630 m) 2 G) and ultrahigh carrier mobility (15000-25000 cm) 2 The material has excellent electrical, thermal and mechanical properties, namely/Vs), thermal conductivity (4840-5300W/mK), young modulus (1000 GPa) and breaking strength (130 GPa), and forbidden band width approximately equal to 0, so that the material becomes one of the most ideal reinforcements of the metal-based nano composite material.
The aluminum alloy has low density, high strength and good ductility, and is widely applied in the fields of aerospace and the like. As a structural material, improvement of strength has been a major direction of research on aluminum alloys. At present, the traditional fusion casting metallurgy methods such as adjusting the components of the aluminum alloy, optimizing the thermomechanical deformation processing and the heat treatment system encounter bottlenecks in improving the performance of the aluminum alloy. The preparation of high-performance aluminum-based composite materials by using graphene as a reinforcement becomes an important direction for the current research of high-performance aluminum alloys.
Patent document CN111101172a discloses a graphene aluminum composite material and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, preparing a graphene aerosol cathode, adopting graphene aerogel as a cathode, adopting metal aluminum as an anode, placing the cathode and the anode in molten electrolytic salt (the electrolytic salt is composed of sodium chloride, potassium chloride and aluminum chloride in different proportions), and electrolyzing under the electrolytic current of 250 mA-350 mA to obtain the graphene aluminum composite material. In the document, the graphene aerosol is high in preparation cost and energy consumption, and meanwhile, the electrolytic production of NaCl and the like can generate polluting chlorine and the like. Patent document CN105112699a discloses a preparation method of a graphene/aluminum alloy composite material, which comprises the following steps: mechanical powder mixing, low-temperature liquid nitrogen ball milling, vacuum sheath packaging, hot isostatic pressing sintering to prepare a blank, and hot extrusion molding of the blank. The method has the advantages that firstly, a large amount of time is consumed for mixing and the low-temperature ball milling process is long, and secondly, the graphene is unevenly distributed due to the density difference between the graphene and the aluminum powder. Patent document CN109112367B discloses a graphene reinforced Al-Si-Mg cast aluminum alloy and a preparation method thereof, the method adopts vacuum melting, the material distribution adopts layered material distribution, and the graphene layer is placed in the middle. The method is characterized in that aluminum particles are required, so that the type of raw materials is difficult to realize in large-scale production, and more than 10 kilograms of aluminum ingots are adopted in general large-scale production; on the other hand, the density difference between the aluminum alloy melt and the graphene is large, and the graphene inevitably floats on the surface of the aluminum alloy melt in the aluminum alloy smelting process, so that the graphene is not uniformly lost and distributed in the aluminum alloy preparation process.
Patent documents CN105081310A, CN104630528a and CN102329976a both propose a method for preparing graphene-metal composite powder by modifying the surface of metal powder with graphene oxide solution, which better solves the problem of uniform dispersion distribution of graphene in a metal matrix, but the accompanying problem is the sintering densification problem of graphene-coated aluminum alloy powder, namely, the sintering performance is not good due to the continuous and dense oxide film on the surface of the aluminum alloy powder, and the sintering performance of the aluminum alloy powder is deteriorated and the densification is reduced because the graphene sheet hinders the diffusion and migration of aluminum atoms and the reaction activity of the carbon material is not high.
The literature reports that addition of trace amounts of low-melting-point metal powder such as tin and lead or addition of boron oxide powder (patent document CN 104999074B) can effectively destroy oxide films to promote improvement of sintering compactness of aluminum alloy, but Sn and Pb particles formed in the sintering process and brittle boron glass can reduce strength or ductility and toughness of the aluminum alloy composite material. Sintering in a high-purity nitrogen atmosphere can also achieve higher sintered density, but the problems are that: the air adsorbed on the surface of the aluminum alloy powder can influence the adsorption of nitrogen on the surface of the powder, particularly the adsorption of powder particles at the center of a green blank to the nitrogen, so that the sintering behavior of the powder can be influenced by the difference of the nitrogen adsorption amount of the powder, and further, a performance gradient is generated in the sintered composite material, and the performance gradient is more obvious for a sintered product with a large size specification.
In conclusion, the preparation method of the powder metallurgy graphene reinforced aluminum matrix composite material is to be further improved. Aiming at the defects in the preparation of the graphene reinforced aluminum matrix composite, the invention provides an effective green preparation method of the graphene reinforced aluminum matrix composite.
Disclosure of Invention
The invention aims to provide a method for preparing a graphene reinforced aluminum alloy matrix composite material based on a powder metallurgy technology, aiming at the defects of the prior art. According to the invention, pure aluminum powder and spherical aluminum alloy pre-prepared powder are used as matrix materials, graphene oxide nanosheets are used as precursors of graphene reinforcements, and the uniformity of distribution of graphene in the aluminum alloy matrix composite material is adjusted.
The invention is realized by the following technical scheme:
according to the preparation method, the graphene oxide is coated on the surface of pure aluminum powder by utilizing the hydrophilicity of the graphene oxide to obtain graphene oxide coated pure aluminum powder, the graphene oxide coated pure aluminum powder is pre-roasted at a low temperature under an inert gas or a reducing gas to reduce the graphene oxide into graphene, the graphene oxide coated pure aluminum powder is obtained, the graphene oxide coated pure aluminum powder and spherical aluminum alloy prefabricated powder are uniformly mixed to form graphene-aluminum alloy mixed powder, the graphene-aluminum alloy mixed powder is subjected to vacuum degassing and surface nitrogen increasing treatment, and finally, a powder metallurgy process is adopted to prepare a dense bulk composite material.
The invention comprises the following steps:
(1) Preparing pure aluminum powder and aluminum alloy pre-prepared powder;
(2) Preparing graphene coated pure aluminum powder: fully dissolving graphene oxide into hot water at the temperature of 90-100 ℃ to prepare a graphene oxide aqueous solution, mixing pure aluminum powder and the graphene oxide solution, fully stirring and mixing to ensure that the pure aluminum powder is completely infiltrated by the graphene oxide solution, and then dehydrating and drying in vacuum to obtain graphene oxide coated pure aluminum powder; placing the graphene oxide coated pure aluminum powder in an inert or reducing atmosphere for low-temperature pre-roasting, performing deoxidation reduction treatment on the graphene oxide, and obtaining graphene coated pure aluminum powder after reduction is completed;
(3) Preparing graphene-aluminum alloy composite powder: placing the graphene-coated pure aluminum powder and spherical aluminum alloy prefabricated powder into a mixer for mechanical mixing to obtain graphene-aluminum alloy composite powder meeting the component requirements;
(4) Surface nitrogen increasing treatment of the composite powder: putting the obtained graphene-aluminum alloy composite powder into a container to perform vacuum desorption treatment on the gas adsorbed on the surface of the powder, stopping vacuumizing when the vacuum degree reaches about 1Pa, refilling high-purity nitrogen until the vacuum degree reaches-0.03 MPa, then vacuumizing again to 1Pa, which is a desorption cycle, wherein the cycle is performed for at least 2 times; after the desorption treatment of the adsorbed gas is finished, re-filling high-purity nitrogen into the container filled with the graphene-aluminum alloy composite powder to one atmospheric pressure and keeping the atmospheric pressure for a proper time so as to realize the sufficient adsorption of the nitrogen on the surface of the graphene-aluminum alloy composite powder, and then removing the graphene-aluminum alloy composite powder with nitrogen added on the surface out of the vacuum container for later use;
(5) And (3) adopting a powder metallurgy process to carry out densification treatment on the graphene-aluminum alloy composite powder through the working procedures of forming, blank making, sintering, hot extrusion and the like, and finally obtaining the dense graphene reinforced aluminum alloy base composite material.
The pure aluminum powder is preferably prepared by a water atomization method, and the water atomization aluminum powder is characterized by fine powder particle size, irregular and rough appearance, which is beneficial for graphene oxide nanosheets to be better coated on the surface of the pure aluminum powder, and meanwhile, the irregular pure aluminum powder is also beneficial for obtaining a prefabricated blank with higher strength in the subsequent forming process; the aluminum alloy pre-prepared powder is preferably prepared by an inert gas atomization method, so that the oxidation burning loss of active elements such as magnesium and the like can be avoided, the accuracy of the components of the pre-prepared powder is better ensured, more spherical powder with high fluidity can be obtained, and the subsequent uniform mixing of graphene coated pure aluminum powder and the aluminum alloy pre-prepared powder is facilitated.
The graphene oxide has a single-layer or at most 5-layer graphite structure, and the thickness of the graphene oxide is less than 2nm.
The graphite oxide adopted by the invention contains more carboxyl, hydroxyl and other oxygen-containing groups on the surface, so that the graphite oxide is easy to disperse in hot water, a uniform graphene oxide aqueous solution can be prepared conveniently without the aid of other surfactants and the like, and meanwhile, the aqueous solution with higher graphene oxide content can be obtained, and the concentration of the graphene oxide can reach 100g/L.
Because the surface of the graphene oxide is modified with more oxygen-containing groups and defects, the oxygen-containing groups and the defects can influence the electrical and thermal properties of the graphene, in order to improve the electrical and thermal conductivity of the final composite material, the graphene oxide needs to be pre-baked at low temperature in an inert or reducing atmosphere, on one hand, the graphene oxide is subjected to deoxidation or reduction treatment, the adverse effect of the oxygen-containing groups on the electrical and thermal properties of the final composite material is reduced, on the other hand, the pre-baking can reduce the structural defects of the nano graphene sheet, promote the self-assembly growth of the nano graphene, and optimize the strengthening effect of the graphene nanosheet.
The published literature reports prove that the high-purity nitrogen environment is beneficial to sintering densification of the aluminum alloy, so that the obtained graphene-aluminum alloy composite powder is subjected to nitrogen increasing treatment on the surface, the adverse effect of harmful gases such as hydrogen, water vapor and the like adsorbed on the surface of the composite powder on the performance of an aluminum alloy-based composite material can be eliminated, and the uniform high-purity nitrogen sintering atmosphere can be obtained, the sintering performance of aluminum alloy powder is improved, and the uniformity of the texture performance of the sintered aluminum alloy is improved.
And (3) molding the obtained graphene-aluminum alloy composite powder to obtain a powder green body, then sintering to change the green body mechanically occluded between the powders into a sintered body metallurgically bonded between the powders, and then performing hot isostatic pressing, hot extrusion and other series of thermal deformation processing on the sintered body to finally obtain the dense graphene reinforced aluminum alloy matrix composite material.
Compared with the prior art, the invention has the following advantages: (1) The water atomized pure aluminum powder serving as one of the basic raw materials has the advantages of low cost and large specific surface area, and is suitable for large-scale green production; (2) Secondly, the irregular and rough shape is beneficial to uniform adsorption of graphene oxide, the rough aluminum powder can realize more zigzag occlusion joint surfaces during compression molding, a prefabricated green body with higher compressive strength can be obtained, and the mechanical production of powder metallurgy is facilitated; (3) Furthermore, the graphene oxide has good hydrophilicity, and the preparation of the graphene oxide solution can avoid the use of other organic solvents which have influence on the environment and have higher cost; (4) The surface nitrogen increasing treatment of the composite powder can effectively reduce the harmful effects of harmful gases such as hydrogen, water vapor and the like absorbed by the powder, and is beneficial to improving the performance of the composite material.
Drawings
FIG. 1 is a flow chart of a method for preparing a graphene reinforced aluminum alloy matrix composite;
fig. 2 is a graphene reinforced 7055 aluminum alloy extrusion rod of example 1 of the present invention.
Detailed Description
The following examples are given for the detailed implementation and the specific operation procedures, but the scope of the present invention is not limited to the following examples.
Table 1 shows the concentration of the graphene oxide solution, the aluminum alloy matrix component, and the aluminum alloy pre-powder component in each example, and is implemented according to the process flow of the graphene-reinforced aluminum alloy matrix composite material preparation method shown in fig. 1.
Table 1 examples graphene content, matrix composition and pre-powder composition
| Addition amount of graphene oxide | Main component of aluminum alloy matrix | Aluminum alloy pre-milling powder component | |
| Example 1 | 0.3wt％ | 7055-Al8Zn2Mg2.4Cu | Al20Zn5Mg6Cu |
| Example 2 | 0.5wt％ | 6061-Al1.0Mg0.6Si0.3Cu | Al2.5Mg1.5Si0.8Cu |
| Example 3 | 0.5wt％ | 2024-Al4.4Cu1.5Mg0.6Mn | Al11Cu4.0Mg1.5Mn |
The preparation method of the graphene reinforced aluminum alloy matrix composite material is shown in figure 1, and the specific process flow is as follows:
(1) Pure aluminum powder is obtained by a water atomization method, and then a standard sieve is used for sieving to obtain-200 meshes of aluminum powder for later use; preparing spherical aluminum alloy pre-prepared powder by an inert gas atomization method according to the components of the aluminum alloy pre-prepared powder shown in the table 1, and screening the spherical aluminum alloy pre-prepared powder by the same method to select-200 meshes of pre-prepared powder for later use;
(2) Preparing a graphene oxide aqueous solution: adding the weighed graphene oxide into a proper amount of hot water with the temperature of 80-95 ℃, and electromagnetically stirring for 30 minutes to fully dissolve the graphene oxide to prepare a graphene oxide aqueous solution;
(3) Preparing graphene coated pure aluminum powder: adding 3 kilograms of pure aluminum powder into a prepared graphene oxide aqueous solution, fully stirring and mixing to enable the pure aluminum powder to be completely infiltrated by the graphene oxide solution to obtain well-mixed graphene oxide pure aluminum powder slurry, then placing the slurry into a gypsum container to carry out preliminary dehydration on the slurry, then placing the preliminarily dehydrated graphene oxide pure aluminum powder mixture into a vacuum drying oven to carry out vacuum drying to obtain graphene oxide coated pure aluminum powder, placing the obtained graphene oxide coated pure aluminum powder in an inert or reducing atmosphere to carry out low-temperature pre-roasting, and enabling graphene oxide to carry out reduction and deoxidation reaction to obtain graphene coated pure aluminum powder;
(4) Preparing graphene-aluminum alloy composite powder: placing the graphene-coated pure aluminum powder and 2 kg of aluminum alloy prefabricated powder into a mixer for mechanical mixing, and uniformly mixing the graphene-coated pure aluminum powder and the aluminum alloy prefabricated powder to obtain graphene-aluminum alloy composite powder consisting of graphene, pure aluminum powder and aluminum alloy prefabricated powder;
(5) Surface nitrogen increasing treatment: placing the graphene-aluminum alloy composite powder in a sealed container for vacuumizing, stopping vacuumizing and keeping for 10 minutes when the vacuum degree of the sealed container reaches about 1Pa, then refilling high-purity nitrogen until the vacuum degree is-0.03 MPa, then vacuumizing again until the vacuum degree is 1Pa, and performing a desorption cycle, wherein the cycle is performed for at least 2 times so as to ensure that the gas adsorbed on the surface of the composite powder is desorbed and released as much as possible; after the desorption treatment of the adsorbed gas is finished, re-filling high-purity nitrogen into the container filled with the graphene-aluminum alloy composite powder to one atmospheric pressure and keeping the atmospheric pressure for a proper time so as to realize the sufficient adsorption of the nitrogen on the surface of the graphene-aluminum alloy composite powder, and then removing the graphene-aluminum alloy composite powder with nitrogen added on the surface from the vacuum container for later use;
(6) Preparing a graphene reinforced aluminum alloy base composite material: carrying out cold isostatic pressing on the graphene-aluminum alloy composite powder subjected to surface nitrogen increasing treatment under the pressure of 200MPa to form a cylindrical blank with the diameter of 90 mm, then sintering the cylindrical blank at 600 ℃ for 2 hours under the protection of nitrogen to obtain a sintered blank, and carrying out hot extrusion on the sintered blank at 400 ℃ with the extrusion ratio of 20: 1 to obtain the dense graphene/aluminum composite material.
The relative properties of the graphene-aluminum alloy-based composite material prepared according to the preparation method are shown in table 2.
TABLE 2 graphene reinforced aluminum alloy based composites Performance
| Example 1 | Reference example 1 | Example 2 | Reference ratio 2 | Example 3 | Reference example 3 | |
| Tensile strength/MPa | 709 | 663 | 355 | 310 | 524 | 485 |
| Yield strength/MPa | 693 | 644 | 330 | 285 | 416 | 375 |
| Elongation/percent | 6.18 | 6.3 | 9.1 | 10 | 12.4 | 15 |
It is obvious that the disclosure of the present invention has been made in detail by the above embodiments, but the above embodiments are only examples for clearly illustrating the invention, and are not limitative to the invention, and all embodiments need not be exhaustive. From the foregoing, it will be appreciated by those skilled in the art that changes and modifications may be made in the foregoing without departing from the principles of the invention, and it is intended to cover such changes and modifications as fall within the true spirit and scope of the invention.
Claims (3)
1. A preparation method of a graphene reinforced aluminum alloy base composite material is characterized by comprising the following steps of firstly preparing graphene-aluminum alloy composite powder; secondly, performing surface nitrogen increasing treatment on the graphene-aluminum alloy composite powder; and thirdly, carrying out processing such as molding, sintering, hot extrusion and the like on the composite powder after nitrogen addition to obtain the graphene reinforced aluminum alloy matrix composite material.
2. The method for preparing the graphene reinforced aluminum alloy matrix composite material as claimed in claim 1, wherein the graphene-aluminum alloy composite powder is composed of pure aluminum powder, aluminum alloy pre-milled powder and graphene, wherein the weight ratio of the pure aluminum powder is 55-75%.
3. The method for preparing graphene reinforced aluminum alloy matrix composite material according to claim 1, comprising the following specific steps:
(1) Preparing the aluminum alloy pre-prepared powder by inert gas atomization;
(2) Preparing pure aluminum powder coated by graphene;
(3) Preparing graphene-aluminum alloy composite powder;
(4) Carrying out surface nitrogen increasing treatment on the graphene-aluminum alloy composite powder;
(5) And preparing the graphene reinforced aluminum alloy base composite material by powder metallurgy.
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