CN115478187B - Preparation method of graphene reinforced aluminum alloy matrix composite - Google Patents
Preparation method of graphene reinforced aluminum alloy matrix composite Download PDFInfo
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- 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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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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Abstract
The invention discloses a preparation method of a graphene reinforced aluminum alloy matrix composite material, which comprises the steps of firstly preparing an aluminum alloy pre-powder by gas atomization, then preparing graphene coated pure aluminum powder, then mixing the graphene coated pure aluminum powder and the aluminum alloy pre-powder into graphene-aluminum alloy composite powder, carrying out surface nitrogen increasing treatment on the graphene-aluminum alloy composite powder to improve and improve the sintering performance of the composite powder, and finally preparing the graphene reinforced aluminum alloy matrix composite material by adopting powder metallurgy processing such as molding, sintering, hot extrusion and the like. The preparation 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 matrix composite material, in particular to a preparation method of a graphene/aluminum alloy composite material.
Background
Graphene is an sp which has been found in recent years 2 Novel two-dimensional planar nano material formed by hybridized carbon atom close-packed has huge specific surface area (up to 2630m 2 Per gram), ultra-high carrier mobility (15000-25000 cm) 2 Vs), thermal conductivity (4840-5300W/mK), young's modulus (1000 GPa), and breaking strength (130 GPa), and a forbidden band width equal to about 0, exhibit excellent electrical, thermal, and mechanical properties, making it one of the most desirable reinforcements for metal-based nanocomposites.
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 the main direction of research on aluminum alloys. At present, the traditional casting metallurgical method such as adjusting the components of the aluminum alloy, optimizing the thermomechanical deformation processing and the heat treatment system and the like encounters a bottleneck in improving the performance of the aluminum alloy. The preparation of high-performance aluminum-based composite materials by using graphene as a reinforcement is an important direction in the current research of high-performance aluminum alloys.
Patent document CN111101172a discloses a graphene-aluminum composite material and a preparation method thereof, the preparation method comprises: firstly preparing a graphene aerosol cathode, adopting graphene aerogel as a cathode, adopting metal aluminum as an anode, placing the anode and the cathode in molten electrolyte (the electrolyte consists of sodium chloride, potassium chloride and aluminum chloride with different proportions), and carrying out electrolysis under the electrolysis current of 250 mA-350 mA to obtain the graphene aluminum composite material. The graphene aerosol in this document is costly and energy-consuming to prepare, and at the same time, electrolysis of NaCl and the like produces 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 and hot isostatic pressing sintering to prepare blanks and hot extrusion molding of the blanks. The method firstly consumes a great deal of time to carry out mixing and has long low-temperature ball milling process, 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 distribution adopts layered distribution, and a graphene layer is placed at the middle position. The method is characterized in that aluminum particles are needed, so that the type of raw materials is difficult to realize in large-scale production, and the general large-scale production adopts more than 10 kg of aluminum ingots; on the other hand, the density difference between the aluminum alloy melt and the graphene is larger, and the graphene is inevitably floated on the surface of the aluminum alloy melt in the aluminum alloy smelting process, so that the loss and the uneven distribution of the graphene in the aluminum alloy preparation process are caused.
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 problem is that the graphene coats aluminum alloy powder to sinter and densify, firstly, because the continuous dense oxide film on the surface of the aluminum alloy powder leads to poor sintering performance, and secondly, the graphene sheets prevent diffusion migration of aluminum atoms and the reactivity of carbon materials is not high, which also worsens the sintering performance of the aluminum alloy powder and reduces densification of the aluminum alloy powder.
The literature reports that adding trace amounts of low-melting metal powder such as tin, lead and the like or adding boron oxide powder (patent document CN 104999074B) can effectively destroy the oxide film to promote the improvement of the sintering density of the aluminum alloy, but Sn and Pb particles and brittle boron glass formed in the sintering process can reduce the strength or the plastic toughness of the aluminum alloy composite material. Higher sintering density can be obtained by sintering in high-purity nitrogen atmosphere, 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 the powder particles on the nitrogen in the core of the green body, so that the difference of the amount of the adsorbed nitrogen of the powder can influence the sintering behavior of the powder, further, the performance gradient is generated in the sintered composite material, and the performance gradient is more obvious for a large-size sintered product.
In view of the above, the preparation method of the powder metallurgy graphene reinforced aluminum matrix composite needs to be further improved. Aiming at the defects in the preparation of the graphene reinforced aluminum-based composite material, the invention provides an effective green preparation method of the graphene reinforced aluminum-based composite material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing a graphene reinforced aluminum alloy matrix composite based on a powder metallurgy technology. According to the invention, pure aluminum powder and spherical aluminum alloy pre-prepared powder are used as matrix materials, and graphene oxide nano-sheets are used as precursors of graphene reinforcements to adjust the uniformity of graphene distribution in the aluminum alloy matrix composite.
The invention is realized by the following technical scheme:
according to the invention, firstly, the hydrophilicity of graphene oxide is utilized to coat the graphene oxide on the surface of pure aluminum powder to obtain graphene oxide coated pure aluminum powder, then the graphene oxide coated pure aluminum powder is pre-baked at low temperature under inert gas or reducing gas, so that graphene oxide is reduced into graphene to obtain graphene coated pure aluminum powder, then the graphene coated pure aluminum powder and spherical aluminum alloy prefabricated powder are uniformly mixed to obtain 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 compact massive composite material.
The invention comprises the following steps:
(1) Preparing pure aluminum powder and aluminum alloy pre-powder;
(2) Preparing pure aluminum powder coated by graphene: fully dissolving graphene oxide into hot water at 90-100 ℃ to prepare 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 fully infiltrated by the graphene oxide solution, and then dehydrating and vacuum drying to obtain graphene oxide coated pure aluminum powder; pre-roasting graphene oxide coated pure aluminum powder at a low temperature in an inert or reducing atmosphere, and carrying out deoxidization and reduction treatment on the graphene oxide to obtain graphene coated pure aluminum powder after reduction;
(3) Preparing graphene-aluminum alloy composite powder: placing the graphene coated pure aluminum powder and the spherical aluminum alloy pre-prepared powder into a mixer for mechanical mixing to obtain graphene-aluminum alloy composite powder meeting component requirements;
(4) Surface nitrogen increasing treatment of composite powder: placing the obtained graphene-aluminum alloy composite powder into a container for vacuum desorption treatment of adsorbing gas on the surface of the powder, stopping vacuumizing when the vacuum degree reaches about 1Pa, recharging high-purity nitrogen until the vacuum degree reaches-0.03 MPa, and vacuumizing again to 1Pa, wherein the vacuum desorption treatment is a desorption cycle which is carried out for at least 2 times; after the adsorption gas desorption treatment is completed, high-purity nitrogen is again filled into a container filled with the graphene-aluminum alloy composite powder to one atmosphere and kept for a proper time, so that the nitrogen is fully adsorbed on the surface of the graphene-aluminum alloy composite powder, and then the graphene-aluminum alloy composite powder with the nitrogen added on the surface is removed from the vacuum container for standby;
(5) And (3) performing densification treatment on the graphene-aluminum alloy composite powder by adopting a powder metallurgy process in the working procedures of forming, blank making, sintering, hot extrusion and the like, and finally obtaining the compact graphene reinforced aluminum alloy matrix composite material.
The pure aluminum powder is preferably prepared by a water atomization method, and the water atomized aluminum powder is characterized in that the powder has fine granularity, irregular and rough appearance, so that graphene oxide nano sheets are better coated on the surface of the pure aluminum powder, and meanwhile, the irregular pure aluminum powder is also favorable for obtaining a preform with higher strength in a subsequent forming process; the aluminum alloy pre-powder is preferably prepared by an inert gas atomization method, so that firstly, oxidation burning loss of active elements such as magnesium can be avoided, the accuracy of the components of the pre-powder is well ensured, secondly, more spherical powder with high fluidity can be obtained, and the subsequent uniform mixing of the graphene coated pure aluminum powder and the aluminum alloy pre-powder is facilitated.
The graphene oxide has a single-layer or at most 5-layer graphite structure, and the thickness is less than 2nm.
The surface of the graphite oxide adopted by the invention contains more oxygen-containing groups such as carboxyl, hydroxyl and the like, so that the graphite oxide is easy to disperse in hot water, a uniform graphene oxide aqueous solution is conveniently prepared without 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 graphene oxide surface is modified with more oxygen-containing groups and defects, the oxygen-containing groups and defects can influence the electrical and thermal properties of graphene, in order to improve the electrical and thermal conductivity of the final composite material, the graphene oxide needs to be subjected to low-temperature pre-baking in an inert or reducing atmosphere, on one hand, the graphene oxide is subjected to deoxidization or reduction treatment, the adverse influence 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 sheets and promote the self-assembly growth of the nano graphene, and the strengthening effect of the graphene nano sheets is optimized.
The published literature reports prove that the high-purity nitrogen environment is favorable for sintering densification of the aluminum alloy, so that the surface of the obtained graphene-aluminum alloy composite powder is subjected to nitrogen increasing treatment, firstly, adverse effects of harmful gases such as hydrogen, water vapor and the like adsorbed on the surface of the composite powder on the performance of the aluminum alloy matrix composite material can be eliminated, secondly, uniform high-purity nitrogen sintering atmosphere is favorable, the sintering performance of the aluminum alloy powder is improved, and the uniformity of the structure performance of the sintered aluminum alloy is improved.
And (3) firstly forming the obtained graphene-aluminum alloy composite powder to obtain a powder green body, then sintering the powder green body to enable the green body which is mechanically occluded between the powders to be changed into a sintered body which is 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 compact graphene reinforced aluminum alloy matrix composite material.
Compared with the prior art, the invention has the following advantages: (1) Firstly, 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 morphology is favorable for uniformly adsorbing graphene oxide, and rough aluminum powder can realize more tortuous occlusion joint surfaces during compression molding, so that prefabricated green bodies 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 other organic solvents with higher cost and influence on the environment can be avoided from being used for preparing the graphene oxide solution; (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 adsorbed by the powder, and is beneficial to the improvement of the performance of the composite material.
Drawings
FIG. 1 is a flow chart of a preparation method of a graphene reinforced aluminum alloy-based composite material;
fig. 2 is a graphene reinforced 7055 aluminum alloy extruded rod of example 1 of the present invention.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Table 1 shows the concentration of graphene oxide solution, the matrix composition of aluminum alloy, and the composition of aluminum alloy preform powder in each example, and was performed according to the process flow of the preparation method of graphene-reinforced aluminum alloy-based composite material shown in fig. 1.
Table 1 example graphene content, matrix composition, and pre-powder composition
| Graphene oxide addition amount | Main component of aluminum alloy matrix | Aluminum alloy pre-powder composition | |
| 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 fig. 1, and the specific process comprises the following steps:
(1) Pure aluminum powder is obtained by a water atomization method, and then is screened by a standard screen to obtain-200 meshes of aluminum powder for standby; preparing spherical aluminum alloy pre-powder by inert gas atomization according to the aluminum alloy pre-powder components shown in table 1, screening the spherical aluminum alloy pre-powder, and selecting-200-mesh pre-powder for later use;
(2) Preparing graphene oxide aqueous solution: adding weighed graphene oxide into a proper amount of hot water at 80-95 ℃ and carrying out electromagnetic stirring for 30 minutes to enable the graphene oxide to be fully dissolved, so as to prepare a graphene oxide aqueous solution;
(3) Preparing pure aluminum powder coated by graphene: adding 3 kg of pure aluminum powder into the prepared graphene oxide aqueous solution, fully stirring and mixing to ensure that the pure aluminum powder is completely infiltrated by the graphene oxide solution, obtaining well mixed graphene oxide pure aluminum powder slurry, then placing the obtained slurry into a gypsum container for preliminary dehydration of the slurry, then placing the preliminarily dehydrated graphene oxide pure aluminum powder mixture into a vacuum drying box for vacuum drying to obtain graphene oxide coated pure aluminum powder, and placing the obtained graphene oxide coated pure aluminum powder into an inert or reducing atmosphere for low-temperature pre-roasting to ensure that the graphene oxide undergoes a reduction deoxidization 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 pre-prepared powder into a mixer for mechanical mixing, and obtaining graphene-aluminum alloy composite powder composed of graphene, pure aluminum powder and aluminum alloy pre-prepared powder after the graphene coated pure aluminum powder and the 2 kg of aluminum alloy pre-prepared powder are uniformly mixed;
(5) Surface nitrogen increasing treatment: placing the graphene-aluminum alloy composite powder in a sealed container for vacuumizing, stopping vacuumizing when the vacuum degree of the sealed container reaches about 1Pa, keeping for 10 minutes, then recharging high-purity nitrogen until the vacuum degree is-0.03 MPa, and vacuumizing again to 1Pa, wherein the cycle is a desorption cycle which is performed for at least 2 times to ensure that the gas adsorbed on the surface of the composite powder is desorbed and released as much as possible; after the adsorption gas desorption treatment is completed, the high-purity nitrogen is again filled into a container filled with the graphene-aluminum alloy composite powder to one atmosphere and kept for a proper time, so that the nitrogen is fully adsorbed on the surface of the graphene-aluminum alloy composite powder, and then the graphene-aluminum alloy composite powder with the nitrogen added on the surface is removed from the vacuum container for standby;
(6) Preparing a graphene reinforced aluminum alloy matrix composite: and (3) carrying out cold isostatic pressing on the graphene-aluminum alloy composite powder with the 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 ℃ to obtain the compact graphene/aluminum composite material with the extrusion ratio of 20:1.
The relevant 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 matrix composite properties
| Example 1 | Reference example 1 | Example 2 | Reference example 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/% | 6.18 | 6.3 | 9.1 | 10 | 12.4 | 15 |
It is to be understood that the present disclosure has been described in detail by way of the foregoing examples, which are provided by way of illustration only and not by way of limitation, and not necessarily all embodiments. Various other changes and modifications may be made by those skilled in the art in light of the foregoing disclosure without departing from the principles of the present invention, and it is intended that all such changes and modifications as fall within the scope of the invention.
Claims (2)
1. The preparation method of the graphene reinforced aluminum alloy matrix composite material is characterized by comprising the steps of firstly preparing graphene-aluminum alloy composite powder; secondly, carrying out surface nitrogen increasing treatment on the graphene-aluminum alloy composite powder; thirdly, forming, sintering and hot extrusion processing are carried out on the graphene-aluminum alloy composite powder after nitrogen addition to prepare the graphene reinforced aluminum alloy-based composite material, and the preparation method of the graphene-aluminum alloy composite powder and the nitrogen addition on the surface thereof are as follows:
(1) Graphene oxide coats pure aluminum powder: completely dissolving graphene oxide into hot water at 90-100 ℃ to prepare graphene oxide aqueous solution, mixing and fully stirring required pure aluminum powder and the graphene oxide solution according to the component requirements of the aluminum-based composite material to enable the pure aluminum powder to be completely infiltrated by the graphene oxide solution, and then dehydrating and vacuum drying to obtain graphene oxide coated pure aluminum powder;
(2) Deoxidizing reduction of graphene oxide: placing pure aluminum powder coated with graphene oxide in inert or reducing atmosphere for low-temperature pre-roasting to deoxidize and reduce the graphene oxide into graphene, so as to obtain graphene coated pure aluminum powder;
(3) Mixing of graphene coated pure aluminum powder and aluminum alloy pre-prepared powder: mixing the graphene coated pure aluminum powder obtained in the step (2) with spherical aluminum alloy pre-powder in a mixer to obtain graphene-aluminum alloy composite powder meeting the component requirements of an aluminum-based composite material;
(4) Degassing treatment of graphene-aluminum alloy composite powder: placing the composite powder obtained in the step (3) into a sealed container for vacuum desorption treatment of the powder surface adsorption gas, stopping vacuumizing when the vacuum degree reaches 1Pa, recharging high-purity nitrogen until the vacuum degree reaches-0.03 MPa, and vacuumizing again to 1Pa, wherein the vacuum desorption treatment is a vacuum desorption cycle which is carried out for at least 2 times so as to fully realize the vacuum desorption of the adsorption gas;
(5) Nitrogen is added on the surface of the graphene-aluminum alloy composite powder: and (3) after the step (4) is finished, the container is refilled with high-purity nitrogen to one atmosphere and kept for proper time, so that the nitrogen is fully adsorbed on the surface of the graphene-aluminum alloy composite powder, the surface nitrogen increasing treatment of the composite powder is finished, and then the graphene-aluminum alloy composite powder with the surface nitrogen increasing effect is removed from the vacuum container for standby.
2. The method for preparing the graphene-reinforced aluminum alloy-based composite material according to claim 1, wherein the graphene-aluminum alloy composite powder consists of pure aluminum powder, aluminum alloy pre-powder and graphene, and the weight ratio of the pure aluminum powder is 55-75%.
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