Micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material and preparation method thereof

Abstract

The invention belongs to the technical field of metal-based composite materials and powder metallurgy, and particularly relates to a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material and a preparation method thereof.The micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material comprises an aluminum alloy matrix and a reinforced phase evenly dispersed and distributed in the aluminum alloy matrix; the aluminum alloy matrix is an Al-Cu-Mg-Si alloy, and the reinforcing phase comprises micron-scale ceramic particles, nano-scale ceramic particles and graphene. The prepared micro-nano hybrid ceramic particle and graphene reinforced aluminum matrix composite comprises an aluminum alloy matrix, and micron-scale ceramic particles, nano-scale ceramic particles and graphene which are uniformly dispersed and distributed in the aluminum alloy matrix, the micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material has the advantages of high strength, high rigidity, good plasticity, low density and the like.

Description

Technical Field

[0001] The present invention belongs to the technical field of metal-based composite materials and powder metallurgy, and specifically relates to a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material and a preparation method thereof. Background Art

[0002] Particle-reinforced aluminum-based composites are a new type of strategic material with excellent comprehensive properties such as low density, high strength, high toughness, high modulus, fatigue resistance, and low expansion. They are important materials for achieving lightweight and high-performance structural parts in the aerospace, automotive, and 3C electronics fields. The aluminum alloy matrix is ​​usually 2xxxAl, 6xxxAl, or 7xxxAl aluminum alloy, and the reinforcing particles are usually micron-sized ceramic particles such as silicon carbide (SiC) and titanium diboride (TiB2). Although micron-sized ceramic particles can improve the strength and stiffness of the material while maintaining a certain degree of plasticity, with the higher requirements for material strength in high-tech fields, traditional particle-reinforced aluminum-based composites can no longer meet the performance index requirements of high-strength and toughness load-bearing structural parts.

[0003] Since the strength of aluminum-based composites reinforced with micron-ceramic particles is usually low, in recent years, more and more scholars have begun to study graphene-doped aluminum-based composites, nano-ceramic particle-doped and micro-nano hybrid aluminum-based composites. Although adding graphene and nano-ceramic particles to aluminum-based composites can improve the strength and stiffness of the material to a certain extent, due to the significant differences between graphene and aluminum alloy powders in terms of morphology and specific gravity, traditional powder mixing methods are also difficult to achieve uniform mixing of the two, and the introduction of high-energy mixing media can easily destroy the structural integrity of the graphene itself. Similarly, because the nano-ceramic particles are too small and have a large surface energy, and at the same time, they differ greatly from the particle size of the matrix powder, nano-ceramic particles are more likely to agglomerate during the powder mixing process, resulting in no significant improvement in material performance. Aluminum-based composites prepared by adding graphene or nano-ceramic particles usually have poor plasticity. Summary of the Invention

[0004] The purpose of the present invention is to provide a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material and a preparation method. The micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material in the present invention includes an aluminum alloy matrix and a reinforcing phase uniformly dispersed in the aluminum alloy matrix, and the reinforcing phase includes micron-sized ceramic particles, nano-sized ceramic particles and graphene, giving full play to the strengthening effect of the three reinforcing phases, so that the micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material has the advantages of high strength, high stiffness, good plasticity and low density.

[0005] The first aspect of the present invention provides a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material, which includes an aluminum alloy matrix and a reinforcing phase uniformly dispersed in the aluminum alloy matrix, wherein the aluminum alloy matrix is ​​an Al-Cu-Mg-Si alloy, and the reinforcing phase includes micron-sized ceramic particles, nano-sized ceramic particles and graphene; the volume percentage of the aluminum alloy matrix is ​​70% to 89%, the volume percentage of the micron-sized ceramic particles is 10% to 20%, the volume percentage of the nano-sized ceramic particles is 0.5% to 6%, and the volume percentage of the graphene is 0.5% to 4%.

[0006] In some embodiments of the present invention, the Al-Cu-Mg-Si alloy includes the following components in weight percentage:

[0007] Cu 0.15%~1.0%, Mg 0.8%~1.5%, Si 0.4%~1.2%, and the balance is Al.

[0008] In some embodiments of the present invention, the nano-scale ceramic particles include at least one of Y2O3, MgO, TiB2, and B4C; and / or the average particle size D50 of the nano-scale ceramic particles is 30 nm to 100 nm.

[0009] In some embodiments of the present invention, the micron-sized ceramic particles include at least one of SiC, B4C, and TiB2; and / or the average particle size D50 of the micron-sized ceramic particles is 5.0 μm to 30.0 μm.

[0010] The second aspect of the present invention also provides a method for preparing the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material described in the first aspect, which includes the following steps: mechanically alloying and mixing Al-Cu-Mg-Si atomized powder with nano-scale ceramic particles, so that the nano-scale ceramic particles are embedded in the Al-Cu-Mg-Si atomized powder to obtain mechanically alloyed powder; mixing the mechanically alloyed powder with graphene and micron-scale ceramic particles using a high-efficiency acoustic resonance method to conduct energy through vibration, so that the graphene and micron-scale ceramic particles are uniformly dispersed in the Al-Cu-Mg-Si atomized powder to obtain a composite powder; cold isostatic pressing, vacuum degassing and hot isostatic pressing of the composite powder to obtain a sintered blank; extrusion molding and heat treatment of the sintered blank to obtain the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material.

[0011] In some embodiments of the present invention, during the mechanical alloying mixing process, the total mass of the Al-Cu-Mg-Si atomized powder and the nano-ceramic particles to the grinding ball ratio is 10:1 to 30:1, the ball mill speed is 200 r / min to 500 r / min, and the mixing time is 5 h to 30 h.

[0012] In some embodiments of the present invention, protective gas is introduced during the high-efficiency acoustic resonance mixing process, the vibration acceleration is 10g to 60g, and the mixing time is 30min to 90min.

[0013] In some embodiments of the present invention, the protective gas includes one of nitrogen and argon.

[0014] In some embodiments of the present invention, the pressure of the cold isostatic pressing is 60 MPa to 100 MPa, and the holding time is 0.5 h to 3.0 h.

[0015] In some embodiments of the present invention, the vacuum degassing temperature is 420°C to 550°C, and the sealing vacuum degree satisfies ≤10 -2 Pa; the metal sheath material used in the vacuum degassing includes one of copper alloy and aluminum alloy.

[0016] In some embodiments of the present invention, the hot isostatic pressing sintering is performed under a pressure of 80 MPa to 200 MPa, a temperature of 420° C. to 550° C., and a holding time of 1.0 h to 3.0 h.

[0017] In some embodiments of the present invention, the heating temperature of the extruded billet is 420° C. to 550° C., the temperature of the extrusion die is 420° C. to 550° C., and the extrusion ratio is 10:1 to 30:1.

[0018] In some embodiments of the present invention, the heat treatment includes solution aging treatment, wherein the solution temperature is 420°C to 550°C, the solution holding time is 1.0h to 3.0h, the quenching transfer time is less than 20s, the water cooling temperature is 20°C to 30°C; the aging temperature is 150°C to 200°C, and the aging holding time is 5h to 15h.

[0019] In some embodiments of the present invention, the preparation of the Al-Cu-Mg-Si atomized powder includes: vacuum melting Al ingots, Cu ingots, Mg ingots, and Al-Si master alloys to prepare Al-Cu-Mg-Si alloy ingots; and gas atomizing and powdering the Al-Cu-Mg-Si alloy ingots to obtain the Al-Cu-Mg-Si atomized powder.

[0020] In some embodiments of the present invention, the vacuum melting temperature of the Al-Cu-Mg-Si alloy ingot is 700°C to 900°C, and the vacuum degree is ≤10 -2 Pa.

[0021] In some embodiments of the present invention, during the gas atomization powder making process, the billet melting heating temperature is 700° C. to 900° C., the gas atomization pouring temperature is 700° C. to 900° C., and the holding time is 10 min to 30 min.

[0022] Because aluminum-based composites reinforced with micron-sized ceramic particles typically have low strength, the addition of nano-sized ceramic particles and graphene can improve their strength. However, the resulting materials often exhibit poor plasticity and are prone to agglomeration during the powder mixing process, hindering overall performance improvements. The preparation method of the present invention can mitigate the agglomeration that occurs during the mixing of aluminum-based composite powders after the addition of reinforcing phases such as nano-sized ceramic particles and graphene. On the one hand, the mechanical alloying mixing method can overcome the problem that the nano-ceramic particles are too small and prone to agglomeration, and the nano-ceramic particles can be embedded in the aluminum alloy matrix powder to play a better role in intracrystalline and grain boundary strengthening; on the other hand, the high-efficiency acoustic resonance method is used to mix graphene, and energy is transmitted through vibration without relying on the mixing medium. On the basis of not destroying the structure of graphene itself, the problem of uneven mixing caused by the large difference in specific gravity between graphene and aluminum alloy matrix powder is solved; at the same time, micron-sized ceramic particles are added, and the graphene and micron-sized ceramic particles are evenly dispersed in the aluminum alloy matrix powder through the high-efficiency acoustic resonance method. Finally, the graphene is directional arranged through extrusion deformation, which further improves the dispersion uniformity of graphene in aluminum-based composite materials, solves the problem of poor compatibility, and improves the comprehensive performance of the material.

[0023] Traditional ball-milled powder mixing cannot achieve uniform dispersion of nano-ceramic particles and graphene, failing to achieve the desired strengthening effect. Mechanical alloying alone destroys the structural integrity of the graphene, significantly reducing the strengthening effect. Similarly, using only high-efficiency acoustic resonance mixing results in the majority of the nanophase being distributed on the surface of the aluminum alloy powder, failing to achieve intragranular and grain boundary strengthening, and the amount of nano-ceramic particles added is limited.

[0024] A powder mixing method combining mechanical alloying and high-efficiency acoustic resonance is used instead of traditional ball milling mixing, avoiding the agglomeration problem caused by adding nano-ceramic particles and graphene in the traditional powder mixing method. Without destroying the structure of graphene itself, the uniform dispersion distribution of nano-ceramic particles, graphene and micron-sized ceramic particles in the aluminum alloy matrix is ​​achieved, and the strengthening effect of the three reinforcing phases is fully utilized to prepare a high-strength, high-rigidity, good plasticity and low-density micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material.

[0025] In the present invention, micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite materials are prepared by mechanical alloying and high-efficiency resonance mixing. The prepared composite material includes an aluminum alloy matrix and micron-sized ceramic particles, nano-sized ceramic particles and graphene uniformly dispersed in the aluminum alloy matrix, so that the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite materials have the advantages of high strength, high stiffness, good plasticity and low density.

[0026] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are specifically listed below. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the specific embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0028] Figure 1 This is SEM photograph 1 of the composite powder obtained after mechanical alloying and high-efficiency acoustic resonance mixing in Example 1 of the present invention.

[0029] Figure 2 This is the second SEM photograph of the composite powder obtained after mechanical alloying and high-efficiency acoustic resonance mixing in Example 1 of the present invention.

[0030] Figure 3 Schematic diagram of the structure of the composite powder obtained after mechanical alloying and high-efficiency acoustic resonance mixing in the present invention.

[0031] Figure 4 Schematic diagram of high-efficiency acoustic resonance mixing in Examples 1 to 2 and Comparative Example 2 of the present invention.

[0032] Figure 5 This is a flow chart of the preparation process of the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material in an embodiment of the present invention.

[0033] Description of reference numerals:

[0034] 1-Al-Cu-Mg-Si atomized powder; 2-micron-sized ceramic particles; 3-nanoscale ceramic particles; 4-graphene; 5-composite powder; 6-high-efficiency acoustic resonance mixing container; 7-material mixing flow; 8-vibration platform. DETAILED DESCRIPTION

[0035] Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although exemplary embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments described herein. Rather, these embodiments are provided to enable a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art.

[0036] It should be understood that the terms used herein are for the purpose of describing specific example embodiments only and are not intended to be limiting. Unless the context clearly indicates otherwise, the singular forms "one", "an" and "said" as used herein may also be meant to include plural forms. The terms "comprise", "include", "contain" and "have" are inclusive and therefore specify the presence of stated features, steps, operations, elements and / or parts, but do not exclude the presence or addition of one or more other features, steps, operations, elements, parts, and / or combinations thereof. The method steps, processes, and operations described herein are not to be construed as necessarily requiring them to be performed in the specific order described or illustrated, unless the order of execution is clearly indicated. It should also be understood that additional or alternative steps may be used.

[0037] In the description of the embodiments of the present invention, technical terms such as "first" and "second" are used solely to distinguish between different objects and should not be understood to indicate or imply relative importance or to implicitly specify the quantity, specific order, or primary and secondary relationship of the technical features indicated. In the description of the embodiments of the present invention, "plurality" means more than two, unless otherwise specifically defined.

[0038] References herein to "embodiments" mean that a particular feature, structure, or characteristic described in connection with the embodiments may be included in at least one embodiment of the present invention. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor does it constitute a separate or alternative embodiment that is mutually exclusive of other embodiments. It is understood, both explicitly and implicitly, by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0039] In the description of the embodiments of the present invention, the term "and / or" is simply a description of the association relationship between associated objects, indicating that three relationships can exist. For example, A and / or B can represent the following three situations: A exists alone, A and B exists simultaneously, and B exists alone. In addition, the character " / " in this document generally indicates that the associated objects are in an "or" relationship.

[0040] In the description of the embodiments of the present invention, the term "multiple" refers to more than two (including two). Similarly, "multiple groups" refers to more than two groups (including two groups), and "multiple pieces" refers to more than two pieces (including two pieces).

[0041] In the description of the embodiments of the present invention, unless otherwise expressly specified or limited, technical terms such as "installed," "connected," "connect," and "fixed" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integration; mechanical connections or electrical connections; direct connections or indirect connections through an intermediate medium; and can refer to internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the embodiments of the present invention based on specific circumstances.

[0042] Currently, the strength of aluminum-based composites reinforced with micron-sized ceramic particles is generally low. Nano-sized ceramic particles and graphene can significantly improve the strength of aluminum-based composites, but the resulting materials have relatively poor plasticity. Currently, there is no effective powder mixing and preparation method for adding micron-sized ceramic particles, nano-sized ceramic particles, and graphene to aluminum-based composites. The main purpose of the present invention is to achieve hybrid reinforcement of micron-sized and nano-sized ceramic particles through material design, while also adding a certain amount of graphene to produce an aluminum-based composite with ultra-high strength and high plasticity.

[0043] The first aspect of the present invention provides a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material, which includes an aluminum alloy matrix and a reinforcing phase uniformly dispersed in the aluminum alloy matrix, wherein the aluminum alloy matrix is ​​an Al-Cu-Mg-Si alloy, and the reinforcing phase includes micron-sized ceramic particles, nano-sized ceramic particles and graphene; the volume percentage of the aluminum alloy matrix is ​​70% to 89%, the volume percentage of the micron-sized ceramic particles is 10% to 20%, the volume percentage of the nano-sized ceramic particles is 0.5% to 6%, and the volume percentage of the graphene is 0.5% to 4%.

[0044] In an embodiment of the present invention, the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material consists of an aluminum alloy matrix and a reinforcing phase. The reinforcing phase includes micron-sized ceramic particles, nano-sized ceramic particles and graphene. The nano-sized ceramic particles, graphene and micron-sized ceramic particles are uniformly dispersed in the aluminum alloy matrix, giving full play to the strengthening effect of the three reinforcing phases.

[0045] In an embodiment of the present invention, the volume percentage of the aluminum alloy matrix is ​​70% to 89%. For example, the volume percentage of the aluminum alloy matrix can be one of 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, or any value that meets the above range.

[0046] In an embodiment of the present invention, the volume percentage of the micron-sized ceramic particles is 10% to 20%. For example, the volume percentage of the micron-sized ceramic particles can be one of 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, or any value within the above range.

[0047] In an embodiment of the present invention, the volume percentage of the nano-scale ceramic particles is 0.5% to 6%. For example, the volume percentage of the nano-scale ceramic particles can be one of 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.5%, 1.8%, 2%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 4.8%, 5%, 5.2%, 5.5%, 5.8%, 6%, or any value within the above range.

[0048] In an embodiment of the present invention, the volume percentage of graphene is 0.5% to 4%. Exemplarily, the volume percentage of graphene is one of 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.5%, 1.8%, 2%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, or any value within the above range.

[0049] In some embodiments of the present invention, the Al-Cu-Mg-Si alloy includes the following components in weight percentage: Cu 0.15% to 1.0%, Mg 0.8% to 1.5%, Si 0.4% to 1.2%, and the balance is Al.

[0050] The mass percentage of Cu in the Al-Cu-Mg-Si alloy provided by the present invention can be one of 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95%, 1.0%, or any value that meets the above range.

[0051] The mass percentage of Mg in the Al-Cu-Mg-Si alloy provided by the present invention can be one of 0.8%, 0.85%, 0.9%, 0.95%, 1.0%, 1.2%, 1.4%, 1.5% or any value that meets the above range.

[0052] The mass percentage of Si in the Al-Cu-Mg-Si alloy provided by the present invention can be one of 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2% or any value that meets the above range.

[0053] In an embodiment of the present invention, the nano-scale ceramic particles include at least one of Y2O3, MgO, TiB2, and B4C.

[0054] In an embodiment of the present invention, the average particle size D50 of the nano-scale ceramic particles is 30 nm to 100 nm. For example, the average particle size D50 of the nano-scale ceramic particles can be one of 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, and 100 nm, or any value within the above range.

[0055] In an embodiment of the present invention, the micron-sized ceramic particles include at least one of SiC, B4C, and TiB2.

[0056] In an embodiment of the present invention, the average particle size D50 of the micron-sized ceramic particles is 5.0 μm to 30.0 μm. For example, the average particle size D50 of the micron-sized ceramic particles can be 5.0 μm, 6.0 μm, 7.0 μm, 8.0 μm, 9.0 μm, 10.0 μm, 11.0 μm, 12.0 μm, 13.0 μm, 14.0 μm, 15.0 μm, 16.0 μm, 17.0 μm, 18.0 μm, 19.0 μm, 20.0 μm, 21.0 μm, 22.0 μm, 23.0 μm, 24.0 μm, 25.0 μm, 26.0 μm, 27.0 μm, 28.0 μm, 29.0 μm, or 30.0 μm, or any value within the above range.

[0057] The second aspect of the present invention provides a method for preparing a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material. The key to this preparation method is to first embed nano-scale ceramic particles into the interior of the aluminum alloy matrix powder through a mechanical alloying method to achieve uniform distribution of nano-scale ceramic particles and improve the strength of the aluminum alloy matrix through intracrystalline and grain boundary strengthening; then, high-efficiency acoustic resonance mixing is used instead of traditional ball milling mixing. The mixing process does not rely on the mixing medium, which avoids the friction and collision of the mixing medium on the aluminum alloy powder and graphene, greatly shortens the mixing time, and at the same time reduces the oxidation of the aluminum alloy powder and the damage of the mixing medium to the structural integrity of the graphene, so that the graphene and micron-scale ceramic particles are evenly dispersed in the aluminum alloy matrix powder; mechanical alloying is combined with high-efficiency acoustic resonance mixing to achieve uniform dispersion distribution of nano-scale ceramic particles, graphene and micron-scale ceramic particles in the aluminum alloy matrix, giving full play to the strengthening effect of the three reinforcing phases.

[0058] In the embodiments of the present invention, see Figure 5 As shown, the preparation method of the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material is specifically carried out in the following steps.

[0059] Al-Cu-Mg-Si alloy vacuum melting

[0060] In an embodiment of the present invention, Al ingots, Cu ingots, Mg ingots, and Al-Si master alloy are vacuum melted to prepare Al-Cu-Mg-Si alloy billets.

[0061] In order to prevent excessive burning of Mg elements during vacuum melting, the vacuum melting temperature should not be too high. This is mainly based on the boiling point of Mg metal is 1090 ℃. When the heating temperature exceeds the boiling point of Mg element, the relevant elements turn into gas and burn seriously, resulting in inaccurate composition of Al-Cu-Mg-Si alloy. Therefore, vacuum melting needs to be carried out below the boiling point of Mg metal. In some embodiments of the present invention, the vacuum melting temperature of Al-Cu-Mg-Si alloy ingot is 700 ℃ ~ 900 ℃, and the vacuum degree is ≤10 -2 Pa.

[0062] Illustratively, the vacuum melting temperature of the Al-Cu-Mg-Si alloy ingot may be one of 700°C, 750°C, 800°C, 850°C, 900°C, or any value within the above range.

[0063] In some embodiments of the present invention, Al ingots, Cu ingots, Mg ingots, and Al-Si master alloy are configured according to alloy ratios and heated and smelted in a vacuum furnace to prepare Al-Cu-Mg-Si alloy ingots.

[0064] atomization powder making

[0065] In an embodiment of the present invention, an Al-Cu-Mg-Si alloy ingot is subjected to gas atomization pulverization to obtain Al-Cu-Mg-Si atomized powder.

[0066] In some embodiments of the present invention, during the gas atomization powder making process, the billet melting heating temperature is 700° C. to 900° C., the gas atomization pouring temperature is 700° C. to 900° C., and the holding time is 10 min to 30 min.

[0067] For example, the billet melting heating temperature can be one of 700°C, 750°C, 800°C, 850°C, 900°C, or any value within the aforementioned range. The gas atomization pouring temperature can be one of 700°C, 750°C, 800°C, 850°C, 900°C, or any value within the aforementioned range. The holding time can be one of 10 min, 15 min, 20 min, 25 min, 30 min, or any value within the aforementioned range.

[0068] In some embodiments of the present invention, during the gas atomization powder making process, the atomization protective atmosphere is any one of nitrogen, argon or helium, and the gas purity is ≥99.5%.

[0069] Mechanical alloying mixing

[0070] In an embodiment of the present invention, Al-Cu-Mg-Si atomized powder is mechanically alloyed with nano-scale ceramic particles, so that the nano-scale ceramic particles are embedded in the Al-Cu-Mg-Si atomized powder to obtain a mechanically alloyed powder.

[0071] Of course, it should be noted that due to the different addition contents of nano-ceramic particles, it is inevitable that a small amount of nano-ceramic particles will adhere to the surface of the Al-Cu-Mg-Si atomized powder during the mechanical alloying mixing process.

[0072] In some embodiments of the present invention, the nano-scale ceramic particles include one or a combination of Y2O3, MgO, TiB2, and B4C.

[0073] In some embodiments of the present invention, the purity of the nano-scale ceramic particles is ≥99.5%.

[0074] In some embodiments of the present invention, the average particle size D50 of the nano-scale ceramic particles is 30 nm to 100 nm. For example, the average particle size D50 of the nano-scale ceramic particles can be one of 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, and 100 nm, or any value within the above range.

[0075] In some embodiments of the present invention, during the mechanical alloying mixing process, the ball-to-material ratio of the total mass of the Al-Cu-Mg-Si atomized powder and the nano-scale ceramic particles to the grinding balls is 10:1 to 30:1, the ball milling speed is 200 r / min to 500 r / min, and the mixing time is 5 h to 30 h. For example, the ball-to-material ratio can be one of 10:1, 12:1, 15:1, 16:1, 18:1, 20:1, 22:1, 25:1, 26:1, 28:1, 30:1, or any value within the above range. The ball milling speed can be one of 200 r / min, 250 r / min, 300 r / min, 350 r / min, 400 r / min, 450 r / min, 500 r / min, or any value within the above range. The mixing time can be one of 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h, 29h, 30h or any value that meets the above range.

[0076] In some embodiments of the present invention, Al-Cu-Mg-Si atomized powder and nano-ceramic particles are loaded into a high-energy ball mill according to a ratio, and the nano-ceramic particles are embedded in the powder through mechanical alloying mixing to achieve uniform mixing of the two.

[0077] High-efficiency acoustic resonance mixing

[0078] The present invention adopts a high-efficiency acoustic resonance method to mix graphene, conducts energy through vibration, and the mixing process does not rely on a mixing medium. On the basis of not destroying the structure of the graphene itself, it solves the problem of uneven mixing caused by the large difference in specific gravity between the graphene and the aluminum alloy matrix powder. At the same time, micron-sized ceramic particles are introduced, and the graphene and micron-sized ceramic particles are evenly dispersed in the aluminum alloy matrix powder through the high-efficiency acoustic resonance method, thereby improving the comprehensive performance of the material.

[0079] In an embodiment of the present invention, mechanically alloyed powder is mixed with graphene and micron-sized ceramic particles using a high-efficiency acoustic resonance mixing method or a high-efficiency acoustic resonance mixing method to conduct energy through vibration, so that the graphene and micron-sized ceramic particles are uniformly dispersed in the Al-Cu-Mg-Si atomized powder to obtain a composite powder.

[0080] It is worth mentioning that due to the different addition levels of nano-ceramic particles, a small amount of nano-ceramic particles will inevitably adhere to the surface of the Al-Cu-Mg-Si atomized powder during the mechanical alloying mixing process, and even agglomerate. Although the volume percentage of nano-ceramic particles is only 0.5% to 6%, because they are nano-sized, they are numerous and fine particles at a given mass. During the mechanical alloying mixing process, mechanical collisions occur, and it is impossible to ensure that all nano-ceramic particles enter the interior of the Al-Cu-Mg-Si atomized powder. Therefore, a small amount of nano-ceramic particles will adhere to the surface of the Al-Cu-Mg-Si atomized powder or agglomerate. Subsequently, through the method of high-efficiency acoustic resonance, the nano-ceramic particles attached to the surface of the Al-Cu-Mg-Si atomized powder can be distributed more evenly, the agglomerations will be broken up, and the particles will be evenly distributed. Of course, in this process, a small amount of nano-ceramic particles will also be evenly distributed on the surface of the micron-sized ceramic particles.

[0081] Figure 3 The schematic diagram of the structure of the composite powder 5 obtained by mechanical alloying and efficient acoustic resonance mixing of Al-Cu-Mg-Si atomized powder, micron-sized ceramic particles, nano-sized ceramic particles and graphene is shown: the nano-sized ceramic particles 3 are embedded in the interior of the Al-Cu-Mg-Si atomized powder 1 by mechanical alloying, and a small amount of nano-sized ceramic particles 3 are attached to the surface of the Al-Cu-Mg-Si atomized powder 1. The mechanical alloying achieves uniform mixing of the two and further enhances the strength of the matrix powder. The graphene 4 and the micron-sized ceramic particles 2 are uniformly dispersed in the Al-Cu-Mg-Si atomized powder 1 by efficient acoustic resonance mixing without destroying the structure of the graphene 4 itself.

[0082] In some embodiments of the present invention, the micron-sized ceramic particles include one or a combination of SiC, B4C, and TiB2.

[0083] In some embodiments of the present invention, the average particle size D50 of the micron-sized ceramic particles is 5.0 μm to 30.0 μm. For example, the average particle size D50 of the micron-sized ceramic particles can be 5.0 μm, 6.0 μm, 7.0 μm, 8.0 μm, 9.0 μm, 10.0 μm, 11.0 μm, 12.0 μm, 13.0 μm, 14.0 μm, 15.0 μm, 16.0 μm, 17.0 μm, 18.0 μm, 19.0 μm, 20.0 μm, 21.0 μm, 22.0 μm, 23.0 μm, 24.0 μm, 25.0 μm, 26.0 μm, 27.0 μm, 28.0 μm, 29.0 μm, 30.0 μm, or any value within the above range.

[0084] In some embodiments of the present invention, the purity of the micron-sized ceramic particles is ≥99.5%.

[0085] In some embodiments of the present invention, a protective gas is introduced during the high-efficiency acoustic resonance mixing process, the vibration acceleration is 10g to 60g, and the mixing time is 30min to 90min. For example, the vibration acceleration can be one of 10g, 20g, 30g, 40g, 50g, 60g, or any value within the above range. The mixing time can be one of 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, 80min, 85min, 90min, or any value within the above range.

[0086] In some embodiments of the present invention, the protective gas includes one of nitrogen and argon. For example, during the high-efficiency acoustic resonance mixing process, one of nitrogen and argon is introduced into the tank to prevent further oxidation.

[0087] In some embodiments of the present invention, mechanical alloying powder, graphene, and micron-sized ceramic particles are loaded into a high-efficiency acoustic resonance device in proportion, and energy is conducted through vibration, so that the graphene and micron-sized ceramic particles are evenly dispersed in the Al-Cu-Mg-Si atomized powder.

[0088] Cold isostatic pressing

[0089] In an embodiment of the present invention, the composite powder after high-efficiency acoustic resonance mixing is subjected to cold isostatic pressing.

[0090] In some embodiments of the present invention, the pressure of cold isostatic pressing is 60 MPa to 100 MPa, and the holding time is 0.5 h to 3.0 h. For example, the pressure of cold isostatic pressing can be one of 60 MPa, 65 MPa, 70 MPa, 75 MPa, 80 MPa, 85 MPa, 90 MPa, 95 MPa, 100 MPa, or any value within the above range. The holding time can be one of 0.5 h, 0.6 h, 0.8 h, 1.0 h, 1.2 h, 1.5 h, 1.6 h, 1.8 h, 2.0 h, 2.2 h, 2.5 h, 2.6 h, 2.8 h, 3.0 h, or any value within the above range.

[0091] In some embodiments of the present invention, the composite powder is encapsulated in a rubber sheath and subjected to cold isostatic pressing. The maximum pressure of the cold isostatic pressing is 60 MPa to 100 MPa, and the holding time is 0.5 h to 3.0 h.

[0092] Vacuum degassing

[0093] In an embodiment of the present invention, the cold-pressed billet formed by cold isostatic pressing is placed in a metal cladding for high-temperature vacuum degassing.

[0094] In some embodiments of the present invention, the vacuum degassing temperature is 420°C to 550°C, and the sealing vacuum degree satisfies ≤10 -2 Pa. Exemplarily, the temperature of the vacuum degassing may be one of 420°C, 425°C, 430°C, 435°C, 440°C, 445°C, 450°C, 455°C, 460°C, 465°C, 470°C, 475°C, 480°C, 485°C, 490°C, 495°C, 500°C, 505°C, 510°C, 515°C, 520°C, 525°C, 530°C, 535°C, 540°C, 545°C, and 550°C, or any value satisfying the above range.

[0095] In some embodiments of the present invention, the metal sheath material used for vacuum degassing includes one of copper alloy and aluminum alloy, ensuring that the sheath can deform evenly and cooperatively with the aluminum alloy material inside the sheath during the hot isostatic pressing densification process of the ingot after vacuum degassing.

[0096] In some embodiments of the present invention, the thickness of the metal sheath used for vacuum degassing is 5 mm to 10 mm. For example, the thickness of the metal sheath can be one of 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, 10 mm, or any value within the above range.

[0097] In some embodiments of the present invention, the metal sheath used for vacuum degassing is made of copper alloy or aluminum alloy, the maximum temperature of vacuum degassing is 420℃~550℃, and the sealing vacuum degree meets ≤10 -2 Pa.

[0098] Hot isostatic pressing

[0099] In an embodiment of the present invention, the ingot after vacuum degassing is subjected to hot isostatic pressing sintering to obtain a sintered blank.

[0100] In some embodiments of the present invention, the pressure of hot isostatic pressing sintering is 80 MPa to 200 MPa, the temperature is 420° C. to 550° C., and the holding time is 1.0 h to 3.0 h.

[0101] Illustratively, the pressure of hot isostatic pressing sintering can be one of 80 MPa, 90 MPa, 100 MPa, 110 MPa, 120 MPa, 130 MPa, 140 MPa, 150 MPa, 160 MPa, 170 MPa, 180 MPa, 190 MPa, 200 MPa, or any value within the above range.

[0102] Illustratively, the temperature of hot isostatic pressing sintering can be one of 420°C, 430°C, 440°C, 450°C, 460°C, 470°C, 480°C, 490°C, 500°C, 510°C, 520°C, 530°C, 540°C, 550°C or any value that meets the above range.

[0103] For example, the holding time of hot isostatic pressing sintering can be one of 1.0 h, 1.5 h, 2.0 h, 2.5 h, 3.0 h, or any value within the above range.

[0104] In some embodiments of the present invention, the maximum pressure of hot isostatic pressing sintering is 80 MPa to 200 MPa, the maximum heating temperature is 420° C. to 550° C., and the holding time is 1.0 h to 3.0 h.

[0105] Extrusion

[0106] In an embodiment of the present invention, the metal sheath outside the ingot is removed after hot isostatic pressing and sintering, and the ingot material is extruded.

[0107] In some embodiments of the present invention, the heating temperature of the extruded billet is 420° C. to 550° C., the temperature of the extrusion die is 420° C. to 550° C., and the extrusion ratio is 10:1 to 30:1.

[0108] For example, the heating temperature of the extruded billet may be one of 420° C., 450° C., 480° C., 500° C., 520° C., 550° C., or any value within the above range.

[0109] For example, the extrusion die temperature for extrusion molding may be one of 420° C., 450° C., 480° C., 500° C., 520° C., 550° C., or any value within the above range.

[0110] Illustratively, the extrusion ratio of extrusion molding can be one of 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, 21:1, 22:1, 23:1, 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1 or any value that meets the above range.

[0111] Heat treatment

[0112] In an embodiment of the present invention, the heat treatment includes a solution aging treatment, and the extruded billet is subjected to a solution aging heat treatment to strengthen it, thereby obtaining a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material.

[0113] In some embodiments of the present invention, the solution temperature is 420°C to 550°C, the solution holding time is 1.0h to 3.0h, the quenching transfer time is less than 20s, and the water cooling temperature is 20°C to 30°C.

[0114] For example, the solution temperature can be 420°C, 450°C, 480°C, 500°C, 520°C, 550°C, or any value within the aforementioned range. The solution holding time can be 1.0 h, 1.5 h, 1.8 h, 2.0 h, 2.5 h, 2.8 h, 3.0 h, or any value within the aforementioned range. The water cooling temperature can be 20°C, 25°C, 30°C, or any value within the aforementioned range.

[0115] In some embodiments of the present invention, the aging temperature is 150° C. to 200° C., and the aging holding time is 5 h to 15 h.

[0116] For example, the aging temperature may be one of 150° C., 180° C., 200° C., or any value within the aforementioned range. The aging holding time may be one of 5 h, 6 h, 7 h, 8 h, 9 h, 10 h, 11 h, 12 h, 13 h, 14 h, 15 h, or any value within the aforementioned range.

[0117] In some embodiments of the present invention, the preparation method of micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite materials includes: vacuum melting of Al-Cu-Mg-Si alloy → gas atomization powder making → mechanical alloying mixing of Al-Cu-Mg-Si atomized powder and nano-scale ceramic particles → adding graphene and micron-scale ceramic particles to the mechanically alloyed powder for high-efficiency acoustic resonance mixing → cold isostatic pressing → vacuum degassing → hot isostatic pressing sintering → extrusion molding → heat treatment to obtain high-performance, lightweight micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite materials.

[0118] Unless otherwise defined, the technical terms used in the following examples have the same meanings as those generally understood by those skilled in the art to which the present invention belongs. The experimental reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the raw materials, instruments and equipment used in the following examples, etc., can all be purchased on the market or can be obtained by existing methods; the amounts of the experimental reagents used, unless otherwise specified, are the amounts of reagents used in conventional experimental operations; the experimental methods, unless otherwise specified, are all conventional methods. It should be further noted that the following description is merely exemplary and does not specifically limit the present invention.

[0119] Example 1

[0120] Provided is a micro-nano hybrid ceramic particle and graphene reinforced aluminum-based composite material (3.0% nano-scale TiB2+0.5% graphene+13% micron-scale SiC / Al-0.9Cu-1.0Mg-0.6Si). The reinforced aluminum-based composite material consists of an aluminum alloy matrix and a reinforcing phase uniformly dispersed in the aluminum alloy matrix, wherein the reinforcing phase includes three types, specifically nano-scale ceramic particles TiB2, with a volume percentage of 3.0%; graphene, with a volume percentage of 0.5%; and micron-scale ceramic particles SiC, with a volume percentage of 13.0%; and the aluminum alloy matrix is ​​Al-0.9Cu-1.0Mg-0.6Si, wherein 0.9, 1.0, and 0.6 represent that the mass percentages of Cu, Mg, and Si are 0.9%, 1.0%, and 0.6%, respectively.

[0121] See also Figure 5 As shown in FIG, the preparation of the aluminum matrix composite material reinforced with micro-nano hybrid ceramic particles and graphene includes: first, Al ingot (purity>99.9%), Cu ingot (purity>99.9%), Mg ingot (purity>99.9%), and Al-Si master alloy (impurity<0.5%) are prepared according to the alloy ratio, and are added into a vacuum furnace for smelting to prepare Al-Cu-Mg-Si alloy billet, with the melting temperature of 800°C and the vacuum degree of <10 -2 Pa; The smelted Al-Cu-Mg-Si ingot was subjected to gas atomization powder making, the ingot melting temperature was 820°C, the gas atomization pouring temperature was 820°C, the atomizing medium was nitrogen (purity>99.5%), and Al-0.9Cu-1.0Mg-0.6Si atomized powder was obtained.

[0122] Then, the Al-0.9Cu-1.0Mg-0.6Si atomized powder and 3.0 vol.% nano-scale TiB2 particles (average particle size D50 is 50 nm) are placed in a high-energy ball mill for mechanical alloying mixing. The ball-to-material mass ratio of the mixed powder is 10:1, and the ball milling is carried out at a speed of 400 r / min for 8 hours. After mechanical alloying mixing, the nano-scale TiB2 particles are embedded in the Al-0.9Cu-1.0Mg-0.6Si atomized powder. Of course, there is still a small amount of nano-scale ceramic particles TiB2 attached to the surface of the atomized powder; embedding nano-scale ceramic particles TiB2 in the aluminum alloy powder can not only achieve uniform dispersion of nano-scale ceramic particles, but also improve the strength of the aluminum alloy matrix itself through intracrystalline and grain boundary strengthening, thereby avoiding the degradation of material properties caused by agglomeration of nano-scale ceramic particles.

[0123] Next, the mechanical alloying powder obtained after mechanical alloying mixing is placed together with 0.5 vol.% graphene and 13 vol.% micron-sized SiC particles (average particle size D50 is 12 μm) in a resonant mixing container for high-efficiency acoustic resonance mixing. Figure 4As shown, argon gas is introduced into the high-efficiency acoustic resonance mixing container 6, and the vibration energy transmitted by the mixed powder through the vibration platform 8 forms a material mixed flow 7. The mixing is performed for 10 minutes at a resonance acceleration of 10g, 10 minutes at a resonance acceleration of 20g, 15 minutes at a resonance acceleration of 40g, and 20 minutes at a resonance acceleration of 60g. The graphene and micron-sized SiC particles are evenly distributed in the Al-0.9Cu-1.0Mg-0.6Si alloy powder through high-efficiency acoustic resonance mixing. The high-efficiency acoustic resonance process transmits energy through vibration, does not rely on the mixing medium, avoids the friction and collision of the mixing medium on the aluminum alloy powder and graphene, and achieves its uniform distribution on the basis of retaining the graphene's own structure. Figure 1 、 Figure 2 The SEM images of the composite powder 5 obtained after high-efficiency acoustic resonance mixing are shown in FIG. Figure 1 It can be seen that the spherical Al-Cu-Mg-Si atomized powder undergoes certain deformation during the mechanical alloying process, and the surface morphology becomes irregular; at the same time, a small portion of nano-ceramic particles that have not entered the Al-Cu-Mg-Si atomized powder are distributed on the surface of the mechanical alloying powder and micron-sized SiC particles. Figure 2 The presence of layered graphene was observed in the .

[0124] Next, the composite powder obtained by high-efficiency acoustic resonance mixing was placed in a rubber sleeve for cold isostatic pressing. The pressure of the cold isostatic pressing was 70 MPa and the holding time was 20 min. The relative density of the powder ingot obtained after cold isostatic pressing was 75%. The powder ingot was placed in a 6061 aluminum alloy sleeve and welded. The sleeve was then placed in a pit-type resistance furnace for vacuum degassing. The maximum temperature of the vacuum degassing process was 500 ° C, and the temperature was kept at 500 ° C for 2 h. When the sleeve was finally sealed, the vacuum degree inside the sleeve was less than 1×10 -2 Pa; then the powder billet with the jacket after vacuum degassing is hot isostatic pressing sintering, the maximum heating temperature of the hot isostatic pressing sintering process is 500℃, the maximum pressure is 90MPa, and the holding time at the maximum pressure is 2.5h; after the metal jacket is removed from the billet after hot isostatic pressing sintering, the billet is kept at 500℃ for 3h, the extrusion die is heated to 500℃ and kept warm for 3h, and a round rod die with an extrusion ratio of 10:1 is selected for material extrusion; the extruded material is heat treated, kept warm at a solution temperature of 530℃ for 1.5h, and the aging temperature is 170℃ for 10h.

[0125] The density of the 3.0% nano-TiB2+0.5% graphene+13% micro-SiC / Al-0.9Cu-1.0Mg-0.6Si composite material prepared in Example 1 is 2.80 g / cm 3, density is 100%, elastic modulus is 103GPa, room temperature tensile strength is 622MPa, yield strength is 558MPa, and elongation is 6.0%.

[0126] Example 2

[0127] The specific operation is the same as that of Example 1. The only difference between Example 2 and Example 1 is that:

[0128] In Example 2, the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material (5% nano-scale Y2O3 + 1.0% graphene + 19% micron-scale SiC / Al-0.4Cu-0.9Mg-0.5Si) is prepared, wherein the nano-scale ceramic particles are Y2O3 (average particle size D50 is 30nm), and the volume percentage is 5.0%; the volume percentage of graphene is 1.0%; the micron-scale ceramic particles are SiC (average particle size D50 is 12μm), and the volume percentage is 19.0%; the aluminum alloy matrix is ​​Al-0.4Cu-0.9Mg-0.5Si, wherein 0.4, 0.9, and 0.5 represent that the mass percentages of Cu, Mg, and Si are 0.4%, 0.9%, and 0.5%, respectively.

[0129] In the preparation of micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composites: the ball-to-material mass ratio of the mixed powder in the mechanical alloying mixing process is 15:1, and the ball milling is carried out at a speed of 400r / min for 10 hours. After mechanical alloying mixing, nano-scale Y2O3 is embedded in the interior and surface of the Al-0.4Cu-0.9Mg-0.5Si atomized powder.

[0130] The mechanically alloyed powder obtained after mechanical alloying mixing was placed together with 1.0 vol.% graphene and 19 vol.% micron-sized SiC particles in a resonance mixing tank for efficient acoustic resonance mixing. The mixing was carried out at a resonance acceleration of 10 g for 15 minutes, a resonance acceleration of 20 g for 15 minutes, a resonance acceleration of 40 g for 20 minutes, and a resonance acceleration of 60 g for 20 minutes. Through efficient acoustic resonance mixing, the graphene and micron-sized SiC particles were evenly distributed in the Al-0.4Cu-0.9Mg-0.5Si alloy powder.

[0131] The density of the 5% nano-sized Y2O3+1.0% graphene+19% micro-sized SiC / Al-0.4Cu-0.9Mg-0.5Si composite material prepared in Example 2 is 2.83 g / cm 3 , density is 100%, elastic modulus is 124GPa, room temperature tensile strength is 698MPa, yield strength is 625MPa, and elongation is 4.5%.

[0132] Comparative Example 1

[0133] The specific operation is the same as that of Example 1. The difference between Comparative Example 1 and Example 1 is only that:

[0134] Comparative Example 1 does not employ mechanical alloying and high-efficiency acoustic resonance mixing. Instead, 3.0% by volume of nano-ceramic TiB2 particles, 0.5% by volume of graphene, 13.0% by volume of micron-sized ceramic SiC particles, and an aluminum alloy powder having a composition of Al-0.9Cu-1.0Mg-0.6Si are mixed using conventional ball milling. The mass ratio of the mixed powders is 2:1, and the milling time is 24 hours. The average particle size of each raw material powder used in Comparative Example 1 is the same as that of Example 1. Conventional ball milling is not only time-consuming, but also results in a significant agglomeration of the nano-ceramic particles and graphene after mixing. This agglomeration defect in the reinforcement leads to a significant decrease in the material strength and elongation.

[0135] Comparative Example 2

[0136] The specific operation is the same as that of Example 1. The difference between Comparative Example 2 and Example 1 is only that:

[0137] Comparative Example 2 did not employ mechanical alloying. Instead, 3.0% by volume of nano-ceramic TiB2 particles, 0.5% by volume of graphene, and 13.0% by volume of micro-ceramic SiC particles were directly mixed with an aluminum alloy powder having a composition of Al-0.9Cu-1.0Mg-0.6Si. The mixing was performed under a resonant acceleration of 10g for 15 minutes, a resonant acceleration of 20g for 15 minutes, a resonant acceleration of 40g for 20 minutes, and a resonant acceleration of 60g for 25 minutes. The average particle size of each raw material powder used in Comparative Example 2 was the same as that of Example 1. After the high-efficiency acoustic resonance mixing, most of the nano-ceramic particles adhered to the surface of the aluminum alloy powder, which was not conducive to interfacial bonding during the subsequent powder sintering process. At the same time, excessive nano-ceramic particles adhering to the surface easily formed brittle grain boundaries, which reduced the material properties.

[0138] Comparative Example 3

[0139] The specific operation is the same as that of Example 1. The difference between Comparative Example 3 and Example 1 is only that:

[0140] Comparative Example 3 did not utilize high-efficiency acoustic resonance mixing. Instead, mechanical alloying was performed directly on 3.0% by volume of nano-ceramic TiB2 particles, 0.5% by volume of graphene, and 13.0% by volume of micro-ceramic SiC particles with an aluminum alloy powder composition of Al-0.9Cu-1.0Mg-0.6Si. The mixed powder had a ball-to-material mass ratio of 20:1 and was subjected to high-energy ball milling at 400 r / min for 15 hours. The average particle size of each raw material powder used in Comparative Example 3 was the same as that in Example 1. After mechanical alloying, most of the nano-ceramic TiB2 particles were embedded within the Al-0.9Cu-1.0Mg-0.6Si alloy powder, but the structural integrity of the graphene itself was destroyed. Simultaneously, the aluminum alloy powder was severely deformed during the mechanical alloying process, resulting in a significant decrease in the material elongation.

[0141] Performance Testing

[0142] The powder mixing methods and powder uniformity results in Examples 1 to 2 and Comparative Examples 1 to 3 are summarized as shown in Table 1.

[0143] Table 1 Summary of powder mixing methods and powder uniformity results in Examples and Comparative Examples

[0144]

[0145] At the same time, the tensile properties refer to GB / T 228.1 2021, and the elastic modulus refers to GB / T 22315-2008. The tensile strength, yield strength and elongation of the aluminum-based composite materials prepared in Examples 1 to 2 and Comparative Examples 1 to 3 are tested. The test results are shown in Table 2.

[0146] Table 2 Summary of properties of the aluminum-based composite materials obtained in the examples and comparative examples

[0147] Group Elastic modulus / GPa Tensile strength / Mpa Yield strength / MPa Elongation / % Example 1 103 622 558 6.0 Example 2 124 698 625 4.5 Comparative Example 1 101 443 386 4.0 Comparative Example 2 101 505 439 6.5 Comparative Example 3 101 537 485 3.0

[0148] It can be seen from the data in Table 1 and Table 2 that the preparation method provided by the present invention can optimize the agglomeration phenomenon that occurs after adding reinforcing phases such as nano-scale ceramic particles and graphene in the mixing of aluminum-based composite material powders. On the one hand, the mechanical alloying mixing method can overcome the problem that the nano-scale ceramic particles are too small and prone to agglomeration, and the nano-scale ceramic particles are embedded in the interior of the aluminum alloy matrix powder, which plays a good role in intragranular and grain boundary strengthening; on the other hand, the graphene is mixed by a high-efficiency acoustic resonance method, which conducts energy through vibration and does not rely on the mixing medium. On the basis of not destroying the structure of the graphene itself, the problem of uneven mixing caused by the large difference in specific gravity between the graphene and the aluminum alloy matrix powder is solved; at the same time, micron-sized ceramic particles are added, and the graphene and micron-sized ceramic particles are evenly dispersed in the aluminum alloy matrix powder by the high-efficiency acoustic resonance method. Finally, the graphene is oriented by extrusion deformation, further improving the dispersion uniformity of graphene in the aluminum-based composite material, solving the problem of poor compatibility, and improving the comprehensive performance of the material.

[0149] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A micro-nano hybrid ceramic particle and graphene reinforced aluminum matrix composite material, characterized in that: The invention comprises an aluminum alloy matrix and a reinforcement phase uniformly dispersed in the aluminum alloy matrix, wherein the aluminum alloy matrix is ​​an Al-Cu-Mg-Si alloy, and the reinforcement phase comprises micron-sized ceramic particles, nano-sized ceramic particles and graphene; The volume percentage of the aluminum alloy matrix is ​​70% to 89%, the volume percentage of the micron-sized ceramic particles is 10% to 20%, the volume percentage of the nano-sized ceramic particles is 0.5% to 6%, and the volume percentage of the graphene is 0.5% to 4%.

2. The micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material according to claim 1, characterized in that: The Al-Cu-Mg-Si alloy includes the following components in weight percentage: Cu 0.15%~1.0%, Mg 0.8%~1.5%, Si 0.4%~1.2%, and the balance is Al.

3. The micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material according to claim 1, characterized in that: The nano-scale ceramic particles include at least one of Y2O3, MgO, TiB2, and B4C; and / or, The average particle size D50 of the nano-scale ceramic particles is 30nm to 100nm.

4. The micro-nano hybrid ceramic particles and graphene reinforced aluminum matrix composite material according to claim 1, characterized in that: The micron-sized ceramic particles include at least one of SiC, B4C, and TiB2; and / or, The average particle size D50 of the micron-sized ceramic particles is 5.0 μm to 30.0 μm.

5. A method for preparing the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material according to any one of claims 1 to 4, characterized in that: The following steps are involved: Mechanically alloying the Al-Cu-Mg-Si atomized powder and nano-scale ceramic particles to embed the nano-scale ceramic particles into the Al-Cu-Mg-Si atomized powder to obtain a mechanically alloyed powder; The mechanically alloyed powder is mixed with graphene and micron-sized ceramic particles by a high-efficiency acoustic resonance method to conduct energy through vibration, so that the graphene and micron-sized ceramic particles are uniformly dispersed in the Al-Cu-Mg-Si atomized powder to obtain a composite powder; The composite powder is subjected to cold isostatic pressing, vacuum degassing, and hot isostatic sintering to obtain a sintered blank; The sintered blank is subjected to extrusion molding and heat treatment to obtain the micro-nano hybrid ceramic particles and graphene reinforced aluminum-based composite material.

6. The preparation method according to claim 5, wherein During the mechanical alloying mixing process, the total mass of the Al-Cu-Mg-Si atomized powder and the nano-ceramic particles to the grinding balls is 10:1 to 30:1, the ball milling speed is 200 r / min to 500 r / min, and the mixing time is 5 h to 30 h.

7. The preparation method according to claim 5, wherein During the high-efficiency acoustic resonance mixing process, protective gas is introduced, the vibration acceleration is 10g to 60g, and the mixing time is 30min to 90min; Preferably, the protective gas includes one of nitrogen and argon.

8. The preparation method according to claim 5, wherein The cold isostatic pressing pressure is 60 MPa to 100 MPa, and the holding time is 0.5 h to 3.0 h; Preferably, the vacuum degassing temperature is 420℃~550℃, and the sealing vacuum degree meets ≤10 -2 Pa; the metal sheath material used in the vacuum degassing includes one of copper alloy and aluminum alloy; Preferably, the hot isostatic pressing sintering is performed at a pressure of 80 MPa to 200 MPa, a temperature of 420° C. to 550° C., and a holding time of 1.0 h to 3.0 h.

9. The preparation method according to claim 5, wherein The heating temperature of the billet for extrusion molding is 420°C to 550°C, the temperature of the extrusion die is 420°C to 550°C, and the extrusion ratio is 10:1 to 30:1; Preferably, the heat treatment includes solution aging treatment, wherein the solution temperature is 420°C to 550°C, the solution holding time is 1.0h to 3.0h, the quenching transfer time is less than 20s, the water cooling temperature is 20°C to 30°C; the aging temperature is 150°C to 200°C, and the aging holding time is 5h to 15h.

10. The preparation method according to claim 5, characterized in that The preparation of the Al-Cu-Mg-Si atomized powder comprises: Vacuum melting Al ingots, Cu ingots, Mg ingots, and Al-Si master alloy to prepare Al-Cu-Mg-Si alloy billets; Gas atomizing the Al-Cu-Mg-Si alloy ingot to obtain the Al-Cu-Mg-Si atomized powder; Preferably, the vacuum melting temperature of the Al-Cu-Mg-Si alloy ingot is 700°C to 900°C, and the vacuum degree is ≤10 -2 Pa; Preferably, in the gas atomization powder making process, the billet melting heating temperature is 700° C. to 900° C., the gas atomization pouring temperature is 700° C. to 900° C., and the holding time is 10 min to 30 min.

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