Preparation method of micron / nano mixed-scale ZrB2 particle reinforced high-strength and high-toughness Al-Cu-based composite material
By adopting the semi-solid stir-casting method in aluminum alloy, the mixing of micron and nanoscale ZrB2 particles is solved, and the problem of difficulty in uniform dispersing of ZrB2 particles in aluminum alloy is achieved, while high strength and high plasticity of the material are achieved, while reducing production costs.
Patent Information
- Application Number
- CN202510338344.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-21
- Publication Date
- 2025-06-27
AI Technical Summary
In the prior art, ZrB2 particles are difficult to disperse uniformly in aluminum alloys, resulting in poor mechanical properties and complex preparation processes, which increases production costs.
By using the semi-solid stir-casting method, by mixing micron and nanoscale ZrB2 particles, the micron-scale particles are used to drive the dispersion of nano-scale particles in the aluminum melt, reducing the agglomeration of nano-scale particles and improving their dispersion uniformity.
The uniform dispersion of ZrB2 particles in the aluminum alloy is achieved, which significantly improves the tensile strength and elongation of the material, reduces production costs, and simplifies the process flow.
Smart Images
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of alloy property improvement, and particularly relates to a semi-solid stirring casting preparation method for a micro / nano ZrB2 particle-reinforced high-strength and high-toughness Al-Cu-based composite material. Background Art
[0002] Al-Cu alloys have advantages such as high strength, low density, and high specific modulus, and are widely used in fields such as aviation, national defense, and civilian industries. However, with the leapfrog development of cutting-edge fields such as weaponry and new energy, the requirements for the comprehensive performance of materials are getting higher and higher. Since the as-cast structure of aluminum alloys has coarse grains, it will face problems that affect its subsequent processing process and forming performance. Therefore, by controlling the morphology of the as-cast structure is an effective means to improve its service performance and subsequent processing performance. Often, the as-cast structure faces problems such as coarse grains and severe segregation, which will lead to the deformation ability and strength of the as-cast alloy not meeting the production requirements of subsequent processing. Currently, in industrial production, the means to improve the as-cast structure of aluminum alloys is usually to perform large plastic deformation in advance, and then through subsequent annealing processes to achieve the purpose of recovery and recrystallization, thereby obtaining a structure with smaller grain size. This process of refining the as-cast structure effectively improves the deformation ability and strength of aluminum alloys, thus meeting the production requirements. However, due to large plastic deformation often leading to the cracking and failure of materials, the production efficiency is reduced, making subsequent secondary processing difficult. Therefore, particle-reinforced aluminum matrix composites have gradually attracted extensive attention from many researchers due to their more excellent mechanical properties, high-temperature properties, etc., and the research on their preparation processes and application technologies has become increasingly perfect.
[0003] Among numerous reinforcements, compared with common aluminum matrix composite reinforcements such as TiC, SiC, and Al2O3, ZrB2 has the advantages of high melting point, high hardness, high modulus, corrosion resistance, and wear resistance, which makes ZrB2 particle-reinforced aluminum matrix composites receive extensive attention. Among them, in-situ ZrB2 particle-reinforced aluminum matrix composites have become a research hotspot in this field due to the good interfacial bonding and high-temperature stability between the reinforcement and the matrix. For example, the invention patent with the application number 20201009831.6 reported that by electromagnetic stirring, K2ZrF6 and KBF4 were added to 6111Al aluminum alloy, and ZrB2 particles were in-situ generated through an endo-reaction to achieve the purpose of refining grains and improving strength. However, this preparation method still has the following disadvantages: 1. The size of the ZrB2 generated by the reaction is mostly nanoscale, and it is easy to form agglomerates in the aluminum melt. Therefore, rare earth elements were pre-introduced in this patent to promote the dispersion of ZrB2 particles in the melt; 2. The ZrB2 particles formed in-situ are mostly nanoscale and are not easy to diffuse in the aluminum melt. Mechanical stirring, electromagnetic stirring, etc. are needed to assist the diffusion of the particles in the melt, which increases its application cost in practical applications; 3. Both K2ZrF6 and KBF4 are fluorides, causing serious environmental pollution and great harm to the human body. Moreover, the decomposition temperature of KBF4 is low and it is easy to react to generate KF + BF3 (gas), resulting in a low recovery rate of B element (in practice, KBF4 generally needs to be in excess of 20wt.%). Summary of the Invention
[0004] In view of the problems existing in the prior art, the present invention provides a preparation method with controllable ceramic particle size and semi-solid stirring addition. Utilizing the characteristic that micron-sized particles are easy to disperse in the aluminum melt, micron-sized and nano-sized ZrB2 particles are mixed and added. The micron-sized particles drive the dispersion of the nano-sized particles in the aluminum melt, reducing the degree of agglomeration of the nano-sized particles.
[0005] To achieve the above object, the present invention provides the following technical solutions:
[0006] The preparation method of the above ZrB2 particle-reinforced high-strength and high-toughness Al-Cu matrix composite material is characterized by including the following steps:
[0007] (1) Prepare a micro / nano ZrB2 particle-Al powder composite powder
[0008] After mixing micron ZrB2 powder and nano ZrB2 powder, ball-mill and mix them with Al powder, and then dry the mixed powder to obtain a micro / nano ZrB2 particle-Al powder composite powder;
[0009] (2) Prepare a micro / nano ZrB2 particle-reinforced high-strength and high-toughness Al-Cu matrix composite material
[0010] A. Crude Al-Cu alloy billet: Aluminum ingots are placed in a melting furnace and heated to 760 - 780 °C while keeping the temperature constant. After the aluminum ingots are completely melted, under stirring conditions, aluminum-copper master alloy is added to the molten liquid until the weight of copper accounts for 4% - 4.8% of the total weight of the target alloy, and then it is allowed to stand for 10 - 15 minutes; under stirring conditions, zinc ingots are added to the molten liquid until the weight of zinc accounts for 0.12% - 0.18% of the total weight of the target alloy, and then it is allowed to stand for 10 - 15 minutes; it is heated to 800 - 820 °C and the temperature is kept constant. Under stirring conditions, magnesium ingots, aluminum-manganese master alloy, silicon ingots, pure iron blocks, and aluminum-titanium master alloy are successively added to the molten liquid until the weights of magnesium, manganese, silicon, iron, and titanium respectively account for 0.6% - 0.8%, 0.8% - 1%, 0.4 - 0.5%, 0% - 0.01%, and 0% - 0.02% of the total weight of the target alloy. After the above materials are completely melted, the furnace temperature is lowered to 740 °C - 760 °C and the temperature is kept constant; under stirring conditions, a drossing and degassing agent is added to the molten liquid for drossing and degassing treatment. After the drossing and degassing are completed, the molten liquid is allowed to stand for 5 - 10 minutes, and then poured into a crucible and cooled to room temperature to obtain an Al-Cu aluminum alloy billet;
[0011] B. Refined billet of micro / nano ZrB2 particle-reinforced high-strength and high-toughness Al-Cu matrix composite: The crude Al-Cu alloy billet is put into a resistance furnace and heated to 740 °C - 780 °C for melting. A drossing and degassing agent is added to the molten liquid for drossing and degassing treatment. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. At the same time, the ZrB2 particle-Al powder composite powder wrapped with two layers of aluminum foil is placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid surface of the Al-Cu alloy melt, and mechanically stirred for 10 min using a mechanical stirring device, heated to 730 °C - 740 °C, and then poured into a mold preheated to 250 °C to obtain a ZrB2 particle-reinforced Al-Cu aluminum matrix composite casting blank.
[0012] C. Hot deformation: The casting blank is placed in a box furnace for homogenization treatment and then hot-rolled.
[0013] D. Heat treatment: Solution aging treatment is carried out after hot rolling.
[0014] Further, in step (1), the component ratio of the micro / nano ZrB2 particle-Al powder composite powder is as follows: the mass percentage of Al powder is 65 - 75%, and the mass percentage of ZrB2 powder is 25 - 35%. The size of the micron ZrB2 powder is 3 - 5 μm or / and 8 - 10 μm, and the size of the nano ZrB2 powder is 50 - 100 nm; the mixing mass ratio of the micron ZrB2 powder and the nano ZrB2 powder is 1:1 - 1:5.
[0015] Further, in step (1), the ball milling process parameters are as follows: the ball-to-material ratio is 5:1 to 10:1, the rotation speed is 150 to 250 rpm / min, and the ball milling time is 18 to 24 h.
[0016] Further, by mass percentage, the measured composition of the Al-Cu aluminum alloy billet is as follows: copper 4.173%, magnesium 0.640%, manganese 0.941%, silicon 0.489%, iron 0.015%, titanium 0.013%, and the balance is aluminum.
[0017] In a preferred embodiment, the mass content of ZrB2 particles contained in the above ZrB2 particle-reinforced high-strength and high-toughness Al-Cu matrix composite is 0.1% to 1%, and preferably the ZrB2 particle content is 0.1% of 10um + 0.5% of 50nm.
[0018] Further, in step B of step (2), the preheating temperature of the metal mold is 240 to 260 °C.
[0019] Further, in C of step (2), the heating temperature for homogenization treatment is 470 °C to 490 °C, and the holding time is 11 h to 13 h. The hot rolling deformation temperature is 430 °C, the total deformation amount is 79% to 81%, and the reduction per pass accounts for about 9.8% to 10.2% of the total deformation amount.
[0020] Further, in step D of step (2), the solution aging treatment is as follows: the solution temperature is 490 °C to 510 °C, and the holding time is 2 h to 2.5 h; the aging temperature is 150 °C to 170 °C, and the holding time is 11 h to 13 h.
[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0022] The present invention preferably modifies the Al-Cu alloy with ZrB2 particles of different sizes and contents. The addition of ZrB2 particles improves the mechanical properties of the Al-Cu alloy. Moreover, the preparation process of the present invention is simple and easy to operate, the raw material cost is low, and it does not consume a large amount of aluminum elements and generate a large amount of corrosive reactants. It can be widely used in large-scale production. The grain distribution of the strengthening phase in the composite material prepared by the method and process of the present invention is uniform. Compared with the Al-Cu alloy matrix alloy, the tensile strength and elongation are significantly improved. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the following drawings are only some embodiments of the present invention. Among them:
[0024] Figure 1 is the as-cast metallographic structure diagram of the Al-Cu alloy;
[0025] Figure 2 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.1% and a particle size of 50 nm.
[0026] Figure 3 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.5% and a particle size of 50 nm.
[0027] Figure 4 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 1% and a particle size of 50 nm.
[0028] Figure 5 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.1% and a particle size of 5 μm.
[0029] Figure 6 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.5% and a particle size of 5 μm.
[0030] Figure 7 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.1% and a particle size of 10 μm.
[0031] Figure 8 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.5% and a particle size of 10 μm.
[0032] Figure 9 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 1% and a particle size of 10 μm.
[0033] Figure 10 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.1% (10 μm) + 0.1% (50 nm).
[0034] Figure 11 It is the as-cast metallographic structure diagram of the alloy with a ZrB2 particle content of 0.1% (10 μm) + 0.5% (50 nm).
[0035] Figure 12 It is the SEM image of the micro-nano hybrid scale ZrB2 reinforced Al-Cu matrix composite material. Detailed implementation manners
[0036] To make the above objects, features, and advantages of the present invention more obvious and understandable, the following detailed description of the specific implementation manners of the present invention will be given in combination with the embodiments of the specification.
[0037] The measured composition of the Al-Cu alloy is: copper 4.173%, magnesium 0.640%, manganese 0.941%, silicon 0.489%, iron 0.015%, titanium 0.013%, and the balance is aluminum.
[0038] Comparative Example 1: Preparation of Al-Cu alloy without adding ZrB2 particles.
[0039] Place the Al-Cu alloy rough-cast in a resistance furnace and melt it at 760 °C - 780 °C to obtain an Al-Cu alloy melt. Add a dried impurity remover to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, let it stand, and then pour it into a casting mold (preheated to 250 °C) to form a casting blank. Homogenize the casting blank, and the homogenization process is 490 °C × 12 h; perform hot rolling deformation on the homogenized material, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, perform solution aging treatment on the material, the solution temperature is 505 °C, the holding time is 2 h, and water quench at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0040] Use the above method to prepare a tensile sample with a thickness of 2 mm, and measure the mechanical properties at room temperature. The results are as follows: the tensile strength is 409 MPa, and the elongation is 5.82%.
[0041] Comparative Example 2: Preparation of Al-Cu matrix composite material with 50 nm 0.1% ZrB2 particle content.
[0042] Ball mill and mix 50 nm ZrB2 powder and Al powder according to a mass ratio of 3:7. The ball milling process parameters are: the ball-to-material ratio is 10:1, the rotation speed is 200 rpm / min, and the ball milling time is 24 h. Subsequently, dry the mixed powder to obtain a 50 nm ZrB2 particle - Al powder composite powder.
[0043] Place the Al-Cu alloy rough-cast in a resistance furnace and melt it at 760 °C - 780 °C to obtain an Al-Cu alloy melt. Add a dried impurity remover to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, let it stand. Subsequently, cool the aluminum melt to 610 °C - 630 °C, weigh an appropriate amount of 50 nm ZrB2 particle - Al powder composite powder to make the ZrB2 particles account for 0.1% of the mass of the Al-Cu alloy. At the same time, wrap the 50 nm ZrB2 particle - Al powder composite powder with two layers of aluminum foil and place it in a resistance furnace, heat it to 500 °C and hold for two hours, then take it out and quickly press it under the liquid surface of the Al-Cu alloy melt, and use a mechanical stirring device to stir mechanically for 10 min, heat up to 730 °C, and then pour it into a casting mold (preheated to 250 °C) to form a casting blank. Homogenize the casting blank, and the homogenization process is 490 °C × 12 h; perform hot rolling deformation on the homogenized material, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, perform solution aging treatment on the material, the solution temperature is 505 °C, the holding time is 2 h, and water quench at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0044] Using the above method to prepare a tensile sample with a thickness of 2 mm, the mechanical properties were measured at room temperature, and the results are as follows: the tensile strength is 448 MPa, and the elongation is 5.59%.
[0045] Comparative Example 3: Preparation of an Al-Cu based composite material with a 50 nm 0.5% ZrB2 particle content.
[0046] 50 nm ZrB2 particle - Al powder composite powder: the same as Comparative Example 2;
[0047] Place the Al-Cu alloy rough-cast billet in an electric resistance furnace and melt it at 760 °C - 780 °C to obtain an Al-Cu alloy melt. Add a dried impurity remover to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, let it stand. Then cool the aluminum melt to 610 °C - 630 °C. Weigh an appropriate amount of 50 nm ZrB2 particle - Al powder composite powder so that the ZrB2 particles account for 0.5% of the mass of the Al-Cu alloy. At the same time, wrap the 50 nm ZrB2 particle - Al powder composite powder with two layers of aluminum foil and place it in an electric resistance furnace, heat it to 500 °C and hold for two hours, then take it out and quickly press it under the liquid surface of the Al-Cu alloy melt. Use a mechanical stirring device to stir mechanically for 10 min, heat up to 730 °C, and then pour it into a casting mold (preheated to 250 °C) to form a casting billet. Subject the casting billet to homogenization treatment, and the homogenization process is 490 °C × 12 h; perform hot rolling deformation on the homogenized material, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, perform solution aging treatment on the material, the solution temperature is 505 °C, the holding time is 2 h, and water quench at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0048] Using the above method to prepare a tensile sample with a thickness of 2 mm, the mechanical properties were measured at room temperature, and the results are as follows: the tensile strength is 441 MPa, and the elongation is 9.5%.
[0049] Comparative Example 4: Preparation of an Al-Cu based composite material with a 1% 50 nm ZrB2 particle content.
[0050] 50 nm ZrB2 particle - Al powder composite powder: the same as Comparative Example 2;
[0051] The Al-Cu alloy rough smelting billet is placed in a resistance furnace and melted at 760 °C - 780 °C to obtain an Al-Cu alloy melt. A dried impurity remover is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is left to stand. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. An appropriate amount of 50 nm ZrB2 particle-Al powder composite powder is weighed, such that the ZrB2 particles account for 1% of the mass of the Al-Cu alloy. At the same time, the 50 nm ZrB2 particle-Al powder composite powder is wrapped with two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid level of the Al-Cu alloy melt, where a mechanical stirring device is used to mechanically stir for 10 min, heated to 730 °C, and then poured into a mold (preheated to 250 °C) to form a casting blank. The casting blank is homogenized, and the homogenization process is 490 °C × 12 h; the homogenized material is hot-rolled and deformed, the hot-rolling temperature is 430 °C, and the deformation amount is 80%; after hot-rolling, the material is solution-treated and aged, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0052] Tensile specimens with a thickness of 2 mm are prepared by the above method, and the mechanical properties are measured at room temperature. The results are as follows: the tensile strength is 402 MPa, and the elongation is 8.57%.
[0053] Comparative Example 5: Preparation of an Al-Cu based composite material with a 5 µm 0.1% ZrB2 particle content.
[0054] 5 µm ZrB2 particle-Al powder composite powder: The preparation method is the same as that of Comparative Example 2, except that the 50 nm ZrB2 particles are replaced with 5 µm ZrB2 particles;
[0055] The Al-Cu alloy rough smelting billet is placed in a resistance furnace and melted at 760 °C - 780 °C to obtain an Al-Cu alloy melt. A dried impurity remover is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is left to stand. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. An appropriate amount of 5 µm ZrB2 particle-Al powder composite powder is weighed, such that the ZrB2 particles account for 0.1% of the mass of the Al-Cu alloy. At the same time, the 5 µm ZrB2 particle-Al powder composite powder is wrapped with two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid level of the Al-Cu alloy melt, where a mechanical stirring device is used to mechanically stir for 10 min, heated to 730 °C, and then poured into a mold (preheated to 250 °C) to form a casting blank. The casting blank is homogenized, and the homogenization process is 490 °C × 12 h; the homogenized material is hot-rolled and deformed, the hot-rolling temperature is 430 °C, and the deformation amount is 80%; after hot-rolling, the material is solution-treated and aged, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0056] Using the above method to prepare a tensile sample with a thickness of 2 mm, and measuring the mechanical properties at room temperature. The results are as follows: the tensile strength is 449 MPa, and the elongation is 8.11%.
[0057] Comparative Example 6: Preparation of an Al-Cu based composite material with 5 μm 0.5% ZrB2 particle content.
[0058] 5 μm ZrB2 particle - Al powder composite powder: The preparation method is the same as that of Comparative Example 5.
[0059] Place the Al-Cu alloy rough-cast blank in an electric resistance furnace and melt it at 760 °C - 780 °C to obtain an Al-Cu alloy melt. Add a dried impurity remover to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, let it stand. Then cool the aluminum melt to 610 °C - 630 °C. Weigh an appropriate amount of 5 μm ZrB2 particle - Al powder composite powder so that the ZrB2 particles account for 0.5% of the mass of the Al-Cu alloy. At the same time, wrap the 5 μm ZrB2 particle - Al powder composite powder with two layers of aluminum foil and place it in an electric resistance furnace, heat it to 500 °C and keep it warm for two hours. Then take it out and quickly press it under the liquid surface of the Al-Cu alloy melt, where a mechanical stirring device is used to mechanically stir for 10 min, heat up to 730 °C, and then pour it into a casting mold (preheated to 250 °C) to form a casting blank. Carry out homogenization treatment on the casting blank, and the homogenization process is 490 °C × 12 h; carry out hot rolling deformation on the homogenized material, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, carry out solution aging treatment on the material, the solution temperature is 505 °C, the holding time is 2 h, and water quench at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0060] Using the above method to prepare a tensile sample with a thickness of 2 mm, and measuring the mechanical properties at room temperature. The results are as follows: the tensile strength is 431 MPa, and the elongation is 7.61%.
[0061] Comparative Example 7: Preparation of an Al-Cu based composite material with 10 μm 0.1% ZrB2 particle content.
[0062] 10 μm ZrB2 particle - Al powder composite powder: The preparation method is the same as that of Comparative Example 2, with the only difference being that the 50 nm ZrB2 particles are replaced with 10 μm ZrB2 particles;
[0063] The Al-Cu alloy rough smelting billet is placed in a resistance furnace and melted at 760 °C - 780 °C to obtain an Al-Cu alloy melt. A dried impurity removing agent is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is allowed to stand. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. An appropriate amount of 10um ZrB2 particle-Al powder composite powder is weighed, such that the ZrB2 particles account for 0.1% of the mass of the Al-Cu alloy. At the same time, the 10um ZrB2 particle-Al powder composite powder is wrapped with two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid level of the Al-Cu alloy melt, where a mechanical stirring device is used to mechanically stir for 10 min, heated to 730 °C, and then poured into a casting mold (preheated to 250 °C) to form a casting blank. The casting blank is subjected to homogenization treatment, and the homogenization process is 490 °C × 12 h; the homogenized material is subjected to hot rolling deformation, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, the material is subjected to solution aging treatment, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0064] Tensile specimens with a thickness of 2 mm are prepared by the above method, and the mechanical properties are measured at room temperature. The results are as follows: the tensile strength is 451 MPa, and the elongation is 8.63%.
[0065] Comparative Example 8: Preparation of an Al-Cu based composite material with a ZrB2 particle content of 0.5% and a particle size of 10um.
[0066] 10um ZrB2 particle-Al powder composite powder: The preparation method is the same as that of Comparative Example 7.
[0067] The Al-Cu alloy rough smelting billet is placed in a resistance furnace and melted at 760 °C - 780 °C to obtain an Al-Cu alloy melt. A dried impurity removing agent is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is allowed to stand. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. An appropriate amount of 10um ZrB2 particle-Al powder composite powder is weighed, such that the ZrB2 particles account for 0.5% of the mass of the Al-Cu alloy. At the same time, the 10um ZrB2 particle-Al powder composite powder is wrapped with two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid level of the Al-Cu alloy melt, where a mechanical stirring device is used to mechanically stir for 10 min, heated to 730 °C, and then poured into a casting mold (preheated to 250 °C) to form a casting blank. The casting blank is subjected to homogenization treatment, and the homogenization process is 490 °C × 12 h; the homogenized material is subjected to hot rolling deformation, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, the material is subjected to solution aging treatment, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0068] The tensile specimens with a thickness of 2 mm were prepared by the above method, and their mechanical properties were measured at room temperature. The results are as follows: the tensile strength is 421 MPa, and the elongation is 9.2%.
[0069] Comparative Example 9: Preparation of Al-Cu matrix composite material with 10 μm and 1% ZrB2 particle content.
[0070] 10 μm ZrB2 particle-Al powder composite powder: The preparation method is the same as that of Comparative Example 7.
[0071] The Al-Cu alloy rough-cast billet was placed in an electric resistance furnace and melted at 760 °C to 780 °C to obtain an Al-Cu alloy melt. A dried impurity remover was added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it was left standing. Subsequently, the aluminum melt was cooled to 610 °C to 630 °C. An appropriate amount of 10 μm ZrB2 particle-Al powder composite powder was weighed so that the ZrB2 particles accounted for 1% of the mass of the Al-Cu alloy. At the same time, the 10 μm ZrB2 particle-Al powder composite powder was wrapped in two layers of aluminum foil and placed in an electric resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid surface of the Al-Cu alloy melt. A mechanical stirring device was used to mechanically stir for 10 min, heated to 730 °C, and then poured into a casting mold (preheated to 250 °C) to form a casting blank. The casting blank was subjected to homogenization treatment, and the homogenization process was 490 °C × 12 h; the homogenized material was subjected to hot rolling deformation, the hot rolling temperature was 430 °C, and the deformation amount was 80%; after hot rolling, the material was subjected to solution aging treatment, the solution temperature was 505 °C, the holding time was 2 h, and water quenching was carried out at room temperature; the aging temperature was 160 °C, and the holding time was 12 h.
[0072] The tensile specimens with a thickness of 2 mm were prepared by the above method, and their mechanical properties were measured at room temperature. The results are as follows: the tensile strength is 402 MPa, and the elongation is 6.71%.
[0073] Example 1: Preparation of Al-Cu matrix composite material with 10 μm 0.1% + 50 nm 0.1% ZrB2 particle content.
[0074] After mixing 10 μm ZrB2 powder and 50 nm ZrB2 powder in a mass ratio of 1:1, they were ball-milled with Al powder. The mass percentage of Al powder was 70%, and the mass percentage of the mixed ZrB2 powder was 30%. Subsequently, the mixed powder was dried to obtain a (10 μm + 50 nm) micro / nano ZrB2 particle-Al powder composite powder;
[0075] The Al-Cu alloy rough-cast billet is placed in a resistance furnace and melted at 760 °C - 780 °C to obtain an Al-Cu alloy melt. A dried impurity remover is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is left to stand. Subsequently, the aluminum melt is cooled to 610 °C - 630 °C. An appropriate amount of (10um + 50nm) micro / nano ZrB2 particle-Al powder composite powder is weighed, such that both 10um ZrB2 particles and 50nm ZrB2 particles account for 0.1% of the mass of the Al-Cu alloy. At the same time, the ZrB2 particle-Al powder composite powder is wrapped in two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid surface of the Al-Cu alloy melt. Among them, a mechanical stirring device is used for mechanical stirring for 10 min, heated to 730 °C, and then poured into a casting mold (preheated to 250 °C) to form a cast billet. The cast billet is homogenized, and the homogenization process is 490 °C × 12 h; the homogenized material is hot-rolled and deformed, the hot-rolling temperature is 430 °C, and the deformation amount is 80%; after hot-rolling, the material is solution-treated and aged, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0076] Tensile specimens with a thickness of 2 mm are prepared by the above method, and the mechanical properties are measured at room temperature. The results are as follows: the tensile strength is 437 MPa, and the elongation is 10.59%.
[0077] Example 2: Preparation of an Al-Cu-based composite material with a ZrB2 particle content of 10um 0.1% + 50nm 0.5%.
[0078] After mixing 10um ZrB2 powder and 50nm ZrB2 powder in a mass ratio of 1:5, they are ball-milled and mixed with Al powder. The mass percentage of Al powder is 70%, and the mass percentage of the mixed ZrB2 powder is 30%. Subsequently, the mixed powder is dried to obtain a (10um + 50nm) micro / nano ZrB2 particle-Al powder composite powder;
[0079] The Al-Cu alloy rough-cast billet is placed in a resistance furnace and melted at 760 °C to 780 °C to obtain an Al-Cu alloy melt. A dried impurity remover is added to the melt for degassing and refining. After skimming off the reaction by-products on the surface of the melt, it is left standing. Subsequently, the aluminum melt is cooled to 610 °C to 630 °C. An appropriate amount of (10um + 50nm) micro / nano ZrB2 particle-Al powder composite powder is weighed, such that the 10um ZrB2 particles and 50nm ZrB2 particles respectively account for 0.1% and 0.5% of the mass of the Al-Cu alloy. At the same time, the ZrB2 particle-Al powder composite powder is wrapped in two layers of aluminum foil and placed in a resistance furnace, heated to 500 °C and held for two hours, then taken out and quickly pressed under the liquid surface of the Al-Cu alloy melt. Among them, a mechanical stirring device is used for mechanical stirring for 10 min, heated to 730 °C, and then poured into a casting mold (preheated to 250 °C) to form a casting blank. The casting blank is subjected to homogenization treatment, and the homogenization process is 490 °C × 12 h; the homogenized material is subjected to hot rolling deformation, the hot rolling temperature is 430 °C, and the deformation amount is 80%; after hot rolling, the material is subjected to solution aging treatment, the solution temperature is 505 °C, the holding time is 2 h, and water quenching is carried out at room temperature; the aging temperature is 160 °C, and the holding time is 12 h.
[0080] Tensile specimens with a thickness of 2 mm are prepared by the above method, and the mechanical properties are measured at room temperature. The results are as follows: the tensile strength is 441 MPa, and the elongation is 10.71%.
[0081] It can be seen from Comparative Examples 1 to 9 and Examples 1 to 2 that adding ZrB2 particles to the Al-Cu alloy, and the preferred addition amount is 10um 0.1% + 50nm 0.5%, can improve the strength and plasticity of the target alloy at the same time. Compared with the Al-Cu matrix alloy, the tensile strength of the material is increased by 7.2%, and the elongation is increased by 45.6%.
[0082] Table 1 Effects of ZrB2 particles with different sizes and contents on the properties of Al-Cu alloy
[0083]
[0084] 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 foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for preparing a micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material, characterized in that: The following steps are included: (1) Preparation of micro / nano ZrB2 particle-Al powder composite powder: Weighing micron ZrB2 powder or / and nano ZrB2 powder, mixing with Al powder by ball milling, and drying the mixed powder to obtain micro / nano ZrB2 particle-Al powder composite powder; (2) Preparation of high-strength and high-toughness Al-Cu composites reinforced with micro / nano hybrid ZrB2 particles: The Al-Cu alloy billet is placed in a resistance furnace for heating and melting, a de-impurity and degassing agent is added to the melt to perform de-impurity and degassing treatment, then the Al-Cu alloy melt is cooled to 610°C-630°C, and at the same time, a micro / nano ZrB2 particle-Al powder composite powder wrapped with two layers of aluminum foil is placed in a resistance furnace, heated to 480-520°C and kept warm for 1-3 hours, then taken out and quickly pressed under the liquid surface of the Al-Cu alloy melt, heated to 720-740°C after mechanical stirring, and then poured into a preheated casting mold to obtain a ZrB2 particle reinforced Al-Cu aluminum-based composite material ingot; (3) Hot deformation: The ingot is placed in a box furnace for homogenization treatment and then hot rolled; (4) Heat treatment: After hot rolling deformation, solid solution aging treatment is performed to obtain a high-strength and toughness Al-Cu based composite material.
2. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: In step (1), the composition ratio of the micro / nano ZrB2 particle-Al powder composite powder is as follows: the mass percentage of Al powder is 65-75%, and the mass percentage of ZrB2 powder is 25-35%.
3. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: In step (1), the size of the micron ZrB2 powder is 3 to 5 um or / and 8 to 10 um, and the size of the nano ZrB2 powder is 50 to 100 nm; the mixing mass ratio of the micron ZrB2 powder and the nano ZrB2 powder is 1:1 to 1:
5.
4. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: In step (1), the ball milling process parameters are: ball-to-material ratio of 5:1 to 10:1, rotation speed of 150 to 250 rpm / min, and ball milling time of 18 to 24 h.
5. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: In the Al-Cu based composite material prepared in step (2), the micro / nano ZrB2 particles account for 0.1% to 1% of the mass content of the Al-Cu aluminum alloy.
6. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 5, characterized in that: The micro / nano ZrB2 particles are obtained by mixing 10um ZrB2 particles and 50nm ZrB2 particles; 10um ZrB2 particles account for 0.1% of the mass content of Al-Cu aluminum alloy, and 50nm ZrB2 particles account for 0.5% of the mass content of Al-Cu aluminum alloy.
7. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: The preheating temperature of the metal mold is 240-260°C.
8. The method for preparing the micro / nano hybrid scale ZrB2 particle reinforced high-strength and toughness Al-Cu based composite material according to claim 1, characterized in that: In step (3), the homogenization treatment is carried out at a heating temperature of 470° C. to 490° C. and a heat preservation time of 11 h to 13 h.
9. The method according to claim 1, characterized in that: In step (3), the hot rolling temperature is 430° C., the total deformation is 79% to 81%, and the pressing amount in each pass accounts for about 9.8% to 10.2% of the total deformation.
10. The method according to claim 1, characterized in that In step (4), the solution aging treatment is as follows: the solution temperature is 490°C to 510°C, and the holding time is 2h to 2.5h; the aging temperature is 150°C to 170°C, and the holding time is 11h to 13h.