GB2590288A - In-situ nano-reinforced aluminum alloy extruded material for lighweight vehicle bodies and isothermal variable-speed extrusion preparation method - Google Patents

In-situ nano-reinforced aluminum alloy extruded material for lighweight vehicle bodies and isothermal variable-speed extrusion preparation method Download PDF

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GB2590288A
GB2590288A GB2101217.4A GB202101217A GB2590288A GB 2590288 A GB2590288 A GB 2590288A GB 202101217 A GB202101217 A GB 202101217A GB 2590288 A GB2590288 A GB 2590288A
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aluminum alloy
temperature
vehicle bodies
extrusion
situ
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Zhao Yutao
Kai Xizhou
Tao Ran
Chen Gang
Pu Jianying
Li Qirong
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Jiangsu University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/01Extruding metal; Impact extrusion starting from material of particular form or shape, e.g. mechanically pre-treated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/001Extruding metal; Impact extrusion to improve the material properties, e.g. lateral extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/002Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B21C31/00Control devices, e.g. for regulating the pressing speed or temperature of metal; Measuring devices, e.g. for temperature of metal, combined with or specially adapted for use in connection with extrusion presses
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/001Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
    • B22D11/003Aluminium alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B22D11/04Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/049Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds for direct chill casting, e.g. electromagnetic casting
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    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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    • C22C32/001Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract

The present invention relates to an aluminum-based composite material, in particular to an in-situ nano-reinforced aluminum alloy for lightweight vehicle bodies and an isothermal variable-speed extrusion method. The method uses in-situ synthesis technology to directly synthesize single-element or multi-element nano-reinforced particles in an aluminum melt by applying an external field to prepare a composite material semi-continuous casting bar with fine grains, wherein an optimally prepared mixed powder containing a generated ceramic phase reinforcement element is used as a reactant, and subjecting the casting bar to four-stage homogenization and isothermal variable-speed extrusion deformation and then to a T4P+ artificial aging heat treatment to finally obtain a high-toughness anti-impact in-situ nano-reinforced aluminum alloy extruded profile for lightweight vehicle bodies. The extruded profile for vehicle bodies as prepared by the present invention has the characteristics of a high strength, a good formability, impact resistance and fatigue resistance, and solves the problem of aluminum alloys for lightweight vehicle bodies having a low comprehensive performance and not being able to completely replace steel as a vehicle body material.

Description

IN-SITU NANO-REINFORCED ALUMINUM ALLOY EXTRUDED MATERIAL FOR LIGHTWEIGHT VEHICLE BODIES AND PREPARATION METHOD OF ISOTHERMAL VARIABLE-SPEED EXTRUSION
Technical Field
The present invention relates to an aluminum-based composite material, and in particular to an in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies and a preparation method of isothermal variable-speed extrusion.
Background
The world automobile industry is now facing increasingly severe problems, mainly involved in energy, environment and safety. For currently widely used steel vehicle bodies, problems such as high fuel consumption and serious environmental pollution are caused due to the heavy weight. Now, the simplest method is to use lightweight materials to reduce the weight of automobiles, and the development of the lightweight materials for vehicle bodies is also a research hotspot at present. A research report of the International Energy Conservation Environmental Protection Association points out that the automobile vehicle body accounts for about 30% of the total weight of the automobile, and the use of an aluminum alloy in place of steel on the vehicle body can reduce the weight of the vehicle body by about 40-50% and reduce the fuel consumption by 26-30%. 6000 Series aluminum alloys have high strength, good formability, corrosion resistance, weldability, and baking paint performance, and thus they are currently the key materials for lightweighting of automobile vehicle bodies. Aluminum materials represented by 6016, 6111, 6022 and 6005A have been more and more widely applied in outer panels of automobile vehicle bodies manufactured abroad.
Chinese Patent No. 20100199928.9 discloses a processing method for improving the stamping formability of 6111 aluminum alloy automobile panels, wherein 6111 alloy ingots produced by semi-continuous casting are heat-treated at 220°C-425°C for 8-15 h, and then homogenized as the furnace heats up, followed by hot rolling, to improve the stamping formability and baking paint strength. Chinese Patent No. 201410800786.5 discloses a 6016 aluminum alloy sheet for automobile vehicle bodies and a production method thereof, wherein through smelting and casting, face milling, hot rolling, cold rolling, and heat treatment process steps, the yield strength of the aluminum alloy sheet and the yield of the stamping type are improved. Chinese Patent No. 200710190078.4 discloses a method for improving the bake hardenability of low Cu-containing aluminum alloy automobile panels, wherein after the 6022 sheet is subjected to solution treatment and water quenching, it is preheated within 1 h at a treatment temperature of 60-200°C for a treatment time of 2-30 min, to significantly improve the bake hardenability of the sheet.
At present, the existing aluminum vehicle body technologies and review literatures further improve the comprehensive performance, and especially the formability of the vehicle body materials, mainly through regulation of the heat treatment process. However, these technologies still suffer from the following disadvantages: (I) it is difficult to get rid of the inverse relationship between strength and plasticity by relying on traditional precipitation strengthening of alloys, where the plasticity is usually improved at the cost of the strength; (2) the heat treatment process has a high temperature, a long time and a complicated process and therefore is not suitable for industrialized continuous batch production; and (3) with the development of industry, traditional aluminum alloys can no longer meet the performance requirements on the new generation of steel sheets, and cannot completely replace steel Therefore, it is urgent to develop a novel high-toughness aluminum-based material.
1n-situ generated nanoparticle-reinforced aluminum-based composite materials have become groundbreaking new materials in the cross field of nanomaterials and aluminum-based composite materials in recent years, because of the advantages, for example, their nano-reinforcement is a thermodynamically stable phase which nucleates and grows in situ from an aluminum matrix through chemical reaction, thus the surface of the reinforcement has no contamination, avoiding the problem of poor compatibility with the matrix, and thus the interface bonding strength is high, so they have a high specific strength, a high specific modulus, an excellent fatigue resistance, a very good heat resistance, a corrosion resistance and the like; and the materials can be directly synthesized by melt reaction, greatly reducing the cost. However, the preparation of the in-situ aluminum-based nanocomposite materials is relatively difficult, and there are still "bottlenecks" that have not been overcome: 1) The morphology and size of the generated particles are not easy to control, and the submicron scale cannot be achieved yet, while the nanoscale is difficult to achieve; and 2) the generated nanoparticles tend to agglomerate and are distributed non-uniformly.
Summary
In view of drawbacks in the prior art, the present invention aims to develop an in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies and a preparation method of isothermal variable-speed extrusion, where a high-frequency pulsed magnetic field and a high-energy ultrasonic field are employed to regulate the preparation process of the material, and in combination with an optimized four-stage homogenization technology and an isothermal variable-speed extrusion technology, to achieve uniform distribution of nanoparticle clusters in grains and grain boundaries, thereby obtaining a fine-grained structure, and significantly improving the strength, formability, impact resistance and fatigue resistance of the vehicle body material.
The present invention can effectively solve disadvantages of 6 Series aluminum alloys currently used for vehicle bodies having a lower strength and a poorer formability compared with steel. These two major disadvantages are the key to determining whether aluminum alloys for lightweighting vehicle bodies can replace steel panels. In-situ generated nanoparticles are a thermodynamically stable phase that nucleates and grows in-situ from an aluminum matrix through chemical reaction, and thus the surface of the reinforcement has no contamination and has a high bonding strength, and in combination with a regulation technology by an external field to promote the dispersion and nucleation of reinforcing particles, a semi-continuous casting of a composite material with nano-reinforcing phase clusters uniformly distributed in grains and grain boundaries and a fine-grained structure can be obtained. Through the Orowan reinforcement of nanoparticles, fine-grain reinforcement, nano-reinforcement toughening, dispersion and reinforcement of nano-precipitated phases, and the damping effect, the contradiction between high strength and good formability of aluminum alloys for lightweighting vehicle bodies is eliminated, and the strength, formability, impact resistance and fatigue resistance of the material itself are maximized. Subsequently, through the optimized four-stage homogenization treatment and isothermal variable-speed extrusion forming technology, the metal deformation resistance and metal flow uniformity are controlled, ensuring that the front and rear ends of the profile have a fine structure and a uniform distribution, to allow the material to have a relatively stable strength, formability, impact resistance and fatigue resistance, thereby obtaining an aluminum-based composite extruded material for vehicle bodies that can replace steel panels.
The system of the present invention adopts a synthesis method through direct melt reaction, wherein an aluminum melt is first melted to the reaction temperature, and then the reactants are mixed into the melt in a predetermined proportion for reaction to generate nano-scale particles. Compared with other methods for preparing composite materials, this method has the following characteristics: (1) excellent thermodynamic stability; (2) smooth interface between the matrix and the reinforcing particles, and firm bonding; and (3) small particle morphology and diffuse distribution.
Particular technical solutions of the present invention are as follows: The method for preparing the aluminum alloy extruded material includes the following steps: smelting an aluminum alloy raw material into a melt at 750-850°C, then wrapping an oven-dried in-situ reactant powder with a high-purity aluminum foil and pressing the oven-dried in-situ reactant powder wrapped with the high-purity aluminum foil into the melt by a high-purity graphite bell jar for reaction for 20-60 min with assistance of an external field applied during the reaction to obtain a product, purifying the product after the reaction to prepare a semi-continuous cast rod of a composite material, followed by four-stage homogenization treatment, and subjecting the treated aluminum alloy cast rod to isothermal variable-speed extrusion processing and heat treatment, to finally prepare a high-toughness impact-resistant in-situ nano-reinforced aluminum alloy extruded material for lightweighting vehicle bodies.
The aluminum alloy raw material has the following chemical constituents and mass percentages thereof: Si 1.2-2.5%, Mg 1.0-1.5%, Cu 0.1-0.2%, Mn 0.1-0.2%, Fe 0.05-0.1%, Zn 0.2-0.4%, La 0.05-0.1%, Ti 0.2-0.3%, Er 0.02-0.05%, and Y 0.05-0.1%, with the balance being aluminum and other inevitable impurities, wherein a percentage content of the other inevitable impurities should be < 0.12%.
In the aluminum alloy raw material, a mass Mn to Fe is 1-4:1-1.5 The oven-dried in-situ reactant powder containing elements that form a ceramic phase reinforcement includes: (1) Potassium fluorozirconate (K2ZrF6) and potassium fluoroborate (KBE°, which react to generate in-situ ZrB2 nanoparticles, wherein a weight ratio of the potassium fluorozirconate (K2ZrF6) to the potassium fluoroborate (KBF4) is 25-27:37-40, and the powder is added in an amount of 10-35% based on the weight of the aluminum alloy raw material, with a reaction formula as follows: 31(7rF6} 6 1(13F4 I okI=3Zx t-9KAIErl. K3AiF (2) Cerium carbonate (Ce)(CO3)3), which reacts to generate in-situ A1/03 nanoparticles, and is added in an amount of 5-20% based on the weight of the aluminum alloy raw material, with a reaction formula as follows: 2Ce2(CO3)3+4 A1.2A1203+1Ce+6Cth.
(3) Borax (Na213407) and potassium fluorozirconate (K2ZrF6), which react to generate bi-component Zr132+A1203 nanoparticles, wherein a mass ratio of the borax to the potassium 5 at o of Si to Mg s 1.2-5:1-2; and a mass at o of fluorozirconate is 5-7.10-15, and the powder is added in an amount of 15-40% based on the weight of the aluminum alloy raw material, with a reaction formula as follows: " 30Kgt-Pc,+60A1,12ir07,+187TB-± I 3A1300,18 K A1 P61-kAIF3±24KE (4) Borax (Na2B407), potassium fluorozirconate (K2ZrF6) and potassium fluorotitanate (K2TiF6), which react to generate multi-component ZrB2+A1203+TiB2 nanoparticles, wherein a mass ratio of the borax, the potassium fluorozirconate and the potassium fluorotitanate is 3-5.2-3.2-3, and the powder is added in an amount of 35-50% based on the weight of the aluminum alloy raw material, with a reaction formula as follows.
4-1 ii.;;ZrE,+ I 5K +16 A1F4+1.
Therefore, the present invention employs four reaction systems to prepare the in-situ nanoparticle reinforced aluminum-based composite material.
The direct melt reaction is performed at a temperature controlled at 780-870°C.
The assistance of the external field is performed by an acousto-magnetic coupling field, which includes a high-frequency pulsed magnetic field and a high-energy ultrasonic field The high-frequency pulsed magnetic field has a frequency of 15-30 Hz and a magnetizing current of 180-240 A. The high-energy ultrasonic field has a power of 1000-1500 W and a frequency of 15-22 kHz. The acousto-magnetic coupling field can generate acoustic streaming in two directions, which can avoid the phenomenon of particle segregation outside caused by a single magnetic field, and the distribution of cavitation bubbles along the axis of the horn due to acoustic streaming of a single ultrasonic field Moreover, the acousto-magnetic coupling field can ensure that the mass and heat transfer process of the entire metal melt is completely carried out, making the concentration of each area in the metal melt uniform and inhibiting the growth of particles. Therefore, the acousto-magnetic coupling field can not only avoid disadvantages of a single physical field, but also amplify advantages of the single physical field.
The semi-continuous cast rod of the composite material is produced through direct water-cooling semi-continuous casting.
The multi-stage homogenization treatment is four-stage homogenization treatment, wherein the cast rod is heated up to 480-490°C for 8-10 h, 495-510°C for 3-5 h, 515-530°C for 3-5 h, and then 540-570°C for 10-15 h. For the homogenization treatment by the gradual heating up, first, the cast rod is kept at a relatively low temperature for a long time to uniformly diffuse alloying elements and eliminate dendrites, then the temperature is increased to near a melting point of a low-melting-point eutectic and kept for a period of time in order to dissolve the low-melting-point eutectic and greatly reduce the size of the remaining eutectic, and finally, the temperature is increased to a high melting point so that the eutectic is sufficiently dissolved and grains do not grow significantly. The problem of single-or two-stage homogenization being incapable of completely eliminating a eutectic phase and element segregation can be solved effectively, which has a positive impact on subsequent extrusion processing and heat treatment.
In the isothermal variable-speed extrusion, an extrusion billet is heated at a temperature of 450-500°C, with an extrusion die being at a temperature of 440-490°C, an extrusion pad being at a temperature of 430-480°C, and an extrusion cylinder being at a temperature of 420-470°C. A self-feedback variable-speed intelligent control system is used during the extrusion process, where due to intelligent correlation between an extrusion speed and an outlet temperature of the extruded material, the extrusion speed can be regulated by constant temperature control, thereby obtaining the extruded material with consistent structure and performance. The extrusion speed is regulated within a range of I mm/s-50 mm/s. The isothermal variable-speed extrusion process can ensure that the temperature of the metal in a deformation zone near an extrusion outlet remains constant, thereby keeping a pressure of a die mouth constant, and thus can control metal deformation resistance and metal flow uniformity, so that the difference in strength between a head and tail of an extruded profile in an experiment is not higher than 10 MPa, which can solve the phenomenon of material cracking and distortion caused by the difference in the die outlet temperature during the extrusion process, so that the profile prepared by the present invention has a relatively high strength, a good formability, an impact resistance and fatigue resistance, and the production efficiency is improved.
The heat treatment is T4P+ artificial aging, including solution quenching at a temperature of 540-570°C for a holding time of 1.5-5 h, water quenching; pre-aging at a temperature of 130-170°C for a holding time of 10-30 min; natural aging by standing at room temperature for 15-20 d; and artificial aging at a temperature of 170-180°C for a holding time of 20-60 min. Finally, a qualified extruded rod for vehicle bodies is obtained.
The present invention has the following beneficial effects: The present invention provides an in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies and a preparation method of isothermal variable-speed extrusion. By an in-situ synthesis technology and a regulation technology through application of an external field, a semi-continuous casting of an in-situ reinforced aluminum-based composite material with uniformly distributed single-component or multi-component in-situ nanoparticle (50 nm-200 nm) clusters and fine grains is obtained. Then, by the designed and optimized four-stage homogenization and isothermal variable-speed extrusion forming, the metal deformation resistance and the metal flow uniformity are controlled, and as a result, the difference in strength between the head and tail of the extruded profile is not higher than 10 MPa, so that the extruded piece prepared by the present invention has a relatively high strength, a good formability, a relatively high impact resistance and fatigue resistance, and can improve the safety of the entire vehicle when applied to a vehicle body and reduce the risk of passenger injury in the event of a collision.
Brief Description of the Drawings
In order to explain the technical solutions of the present invention more clearly, the accompanying drawings that need to be used will be briefly introduced below. Obviously, the accompanying drawings in the following description are some examples of the present invention. For those of ordinary skill in the art, other accompanying drawings can be further obtained based on these accompanying drawings without creative work.
FIG. I is a flow diagram of the preparation process according to the present invention.
FIG. 2 is a structure image of an ingot of the in-situ nano-reinforced aluminum-based composite material for vehicle bodies according to the present invention.
(a) ZrB2 reinforced aluminum-based composite material; (b) A1103 reinforced aluminum-based composite material; (c) ZrB2+A1203 reinforced aluminum-based composite material; and (d) ZrB2+A1203+TiB2 reinforced aluminum-based composite material.
FIG. 3 is a structure image with hot extrusion of the in-situ nano-reinforced aluminum-based composite material for vehicle bodies according to the present invention.
(a) ZrB2 extruded material; (b) A1203 extruded material; (c) ZrB2+A1203 extruded material; and (d) ZrB2+A1203+TiB2 extruded material.
FIG. 4 is a morphological image of the nano-reinforcing particles according to the present invention.
(a) ZrB2 particles (b) A120; particles (c) ZrB2+A1203 particles and (d) ZrB2+A1203+TiB2 particles.
Detailed Description of the Embodiments
In order to make the objectives, technical solutions, and advantages of the examples of the present invention clearer, the technical solutions in the examples of the present invention will be described clearly and completely in combination with the accompanying drawings in the examples of the present invention. Obviously, the examples described are a part of the examples of the present invention, but not all the examples. Based on the examples of the present invention, all other examples obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present invention.
Example 1:
Raw material: Cu 0.2%, Mg 1%, Si 1.2%, Fe 0.05%, Mn 01%, Zn 0.4%, La 0.1%, Ti 01%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6) and potassium fluoroborate (KBF4) powder with a purity of 98%.
The method for preparing the automobile vehicle body material included the following steps: (1) Smelting of aluminum alloy: During smelting of 1 kg of an aluminum alloy raw material, when a molten aluminum formed by melting the aluminum alloy reached a temperature of 850°C, a powder oven-dried at 200°C and then mixed and ground was added in portions (with a particle size less than 100 pm, the mass of potassium fluorozirconate: 163 g, and the mass of potassium fluoroborate: 177 g). At the same time, a combined device of a high-frequency pulsed magnetic field and a high-energy ultrasonic field was switched on (magnetic field: frequency 20 Hz, magnetizing current 200 A; ultrasonic field: power 1000 W, frequency 20 kHz) for reaction over 30 min. At the end of the reaction, the scum on the surface was removed, and after the temperature was reduced to 780°C, the molten alloy was purified (a refining agent hexachloroethane was sprayed into the molten alloy in portions to perform refinement for 10 min, followed by slagging).
(2) Semi-continuous casting: When the melt was at a temperature of 750°C, the melt was injected into a crystallizer. After the melt was solidified and crusted at a graphite ring, the starter head was lowered at a speed of 30 mm/min, and at the same time, cooling water was turned on for cooling at a water temperature of 25°C and a water pressure of 0.2 ATPa. After the casting was completed, the cast rod was lifted, obtaining a semi-continuous cast rod of 3% vol ZrB2/AA611 I aluminum-based composite material with a diameter of 60 mm.
(3) Four-stage homogenization treatment: The cast rod obtained in Step (2) was cut at the head and the tail and subjected to face milling, producing a short cast rod with a length of 100 mm. Then the cast rod was placed into a box-type resistance furnace, heated up to 480°C for 8 h, 500°C for 5 h, 530°C for 5 h, and then 570°C for 12 It (4) Isothermal variable-speed extrusion: The cast rod obtained in Step (3) was placed in a resistance furnace for preheating at a temperature of 500°C, then the heating temperature of the extrusion die was set to 490°C, the temperature of the extrusion pad was set to 480°C, and the temperature of the extrusion cylinder was set to 470°C. The average extrusion speed was 45 mm/s. Finally, an extruded rod with a diameter of 200 mm and a length of 500 mm was obtained.
(5) T4P+ artificial aging: The extruded rod was subjected to heat treatment. Solution quenching at a temperature of 545°C for a holding time of 2 h, water quenching; pre-aging at a temperature of 150°C for a holding time of 10 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 170°C for a holding time of 30 min. Finally, a qualified extruded rod for vehicle bodies was obtained.
Example 2:
Raw material: Cu 0.2%, Mg 1%, Si 1.2%, Fe 0.05%, Mn 0.2%, Zn 0.4%, La 0.1%, Ti 0.2%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial cerium carbonate (Ce2(CO3)3) powder with a purity of 99.9%.
The preparation method was substantially the same as that in Example 1, except for 1) using a different reaction system, where 3% vol A1203/AA6111 aluminum-based composite material was prepared with cerium carbonate. The cerium carbonate powder was oven-dried at 250°C, and then mixed and ground (with a particle size less than 100 um, and the mass of cerium carbonate: 180 g). 2) Four-stage homogenization: Heating up to 480°C for 10 h, 500°C for 4 h, 530°C for 4 h, and then 560°C for 10 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 550°C for a holding time of 2 h, water quenching; pre-aging at a temperature of 160°C for a holding time of 10 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 170°C for a holding time of 30 min.
Example 3:
Raw material: Cu 0.2%, Mg 1%, Si 1.2%, Fe 0.05%, Mn a2%, Zn 0.4%, La 0.1%, Ti 01%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6) and borax (Na2B407) powder with a purity of 98%.
The preparation method was substantially the same as that in Example 1, except for 1) using a different reaction system, where 3% vol A1203+ZrR2/AA611 I aluminum-based composite material was prepared with potassium fluorozirconate and borax. The powder was oven-dried at 200°C, and then mixed and ground (with a particle size less than 100 l.tm, the mass of borax: 101 g, and the mass of potassium fluorozirconate: 240 g). 2) Four-stage homogenization: Heating up to 480°C for 8 h, 500°C for 3 h, 530°C for 3 h, and then 560°C for 15 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 560°C for a holding time of 2 h, water quenching; pre-aging at a temperature of 160°C for a holding time of 10 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 170°C for a holding time of 30 min
Example 4:
Raw material: Cu 0.2%, Mg 1%, Si 1.2%, Fe 0.05%, Mn 01%, Zn 0.4%, La 0.1%, Ti 01%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6), potassium fluorotitanate (K2TiF6) and borax (Na2B407) powder with a purity of 98%.
The preparation method was substantially the same as that in Example I, except for 1) using a different reaction system, where 3% vol A12013+Zrth+TiB2 aluminum-based composite material was prepared with potassium fluorozirconate, potassium fluorotitanate and borax powder. The powder was oven-dried at 200°C, and then mixed and ground (with a particle size less than 100 pm, the mass of borax: 344 g, the mass of potassium fluorozirconate: 134 g, and the mass of potassium fluorotitanate: 137). 2) Four-stage homogenization: Heating up to 480°C for 10 h, 510°C for 5 h, 530°C for 5 h, and then 570°C for 12 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 570°C for a holding time of 4 h, water quenching; pre-aging at a temperature of 170°C for a holding time of 30 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 180°C for a holding time of 40 min
Example 5:
Raw material: Cu 0.1%, Mg 1.0%, Si 2.5%, Fe 0.05%, Mn 0.15%, Zn 0.2%, La 0.1%, Ti 0.2%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6) and potassium fluoroborate (KBF4) powder with a purity of 98%.
Steps (1) and (2) of the method for preparing the automobile vehicle body material were the same as those of Example 1, but the following steps were different from those of Example 1.
(3) Four-stage homogenization treatment: The cast rod obtained in Step (2) was cut at the head and the tail and subjected to face milling, producing a short cast rod with a length of 200 mm. Then the cast rod was placed into a box-type resistance furnace, heated up to 490°C for 8 h, 5 I 0°C for 5 h, 520°C for 5 h, and then 565°C for 12 h. (4) Isothermal variable-speed extrusion: The cast rod obtained in Step (3) was placed in a resistance furnace for preheating at a temperature of 450°C, then the heating temperature of the extrusion die was set to 440°C, the temperature of the extrusion pad was set to 430°C, and the temperature of the extrusion cylinder was set to 420°C. The average extrusion speed was 45 mm/s. Finally, an extruded rod with a diameter of 200 mm and a length of 500 mm was obtained.
(5) T4P+ artificial aging: The extruded rod was subjected to heat treatment. Solution quenching at a temperature of 550°C for a holding time of 4 h, water quenching; pre-aging at a temperature of 160°C for a holding time of I 0 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 180°C for a holding time of 30 min. Finally, a qualified extruded rod for vehicle bodies was obtained.
Example 6:
Raw material: Cu 0.1%, Mg 1.0%, Si 2.5%, Fe 0.05%, Mn 0.15%, Zn 0.2%, La 0.1%, Ti 0.2%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial cerium carbonate (Ce2(CO3)3) powder with a purity of 99.9%.
The preparation method was substantially the same as that in Example 4, except for 1) using a different reaction system, where 3% vol A1201/AA6016 aluminum-based composite material was prepared with cerium carbonate. The cerium carbonate powder was oven-dried at 250°C, and then mixed and ground (with a particle size less than 100 (tin, and the mass of cerium carbonate: 180 g). 2) Four-stage homogenization: Heating up to 490°C for 10 h, 510°C for 4 h, 520°C for 4 h, and then 565°C for 10 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 555°C for a holding time of 4 h, water quenching; pre-aging at a temperature of 160°C for a holding time of 15 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 180°C for a holding time of 30 min.
Example 7:
Raw material: Cu 0.1%, Mg 1.0%, Si 2.5%, Fe 0.05%, Mn 0.15%, Zn 0.2%, La 0.1%, Ti 0.2%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6) and borax (Na2B407) powder with a purity of 98% The preparation method was substantially the same as that in Example 4, except for 1) using a different reaction system, where 3% vol A1203+ZrB2 aluminum-based composite material was prepared with potassium fluorozirconate and borax. The powder was oven-dried at 200°C, and then mixed and ground (with a particle size less than 100 pm, the mass of borax: 101 g, and the mass of potassium fluorozirconate: 240 g). 2) Four-stage homogenization: Heating up to 490°C for 8 h, 510°C for 3 h, 520°C for 3 h, and then 565°C for 12 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 560°C for a holding time of 4 h, water quenching; pre-aging at a temperature of 160°C for a holding time of 20 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 180°C for a holding time of 30 min
Example 8:
Raw material: Cu 0.1%, Mg 10%, Si 2.5%, Fe 0.05%, Mn 015%, Zn a2%, La 0.1%, Ti 0.2%, Er 0.05%, and Y 0.05%, with the balance being Al and other inevitable impurities, where the percentage content of the other inevitable impurities should be < 0.12%.
Solid powder: Industrial potassium fluorozirconate (K2ZrF6), potassium fluorotitanate (K2TiF6) and borax (Na2B407) powder with a purity of 98%.
The preparation method was substantially the same as that in Example 4, except for 1) using a different reaction system, where 3% vol A1203+Zrth+TiB2 aluminum-based composite material was prepared with potassium fluorozirconate, potassium fluorotitanate and borax powder. The powder was oven-dried at 200°C, and then mixed and ground (with a particle size less than 100 pm, the mass of borax: 344 g, the mass of potassium fluorozirconate: 134 g, and the mass of potassium fluorotitanate: 137). 2) Four-stage homogenization: Heating up to 490°C for 10 h, 510°C for 4 h, 520°C for 5 h, and then 570°C for 14 h. 3) Using a different heat treatment process: Solution quenching at a temperature of 570°C for a holding time of 4 h, water quenching; pre-aging at a temperature of 170°C for a holding time of 30 min; natural aging by standing at room temperature for 20 d; and artificial aging at a temperature of 180°C for a holding time of 40 min. In the examples, the performance of the specific materials is shown in the following table: Table 1. Performance test results of the nano-reinforced composite extruded material provided by each of the examples \ Performance Impact energy Tensile strength Yield strength Elongation 0 (MPa) (MPa) (/0) (10*I0*10,
Example
U-shaped notch) Example 1 342 239 23.5 20 Example 2 330 225 24.1 22 Example 3 350 250 25.2 25 Example 4 362 270 26.5 27 Example 5 315 218 24.5 22 Example 6 310 215 26 26 Example 7 322 223 26.8 27 Example 8 345 238 28.1 29 In sum -nary, the examples of the present invention have the following beneficial effects: The tensile strength and the yield strength are greatly improved. The elongation is high, and the formability is good. Also, it can be seen that ZrB2 particle reinforcement can significantly improve the strength, but the elongation is not significantly improved. A1203 particle reinforcement can significantly increase the elongation, but the strength is not significantly improved. However, each performance is significantly improved in the case of bi-component particle and tri-component particle reinforcement. Therefore, the performance indicators in the examples of the present invention consistently show better performance than the matrix alloy, and each mechanical performance can meet the requirements for automobile vehicle body materials.
The present invention provides an in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies and a preparation method of isothermal variable-speed extrusion, and in combination with the accurate control of the process parameters of the preparation method and the selection of the reaction system, the present invention obtains a lightweight high-toughness vehicle body material. This provides a reference basis for the preparation of high-performance materials for lightweight vehicle bodies in the future, and has broad market prospects and economic value.
The above descriptions are only preferred examples of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, and the like, made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims (8)

  1. Claims What is claimed is: 1. A preparation method of isothermal variable-speed extrusion of an in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies, characterized by comprising the following steps: adding a mixed powder containing elements that form a ceramic phase reinforcement as a reactant into a melt formed by smelting an aluminum alloy raw material, in situ synthesizing single-component or multi-component nano-reinforcing particles by a direct melt reaction with assistance of an external field to produce a semi-continuous cast rod of a composite material, and then performing isothermal variable-speed extrusion processing and heat treatment on the aluminum alloy cast rod after four-stage homogenization treatment to obtain the high-toughness impact-resistant in-situ nano-reinforced aluminum alloy extruded material for lightweighting vehicle bodies.
  2. 2. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim 1, characterized in that the aluminum alloy raw material has the following chemical constituents and mass percentages thereof: Si 1.2-2.5%, Mg 1.0-1.5%, Cu 0.1-0.2%, Mn 0.1-0.2%, Fe 0.05-0.1%, Zn 0.2-0.4%, La 0.05-0.1%, Ti 0.2-0.3%, Er 0.02-0.05%, and Y 0.05-0.1%, with the balance being aluminum and other inevitable impurities, wherein a percentage content of the other inevitable impurities should be < 0.12%; and in the aluminum alloy raw material, a mass ratio of Si to Mg is 1.2-5:1-2; and a mass ratio of Mn to Fe is 1-4:1-1.5.
  3. 3. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim 1, characterized in that different nano-reinforcing particles are prepared by four reaction systems; the mixed powder containing the elements that form the ceramic phase reinforcement comprises: (1) potassium fluorozirconate (K2ZrF6) and potassium fluoroborate (KBF4), which react to generate in-situ Zr132 nanoparticles, wherein a weight ratio of the potassium fluorozirconate (K2ZrF6) to the potassium fluoroborate (KI3F4) is 25-27:37-40, and the powder is added in an amount of 10-35% based on the weight of the aluminum alloy raw material; (2) cerium carbonate (C$CO3)3), which reacts to generate in-situ A1203 nanoparticles, and is added in an amount of 5-20% based on the weight of the aluminum alloy raw material; (3) borax (Na213407) and potassium fluorozirconate (K2ZrF6), which react to generate bi-component Zr132+A1203 nanoparticles, wherein a mass ratio of the borax to the potassium fluorozirconate is 5-7:10-15, and the powder is added in an amount of 15-40% based on the weight of the aluminum alloy raw material; or (4) borax (Na23407), potassium fluorozirconate (K2ZrF6) and potassium fluorotitanate (K2TiF6), which react to generate multi-component Zr132-EA1203+TiB2 nanoparticles, wherein a mass ratio of the borax, the potassium fluorozirconate and the potassium fluorotitanate is 3-5:2-3:2-3, and the powder is added in an amount of 35-50% based on the weight of the aluminum alloy raw material.
  4. 4. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim 1, characterized in that the direct melt reaction is performed at a reaction temperature controlled at 780-870°C.
  5. 5. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim I, characterized in that the assistance of the external field is performed by an acousto-magnetic coupling field, which comprises a high-frequency pulsed magnetic field and a high-energy ultrasonic field, wherein the high-frequency pulsed magnetic field has a frequency of 15-30 Hz and a magnetizing current of 180-240 A; and the high-energy ultrasonic field has a power of 1000-1500 W and a frequency of 15-22 kHz.
  6. 6. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim 1, characterized in that the four-stage homogenization treatment is performed by heating the cast rod up to 480-490°C for 8-10 h, 495-510°C for 3-5 h, 515-530°C for 3-5 h, and then 540-570°C for 10-15 h; for the homogenization treatment by the gradual heating up, first, the cast rod is kept at a relatively low temperature for a long time to uniformly diffuse alloying elements and eliminate dendrites, then the temperature is increased to near a melting point of a low-melting-point eutectic and kept for a period of time in order to dissolve the low-melting-point eutectic and greatly reduce the size of the remaining eutectic, and finally, the temperature is increased to a high melting point so that the eutectic is sufficiently dissolved and grains do not grow significantly; and the problem of single-or two-stage homogenization being incapable of completely eliminating a eutectic phase and element segregation can be solved effectively, which has a positive impact on subsequent extrusion processing and heat treatment.
  7. 7. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim 1, characterized in that in the isothermal variable-speed extrusion, an extrusion billet is heated at a temperature of 450-500°C, with an extrusion die being at a temperature of 440-490°C, an extrusion pad being at a temperature of 430-480°C, and an extrusion cylinder being at a temperature of 420-470°C; and an extrusion speed is regulated within a range of 1 mm/s-50 mm/s.
  8. 8. The preparation method of isothermal variable-speed extrusion of the in-situ nano-reinforced aluminum alloy extruded material for lightweight vehicle bodies according to claim I, characterized in that the heat treatment is T4P+ artificial aging, comprising solution quenching at a temperature of 540-570°C for a holding time of 1.5-5 h, water quenching; pre-aging at a temperature of 130-170°C for a holding time of 10-30 min; natural aging by standing at room temperature for 15-20 d; and artificial aging at a temperature of 170-180°C for a holding time of 20-60 min.
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