WO2021114967A1 - 一种原位三元纳米颗粒增强铝基复合材料的制备方法 - Google Patents

一种原位三元纳米颗粒增强铝基复合材料的制备方法 Download PDF

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WO2021114967A1
WO2021114967A1 PCT/CN2020/126671 CN2020126671W WO2021114967A1 WO 2021114967 A1 WO2021114967 A1 WO 2021114967A1 CN 2020126671 W CN2020126671 W CN 2020126671W WO 2021114967 A1 WO2021114967 A1 WO 2021114967A1
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tib
composite material
reinforced
aluminum
based composite
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French (fr)
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赵玉涛
靳利伟
钱炜
怯喜周
高旭
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江苏大学
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1068—Making hard metals based on borides, carbides, nitrides, oxides or silicides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides

Definitions

  • the invention provides a method for preparing an in-situ ternary nano-particle reinforced aluminum-based composite material, which belongs to the technical field of aluminum-based composite material preparation.
  • In-situ particle-reinforced aluminum-based composites are made by adding solid powder reaction salt containing reinforcement phase particle forming elements to the surface of molten aluminum alloy at a certain temperature, and then stirring to make it fully proceed, thereby generating reinforcement in the aluminum melt Particles.
  • in-situ composite materials have the following characteristics: (1) The reinforcement particles are thermodynamically stable phases that nucleate and grow in-situ from the matrix. Therefore, when acting at high temperatures, the reinforcement particles are not Will decompose or transform into other compounds. (2) By rationally selecting the type and composition of the compound, the type, size and quantity of the in-situ reinforcement can be effectively controlled.
  • Chinese patent 201811286812.1 adopts the Zr and H 3 BO 3 system, the melt direct reaction technology and the electromagnetic control technology to prepare ZrB 2 and Al 2 O 3 dual-phase nano-reinforced particles solve the problem of uneven particle distribution, forming square ZrB2 particles and round Al 2 O 3 particles with uniform distribution and sizes of 50-100nm.
  • the composite material is treated with T6 heat treatment. After that, the strength increased by 23.4%, the elongation increased by 62%, and the impact resistance increased by 38%.
  • Chinese patent 201811286813.6 uses borax (Na 2 B 4 O 7 ) and potassium fluorozirconate (K 2 ZrF 6 ) powder as a mixed reaction salt to prepare ZrB 2 and Al 2 O 3 dual-phase nano-reinforced particles, and uses mechanical stirring to control its aluminum alloy
  • the smelting process and the addition of rare earth master alloys to refine the matrix grains, the use of acousto-magnetic coupling to control the in-situ reaction process of the composite material, and the application of ultrasonic vibration during the solidification process make the size of the binary nanoparticles smaller and the distribution more uniform, making The strength and toughness of composite materials have been significantly improved.
  • the nano-particle reinforcement phase prepared by in-situ reaction technology is mainly concentrated in the unit, but there are few related literature reports on the preparation of multi-element nano-particle reinforced aluminum-based composites by in-situ melt reaction, so there is an urgent need to develop a new type of reaction system and method To solve the problem of reaction preparation of multi-component nanoparticles and low particle yield.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide an in-situ ternary nanoparticle-reinforced aluminum-based composite preparation method, combining electromagnetic control technology and ultrasonic dispersion technology, adding TiB 2 reinforced particles in the form of a master alloy (ZrB 2 +Al 2 O 3 ) Nano-particle-reinforced AA6111-based composite material to obtain high-strength, high-modulus ternary nano-particle-reinforced aluminum-based composite with fine grains, uniform particle dispersion, and particle size control at 20 to 80 nanometers material.
  • the preparation method of the in-situ (ZrB 2 +Al 2 O 3 +TiB 2 ) nanoparticle-reinforced AA6111-based composite material of the present invention adopts a two-step reaction method, combined with a low-frequency rotating magnetic field/ultrasonic control technology, and places TiB 2 reinforced particles in the middle
  • the alloy form is added to (ZrB 2 +Al 2 O 3 ) nano-particle reinforced AA6111-based composite material, and the obtained composite material contains three nano-particle reinforcement phases of ZrB 2 , Al 2 O 3 , and TiB 2.
  • Multi-element particle reinforcement has better physical and chemical properties than single-particle aluminum-added composite materials.
  • TiB 2 and ZrB 2 are the metalloid compounds of the hexagonal crystal system. They have good stability, higher melting point, lower coefficient of thermal expansion, higher elastic modulus and high temperature strength, and both Ti and B elements It has a refinement effect on crystal grains.
  • the size of Al 2 O 3 particles is very stable, the hardness is high, and it has good chemical compatibility with the matrix and will not cause interface chemical reactions.
  • the ZrB 2 , Al 2 O 3 , and TiB 2 nanoparticles produced by the invention have stable thermodynamic properties, high melting point, and will not decompose under the action of a high temperature environment.
  • the present invention uses borax (Na 2 B 4 O 7 10H 2 O), potassium fluoroborate (KBF 4 ), potassium fluorozirconate (K 2 ZrF 6 ), and potassium fluorotitanate (K 2 TiF 6 ) as Reaction salt, industrial pure aluminum and AA6111 alloy are the matrix.
  • reaction salt powder is dried at 200 ⁇ 250°C for 2 ⁇ 3h, KBF 4 , K 2 TiF 6 reaction salt is weighed according to the intermediate alloy that produces 5wt.% TiB 2 reinforced particles, K 2 ZrF 6 and borax (Na 2 B 4 O 7 ⁇ 10H 2 O) reaction salt is generated according to the final in-situ (ZrB 2 + Al 2 O 3 + TiB 2 ) nanoparticle-reinforced AA6111-based composite material (ZrB 2 + Al 2 O 3 ) volume fraction of 1 -3% is weighed and mixed evenly, wrapped in aluminum foil for later use.
  • TiB 2 reinforced particle master alloy (2) Preparation of TiB 2 reinforced particle master alloy: Put the weighed industrial pure aluminum ingot into a preheated crucible to melt, heat up to 830 ⁇ 870°C, and mix the weighed KBF 4 and K 2 TiF 6 The reaction salt powder is added to the aluminum melt; after the reaction salt is completely added, the acousto-magnetic coupling field is turned on. After reacting at 850°C for 30 minutes, the solution is cooled to 730 ⁇ 750°C for scouring and slagging, and then casting with a copper mold. The wedge-shaped ingot after casting is the TiB 2 reinforced particle master alloy for use.
  • the proportion of TiB 2 particles is 5% (mass fraction), and the remaining element is Al.
  • step (3) the sound field magnetic coupling parameters consistent with the step (2), the amount of the alloy in accordance with the intermediate TiB 2 TiB 2 occupied (ZrB 2 + Al 2 O 3 + TiB 2) nanoparticles weight of the composite reinforced AA6111 1 ⁇ 3wt.% of it is weighed.
  • the obtained composite material is subjected to T6 heat treatment, including solution treatment and aging treatment: the solution treatment temperature is set to rise from room temperature to 545 ⁇ 550°C, hold for 2.5 ⁇ 3h, and then quench treatment in a water bath at a temperature not exceeding 30°C. The quenching transfer time is less than 10s; the aging treatment temperature is set to rise from room temperature to 160 ⁇ 180°C, keep it for 6 ⁇ 8h and then cool down with the furnace.
  • the parameters of the acousto-magnetic coupling field are that the excitation current is 200-250A, the magnetic field frequency is 15-20Hz, the ultrasonic power is 1.5-2Kw, and the ultrasonic frequency is 20-30KHz.
  • the invention provides a method for preparing an in-situ (ZrB 2 +Al 2 O 3 +TiB 2 ) ternary nano-particle reinforced aluminum-based composite material, which belongs to the technical field of aluminum-based composite material preparation.
  • the method adopts a two-step melt reaction method, combined with low-frequency rotating magnetic field/ultrasonic field control technology, and adopts nano-reinforced particle master alloy remelting to prepare aluminum-based composite materials.
  • the invention mainly has the following advantages:
  • TiB 2 reinforced particles are added to the (ZrB 2 +Al 2 O 3 ) nanoparticle reinforced AA6111-based composite material in the form of a master alloy, which avoids the by-products caused by the addition of too many kinds of reaction mixed salts in the reaction system. It overcomes the problems of side reactions caused by excessive addition of reactive salt species, difficult control of the reaction process, large amount of reactive salt added and long reaction time, which increase the burning loss of molten aluminum.
  • the acousto-magnetic coupling external field has the advantages of a magnetic field and an ultrasonic field. Under the effects of acoustic cavitation, acoustic current, and rotating magnetic field stirring of the ultrasonic field, the crystal grains in the matrix structure become smaller and rounder, and the particles are strengthened. The distribution in the matrix is more uniform and the size is smaller. Under the combined action of the magnetic field and the ultrasonic field, the size, morphology and distribution of the nanoparticles have been improved.
  • Figure 1 is a matrix (a) and 1 vol% ZrB 2 +1 vol% Al 2 O 3 +1 wt% TiB 2 (b) OM diagram.
  • Figure 2 is an SEM image of the morphology of 2vol.% ZrB 2 + 2vol.% Al 2 O 3 + 2wt.% TiB 2 ternary nanoparticles obtained in the present invention.
  • Figure 3 is an SEM image of the morphology of 2vol.% ZrB 2 + 2vol.% Al 2 O 3 binary nanoparticles prepared by in-situ reaction technology.
  • Fig. 4 is a diagram of ternary particles of 1 vol.% ZrB 2 +1 vol.% Al 2 O 3 +1 wt.% TiB 2 prepared by the present invention.
  • a two-step melt reaction method is used.
  • an aluminum-based composite material with 5wt.% TiB 2 reinforced particles is prepared, using K 2 BF 6 and K 2 TiF 6 powders as reactants, and the reactants are dried in a drying box to remove crystal water, and the drying temperature is 200 °C, the drying time is 120min.
  • the composition is designed according to the mass fraction of nano-TiB 2 particles at 5%. Weigh 254.91 g of dried potassium fluoroborate and 246.10 g of potassium fluorotitanate, mix them uniformly and wrap them with aluminum foil for later use.
  • the weighed 886.25g industrial pure aluminum is heated to 850°C in a high-frequency induction heating furnace, and the mixed reaction salt is pressed into the melt with a graphite bell to react, and the acousto-magnetic coupling field is opened at the same time, where the excitation current is 200A, the magnetic field frequency is 15Hz, the ultrasonic power is 1.8Kw, the ultrasonic frequency is 20KHz, after the heat preservation reaction for 30 minutes, the melt is cooled to 750°C for scouring, slagging, and casting at 720°C.
  • the wedge-shaped ingot after casting is TiB 2 Reinforced grain master alloy.
  • the second step is to prepare (ZrB 2 +Al 2 O 3 ) nanoparticle-reinforced AA6111-based composites: the composition is designed according to the volume fraction of nanoparticles (ZrB 2 +Al 2 O 3 ) of 1%. Weigh 1328.64 g of AA6111 aluminum alloy, 48.77 g of borax (Na 2 B 4 O 7 ⁇ 10H 2 O), and 113.88 g of potassium fluorozirconate (K 2 ZrF 6 ).
  • the obtained composite material ingot is processed into standard tensile specimens, and then the tensile specimens are subjected to T6 heat treatment.
  • the solution treatment temperature was set to rise from room temperature to 550°C and kept for 3 hours, and the aging treatment temperature was set to rise from room temperature to 160°C, kept for 8 hours and then cooled with the furnace.
  • a two-step melt reaction method is used.
  • an aluminum-based composite material with 5 wt.% TiB 2 reinforced particles is prepared, and the composition is designed according to the mass fraction of nano-TiB 2 particles at 5%.
  • the composite material is used as a nanoparticle master alloy.
  • the second step is to prepare (ZrB 2 +Al 2 O 3 ) nanoparticle-reinforced AA6111-based composite materials: the composition design is carried out according to the volume fraction of nanoparticles (ZrB 2 +Al 2 O 3) of 2%.
  • Magnetic coupling field after 15 minutes of reaction, refining and slagging; cooling to 750°C, add the pre-weighed (487.46) TiB 2 master alloy to the melt and turn on the acousto-magnetic coupling field at the same time, keep it for 15 minutes. Refining, slagging, and casting at 720°C to obtain 2vol% ZrB 2 + 2vol% Al 2 O 3 + 2wt% TiB 2 nano-particle reinforced aluminum-based composite material.
  • the obtained composite material ingot is processed into standard tensile specimens, and then the tensile specimens are subjected to T6 heat treatment.
  • the solution treatment temperature was set to rise from room temperature to 550°C and kept for 3 hours, and the aging treatment temperature was set to rise from room temperature to 160°C, kept for 8 hours and then cooled with the furnace.
  • the ternary particle-reinforced aluminum-based composite material prepared by the present invention has a higher particle yield than binary particles.
  • the TiB 2 particles are added in the form of intermediate alloys, making the particles and the matrix
  • the interface bonding strength is high, the surface of the material is clean, and the strength and plasticity of the composite material are significantly improved.
  • the test results of the mechanical properties at room temperature show that the tensile strength and elongation of the composite material prepared by the method of the present invention are 368.41 MPa and 24.6%, respectively.
  • a two-step melt reaction method is used.
  • an aluminum-based composite material with 5 wt.% TiB 2 reinforced particles is prepared, and the composition is designed according to the mass fraction of nano-TiB 2 particles at 5%.
  • the composite material is used as a nanoparticle master alloy.
  • the second step is to prepare (ZrB 2 +Al 2 O 3 ) nanoparticle-reinforced AA6111-based composite material: the composition design is carried out according to the volume fraction of nanoparticles (ZrB 2 +Al 2 O 3) of 3%.
  • Magnetic coupling field after 15 minutes of reaction, refining and slagging; cooling to 750°C, add the pre-weighed (541.84) nano TiB 2 master alloy to the melt and turn on the acousto-magnetic coupling field at the same time. After 15 minutes of heat preservation Refining, slagging off, and casting at 720°C to obtain 3vol.% ZrB 2 + 3vol.% Al 2 O 3 + 2wt.% TiB 2 nano-particle reinforced aluminum-based composite material.
  • the obtained composite material ingot is processed into standard tensile specimens, and then the tensile specimens are subjected to T6 heat treatment.
  • the solution treatment temperature was set to rise from room temperature to 550°C and kept for 3 hours, and the aging treatment temperature was set to rise from room temperature to 160°C, kept for 8 hours and then cooled with the furnace.
  • the tensile performance is tested in accordance with ASTM E8M-09 test standard, the tensile rate is 1mm/min, and the test is performed at room temperature.
  • the test results of the mechanical properties at room temperature show that the tensile strength and elongation of the composite material prepared by the method of the present invention are 352.84 MPa and 21.3%, respectively.

Abstract

一种原位三元纳米颗粒增强铝基复合材料的制备方法。该方法采用原位反应生成技术，以含有生成增强颗粒形成元素的粉剂作为反应物，结合低频旋转磁场/超声场调控技术，采用纳米颗粒中间合金重熔制备铝基复合材料。三元纳米颗粒增强AA6016基复合材料，其颗粒平均粒度为65nm，比较单元和双相纳米颗粒有明显细化现象。室温力学性能测试表明，三元纳米颗粒增强AA6016基复合材料，与基体铝合金相比，抗拉强度提高了27.46％-33.5％，延伸率提高了23.56％-30.89％，在航空、航天、尖端武器、汽车工业、精密仪器等领域以及其他民用工业存在很大的应用潜力。

Description

一种原位三元纳米颗粒增强铝基复合材料的制备方法 技术领域
本发明提供一种原位三元纳米颗粒增强铝基复合材料的制备方法，属于铝基复合材料制备技术领域。
背景技术
近年来，随着环境污染、能源缺乏问题日益凸显和汽车轻量化制造的需求的增加，航空航天、轨道交通、新能源汽车等高技术领域对原位铝基复合材料的需求潜力巨大，且对其综合性能的要求也越来越高。因此进一步提高原位铝基复合材料的综合力学性能和成形加工性能，已成为目前亟待解决的问题。
原位颗粒增强铝基复合材料，是通过将含有增强相颗粒形成元素的固体粉末反应盐在某一温度下加入熔融的铝合金表面，然后搅拌使其充分进行，从而在铝熔体中生成增强颗粒。原位复合材料与传统合成制备技术制备的材料相比具有以下特点：(1)增强体颗粒是从基体中原位形核长大的热力学稳定相，因此，在高温下作用时，增强相颗粒不会发生分解或者转化为其它化合物。(2)通过合理选择化合物的类型、成分，可以有效的控制原位生成增强体的种类、大小和数量。(3)原位内生颗粒与基体界面结合良好，相比外加颗粒尺寸更加细小，并且容易实现在铝基体中均匀分布，从而使得原位铝基复合材料弹性模量、抗拉强度得到明显提升。但是，目前这类技术还不够完善，主要表现在以下方面：(1)反应体系少，大多集中在Al-Ti-x(Al-Ti-O、Al-Ti-B)系，且体系的反应温度较高，不仅反应合成的增强相形貌难以控制，而且也会严重恶化铝液。(2)纳米颗粒尺寸小，比表面积效应十分明显，导致颗粒与颗粒之间更容易团聚，在铝熔体中难以分散。(3)颗粒与基体的润湿性差，二元纳米颗粒收得率低。
对现有技术文献和综述文献调研表明，原位双相纳米颗粒取得了一些进展，如中国专利201811286812.1本发明通过Zr和H 3BO 3体系，采用熔体直接反应技术并结合电磁调控技术制备了ZrB 2和Al 2O 3双相纳米增强颗粒,解决了颗粒分布不均匀的问题，形成了分布均匀且尺寸为50-100nm的方形ZrB2颗粒和圆形Al 2O 3颗粒，复合材料经过T6热处理后，强度提高了23.4％，伸长率提高了62％，抗冲击性能提高了38％。中国专利201811286813.6以硼砂(Na 2B 4O 7)和氟锆酸钾(K 2ZrF 6)粉末作为混合反应盐制备ZrB 2和Al 2O 3双相纳米增强颗粒，采用机械 搅拌调控其铝合金熔炼过程并加入稀土中间合金，细化基体晶粒，利用声磁耦合调控复合材料的原位反应过程，以及在凝固过程中施加超声振动，使得二元纳米颗粒尺寸更小，分布更加均匀，使得复合材料的强度和韧性都得到了明显提升。目前通过原位反应技术制备出的纳米颗粒增强相主要集中在单元，但鲜有相关文献报道原位熔体反应制备多元纳米颗粒增强铝基复合材料，所以急需开发一种新型的反应体系和方法来解决多元纳米颗粒反应制备和颗粒收得率低的问题。
发明内容
本发明的目的在于克服现有技术不足，提供一种原位三元纳米颗粒增强铝基复合材料的制备方法，结合电磁调控技术和超声分散技术，把TiB 2增强颗粒以中间合金的形式加入到(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料，获得晶粒细小，颗粒分散均匀且颗粒尺寸控制在20～80纳米的高强度、高模量的三元纳米颗粒增强铝基复合材料。
本发明的原位(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料的制备方法，采用两步反应法，结合低频旋转磁场/超声调控技术，把TiB 2增强颗粒以中间合金的形式加入到(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料，所得到的复合材料中包含了ZrB 2、Al 2O 3、TiB 2三种纳米颗粒增强相。多元颗粒增强相比单一颗粒增铝基复合材料具有更好的物理及化学特性。多元颗粒间相互作用可以有效的改善颗粒与基体间的润湿性，提高了颗粒与基体间的界面结合强度，显著改善了复合材料的组织和性能。TiB 2与ZrB 2两种颗粒作为六方晶系的准金属化合物，具有良好的稳定性，较高的熔点，较低的热膨胀系数，较高的弹性模量和高温强度，并且Ti和B元素都对晶粒有着细化作用。Al 2O 3颗粒的尺寸非常稳定，硬度高，与基体有着良好的化学相容性不会发生界面化学反应。本发明所生成的ZrB 2、Al 2O 3、TiB 2纳米颗粒热力学性能稳定、熔点高，在高温环境作用下不会发生分解。
本发明采用的技术方案具体步骤如下：
(1)本发明以硼砂(Na 2B 4O 7·10H 2O)、氟硼酸钾(KBF 4)、氟锆酸钾(K 2ZrF 6)、氟钛酸钾(K 2TiF 6)为反应盐，工业纯铝和AA6111合金为基体。首先将反应盐粉末在200～250℃烘干2～3h，KBF 4、K 2TiF 6反应盐按生成5wt.％TiB 2增强颗粒的中间合金称量，K 2ZrF 6和硼砂(Na 2B 4O 7·10H 2O)反应盐按照生成最终得到的原位(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料中(ZrB 2+Al 2O 3)体积分数的 1-3％称量并混合均匀，用铝箔包裹待用。
(2)制备TiB 2增强颗粒中间合金：将称量好的工业纯铝锭放入预热的坩埚中进行融化，升温至830～870℃，将称量好的KBF 4、K 2TiF 6混合反应盐粉末加到铝熔体中；待反应盐完全加入后开起声磁耦合场，在850℃反应30min后，将溶体冷却至730～750℃精练、扒渣，然后用铜模进行浇铸，浇铸后的楔形铸锭即为TiB 2增强颗粒中间合金，以备用。
所述步骤(2)中，浇铸所得的TiB 2增强颗粒中间合金中，TiB 2颗粒所占的比重是5％(质量分数)，剩余的元素为Al。
(3)制备(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料：将称量好的AA6111铝合金放入到预热的石墨坩埚中融化，升温至830～870℃，将称量好的氟锆酸钾和硼砂加入到AA6111合金熔体中，完全加入反应盐粉末后开启声磁耦合场，在850℃反应15min后，进行精炼、扒渣；等温度冷却到750℃，把预先称量好的TiB 2中间合金加入到熔体中，待TiB 2中间合金完全融化后开启声磁耦合场，保温15～20min后进行精炼、扒渣，然后用铜模进行浇铸，从而获得(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料。
所述步骤(3)中，声磁耦合场参数与步骤(2)中一致，TiB 2中间合金量按照TiB 2所占(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111复合材料重量的1～3wt.％称取。
将得到的复合材料进行T6热处理，包括固溶和时效处理：固溶处理温度设定为自室温升至545～550℃，保温2.5～3h，随后在温度不超过30℃的水浴中淬火处理，淬火转移时间小于10s；时效处理温度制定为自室温升至160～180℃，保温6～8h后随炉冷却。
所述的声磁耦合场的参数是励磁电流为200～250A，磁场频率为15～20Hz，超声功率为1.5～2Kw，超声频率为20～30KHz。
本发明提供一种原位(ZrB 2+Al 2O 3+TiB 2)三元纳米颗粒增强铝基复合材料的制备方法，属于铝基复合材料制备技术领域。该方法采用两步熔体反应法，结合低频旋转磁场/超声场调控技术，采用纳米增强颗粒中间合金重熔制备铝基复合材料。该发明主要有以下优点：
(1)利用原位反应技术制备三元纳米颗粒(ZrB 2+Al 2O 3+TiB 2)增强铝基复合材料，颗粒与基体界面结合良好、界面清洁无污染、无界面反应产生，克服 传统外加法带来的颗粒与基体润湿性差，界面反应等问题。
(2)TiB 2增强颗粒以中间合金的形式加入到(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料，避免了本反应体系因加入反应混合盐种类过多而产生的副产物，克服了因反应盐种类加入过多而产生的副反应，反应过程难以控制、反应盐加入量多和反应时间长而加大对铝液的烧损等问题。
(3)声磁耦合外场具有磁场和超声场的优点，在超声场的声空化、声流，以及旋转磁场搅拌的作用下，基体组织中晶粒变得更加细小而圆顿，增强颗粒在基体中的分布更加均匀、尺寸更加细小。在磁场和超声场的共同作用下，纳米颗粒的尺寸、形貌以及分布状态均得到了改善。
(4)利用原位反应技术制备的ZrB 2、Al 2O 3和TiB 2颗粒增强相，其颗粒大小、分布和数量均是可控的。
附图说明
为了更清楚地说明本发明的技术方案，下面将对所需要使用的附图做简单地介绍,显而易见地，下面描述中的附图是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为基体(a)和1vol％ZrB 2+1vol％Al 2O 3+1wt％TiB 2(b)OM图。
图2为本发明得到的2vol.％ZrB 2+2vol.％Al 2O 3+2wt.％TiB 2三元纳米颗粒的形貌SEM图。
图3为采用原位反应技术制备的2vol.％ZrB 2+2vol.％Al 2O 3双元纳米颗粒的形貌SEM图。
图4为本发明制备的1vol.％ZrB 2+1vol.％Al 2O 3+1wt.％TiB 2三元颗粒图。
具体实施方式
本发明可以根据以下示例实施，但不限于以下实例在本发明中所使用的术语，除非有另外的说明，一般具有本领域普通技术人员通常理解的含义应理解，这些实例只是为了举例说明本发明，而非以任何方式限制本发明的范围在以下的实施例中，未详细描述的各种过程和方法是本领域中公知的常规方法。
实施例1
制备1vol.％ZrB 2+1vol.％Al 2O 3+1wt.％TiB 2纳米颗粒增强铝基复合材料
采用两步熔体反应法。第一步制备5wt.％TiB 2增强颗粒的铝基复合材料， 使用K 2BF 6和K 2TiF 6粉剂作为反应物，将反应物在干燥箱中烘干去除结晶水，烘干温度为200℃，烘干时间为120min。然后按照纳米TiB 2颗粒质量分数5％进行成分设计。称取烘干后的氟硼酸钾254.91g，氟钛酸钾246.10g混合均匀并用铝箔包裹待用。把称取的886.25g的工业纯铝在高频感应加热炉中加热到850℃，用石墨钟罩将混合反应盐压入熔体中进行反应，同时开起声磁耦合场，其中励磁电流为200A，磁场频率为15Hz，超声功率为1.8Kw，超声频率为20KHz，保温反应30min后，将熔体冷却至750℃精练、扒渣，720℃进行浇铸，浇铸后的楔形铸锭即为TiB 2增强颗粒中间合金。第二步制备制备(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料：按照纳米颗粒(ZrB 2+Al 2O 3)体积分数为1％进行成分设计。称量AA6111铝合金1328.64g，硼砂(Na 2B 4O 7·10H 2O)48.77g，氟锆酸钾(K 2ZrF 6)113.88g。把称取的AA6111铝合金在高频感应加热炉中加热到850℃融化，将称量好的K 2ZrF 6和硼砂少量多批次加入到铝熔体中，完全加入反应盐粉末后开启声磁耦合场，反应15min后，进行精炼、扒渣；等温度冷却到750℃，把预先称量好的(245.6g)TiB 2中间合金加入到熔体中同时开启声磁耦合场，保温15min后进行精炼、扒渣，720℃进行浇铸，从而获得1vol.％ZrB 2+1vol.％Al 2O 3+1wt.％TiB 2纳米颗粒增强铝基复合材料。
将得到的复合材料铸锭加工成标准拉伸试样，然后对拉伸试样进行T6热处理。固溶处理温度设定为自室温升至550℃，保温3h，时效处理温度制定为自室温升至160℃，保温8h后随炉冷却。
从图1和图4可以看出，与基体晶粒相比，复合材料的晶粒组织得到了细化，晶粒组织的尺寸相对均匀，颗粒尺寸细小且分布均匀，没有发现明显的颗粒团簇现象，从而提高了材料的强度和塑性。室温力学性能测试结果表明，采用本发明方法制备的复合材料的抗拉强度和延伸率分别为343.6MPa和22.87％。
实施例2
制备2vol.％ZrB 2+2vol.％Al 2O 3+2wt.％TiB 2纳米颗粒增强铝基复合材料
采用两步熔体反应法。第一步制备5wt.％TiB 2增强颗粒的铝基复合材料，按照纳米TiB 2颗粒质量分数5％进行成分设计。将该复合材料用作纳米颗粒中间合金。第二步制备制备(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料：按照纳米颗粒(ZrB 2+Al 2O 3)体积分数为2％进行成分设计。称量AA6111铝合金1218.64g，硼砂(Na 2B 4O 7·10H 2O)96.31g，氟锆酸钾(K 2ZrF 6)224.89g。把称取的AA6111 铝合金在高频感应加热炉中加热到850℃融化，将称量好的K 2ZrF 6和硼砂少量多批次加入到铝熔体中，完全加入反应盐粉末后开启声磁耦合场，反应15min后，进行精炼、扒渣；等温度冷却到750℃，把预先称量好的(487.46)TiB 2中间合金加入到熔体中同时开启声磁耦合场，保温15min后进行精炼、扒渣，720℃进行浇铸，从而获得2vol％ZrB 2+2vol％Al 2O 3+2wt％TiB 2纳米颗粒增强铝基复合材料。
将得到的复合材料铸锭加工成标准拉伸试样，然后对拉伸试样进行T6热处理。固溶处理温度设定为自室温升至550℃，保温3h，时效处理温度制定为自室温升至160℃，保温8h后随炉冷却。
结合图2和图3可以看出，本发明制备的三元颗粒增强铝基复合材料与双元颗粒相比，颗粒收得率高，由于TiB 2颗粒以中间合金的形式加入，使得颗粒与基体界面结合强度高，材料表面清洁，复合材料的强度和塑性明显得到提升。室温力学性能测试结果表明，采用本发明方法制备的复合材料的抗拉强度和延伸率分别为368.41MPa和24.6％。
实施例3
制备3vol％ZrB 2+3vol％Al 2O 3+2wt％TiB 2纳米颗粒增强铝基复合材料
采用两步熔体反应法。第一步制备5wt.％TiB 2增强颗粒的铝基复合材料，按照纳米TiB 2颗粒质量分数5％进行成分设计。将该复合材料用作纳米颗粒中间合金。第二步制备制备(ZrB 2+Al 2O 3)纳米颗粒增强AA6111基复合材料：按照纳米颗粒(ZrB 2+Al 2O 3)体积分数为3％进行成分设计。称量AA6111铝合金1354.62g，硼砂(Na 2B 4O 7·10H 2O)159.87g，氟锆酸钾(K 2ZrF 6)373.30g。把称取的AA6111铝合金在高频感应加热炉中加热到850℃融化，将称量好的K 2ZrF 6和硼砂少量多批次加入到铝熔体中，完全加入反应盐粉末后开启声磁耦合场，反应15min后，进行精炼、扒渣；等温度冷却到750℃，把预先称量好的(541.84)纳米TiB 2中间合金加入到熔体中同时开启声磁耦合场，保温15min后进行精炼、扒渣，720℃进行浇铸，从而获得3vol.％ZrB 2+3vol.％Al 2O 3+2wt.％TiB 2纳米颗粒增强铝基复合材料。
将得到的复合材料铸锭加工成标准拉伸试样，然后对拉伸试样进行T6热处理。固溶处理温度设定为自室温升至550℃，保温3h，时效处理温度制定为自室温升至160℃，保温8h后随炉冷却。
拉伸性能按照ASTM E8M-09实验标准测试，拉伸速率为1mm/min，室 温下测试。室温力学性能测试结果表明，采用本发明方法制备的复合材料的抗拉强度和延伸率分别为352.84MPa和21.3％。

Claims (7)

  1. 一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，采用两步法制备三元纳米颗粒增强铝基复合材料，第一步:首先将含有TiB 2增强颗粒形成元素的反应混合盐加入到熔融态的纯铝熔体中，同时施加声磁耦合场，制备出含有TiB 2增强颗粒的铝基复合材料，该复合材料用作增强颗粒中间合金；第二步：按照所需要不同体积分数的增强颗粒(ZrB 2+Al 2O 3)把称量好的反应混合盐加入到AA6111溶体中，反应过程中施加声磁耦合场，反应结束后加入TiB 2纳米颗粒中间合金，经保温静置、精练、打渣、浇铸制得AA6111基复合材料铸锭，最后对铸锭进行T6热处理获得三元(ZrB 2+Al 2O 3+TiB 2)高强度、高模量纳米颗粒增强铝基复合材料。
  2. 如权利要求1所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，具体步骤为：
    (1)以硼砂、氟硼酸钾、氟锆酸钾、氟钛酸钾为反应盐，工业纯铝和AA6111合金为基体；首先将反应盐粉末烘干，KBF 4、K 2TiF 6反应盐按生成5wt.％TiB 2增强颗粒的中间合金称量，K 2ZrF 6和硼砂反应盐按照生成最终得到的原位(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料中(ZrB 2+Al 2O 3)体积分数的1-3％称量并混合均匀，用铝箔包裹待用；
    (2)制备TiB 2增强颗粒中间合金：将称量好的工业纯铝锭放入预热的坩埚中进行融化，升温至830～870℃，将称量好的KBF 4、K 2TiF 6混合反应盐粉末加到铝熔体中；待反应盐完全加入后开起声磁耦合场，在850℃反应30min后，将溶体冷却至730～750℃精练、扒渣，然后用铜模进行浇铸，浇铸后的楔形铸锭即为TiB 2增强颗粒中间合金，以备用；
    (3)制备(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料：将称量好的AA6111铝合金放入到预热的石墨坩埚中融化，升温至830～870℃，将称量好的氟锆酸钾和硼砂加入到AA6111合金熔体中，完全加入反应盐粉末后开启声磁耦合场，在850℃反应15min后，进行精炼、扒渣；等温度冷却到750℃，把预先称量好的TiB 2中间合金加入到熔体中，待TiB 2中间合金完全融化后开启声磁耦合场，保温15～20min后进行精炼、扒渣，然后用铜模进行浇铸，从而获得(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111基复合材料；
    (4)将得到的复合材料进行T6热处理，包括固溶和时效处理。
  3. 如权利要求2所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，步骤(1)中，反应盐粉末烘干温度为200～250℃，烘干时间为2～3h。
  4. 如权利要求2所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，步骤(2)中，浇铸所得的TiB 2增强颗粒中间合金中，TiB 2颗粒所占的比重是5wt％，剩余的元素为Al。
  5. 如权利要求2所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，步骤(3)中，声磁耦合场参数与步骤(2)中一致，TiB 2中间合金量按照TiB 2所占(ZrB 2+Al 2O 3+TiB 2)纳米颗粒增强AA6111复合材料重量的1～3wt.％称取。
  6. 如权利要求2所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，步骤(4)中，固溶处理温度设定为自室温升至545～550℃，保温2.5～3h，随后在温度不超过30℃的水浴中淬火处理，淬火转移时间小于10s；时效处理温度制定为自室温升至160～180℃，保温6～8h后随炉冷却。
  7. 如权利要求2所述的一种原位三元纳米颗粒增强铝基复合材料的制备方法，其特征在于，所述的声磁耦合场的参数是励磁电流为200～250A，磁场频率为15～20Hz，超声功率为1.5～2Kw，超声频率为20～30KHz。
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