WO2010051675A1 - A method of synthesizing metal-based composite material by melt reaction in coupling magnetic field and ultrasonic field - Google Patents

A method of synthesizing metal-based composite material by melt reaction in coupling magnetic field and ultrasonic field Download PDF

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Publication number
WO2010051675A1
WO2010051675A1 PCT/CN2009/000252 CN2009000252W WO2010051675A1 WO 2010051675 A1 WO2010051675 A1 WO 2010051675A1 CN 2009000252 W CN2009000252 W CN 2009000252W WO 2010051675 A1 WO2010051675 A1 WO 2010051675A1
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magnetic field
ultrasonic
field
melt
reaction
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PCT/CN2009/000252
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French (fr)
Chinese (zh)
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赵玉涛
陈刚
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江苏大学
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Priority to US13/126,510 priority Critical patent/US20110247778A1/en
Publication of WO2010051675A1 publication Critical patent/WO2010051675A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/10—Supplying or treating molten metal
    • B22D11/11—Treating the molten metal
    • B22D11/114—Treating the molten metal by using agitating or vibrating means
    • B22D11/115—Treating the molten metal by using agitating or vibrating means by using magnetic fields
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/02—Use of electric or magnetic effects

Definitions

  • the invention relates to the technical field of novel composite material synthesis preparation, in particular to a novel method for preparing a particle reinforced metal matrix composite material by in-situ reaction of a melt under the coupling of an electromagnetic field and an ultrasonic field. Background technique
  • Particle-reinforced metal matrix composites have good mechanical properties and physical and chemical properties due to their composite structural features. They have broad application prospects in advanced electrical and electronic devices, aerospace, machinery, bridge and tunnel engineering, etc.
  • the in-situ reaction synthesis method is currently the main method for preparing particle-reinforced metal matrix composites.
  • the principle of the method is to add an alloying element or compound capable of forming a second phase to the molten metal of the metal matrix, which occurs at a certain temperature with the molten metal.
  • the in-situ reaction produces a particulate phase to produce an endogenous particle reinforced composite.
  • the composite material prepared by the method has the interface of the particle phase in situ, and the interface with the matrix metal is clean, the wettability is good, and the bonding strength is ⁇ .
  • this technology still has a series of problems, the reaction process is difficult to control, the particles are easy to grow, even agglomerate, and the distribution is not uniform.
  • Electromagnetic parameter range of low-frequency alternating magnetic field frequency: 0.1Hz ⁇ 60Hz, working current: 1A ⁇ 10000A, adjust electromagnetic parameters according to melt amount, type and stirring intensity.
  • higher frequency can be used.
  • iron-based, nickel-based, and zinc-based melts lower frequencies are used.
  • the specific steps are as follows: After the metal-based melt is refined, it is adjusted to the reaction starting temperature, and a reactant powder which can react with the metal melt in situ to form a particulate phase is added, and after the magnetic field is stirred and stabilized, the ultrasonic horn is inserted into the liquid surface. ⁇ 6mm, turn on the ultrasonic device, the ultrasonic treatment time is 60s ⁇ 600s. After the time is up, stop the ultrasonic equipment, turn off the magnetic field, and let it stand after the pouring temperature.
  • the low-frequency alternating magnetic field can also adopt the rotating stirring magnetic field or the traveling wave stirring magnetic field in the above parameter range, the rotating stirring magnetic field is applied to the side of the molten pool, or the traveling wave magnetic field is applied to the bottom of the molten pool, which is proposed by the present invention. Program.
  • This method can be used for small batch production as well as for large scale industrial applications.
  • the composite material is synthesized under the coupling of magnetic field and ultrasonic field, and the magnetic field and the ultrasonic field are coupled to make the particle size finer and evenly dispersed;
  • Figure 1 is a schematic illustration of the apparatus used in the method of the present invention.
  • Figure 2 is a schematic illustration of the second apparatus used in the method of the present invention.
  • Figure 3 is a schematic diagram of an embodiment apparatus.
  • Example 4 is a photograph showing the microstructure of an (Al 3 Zr( s )+ Z r B 2 ( s )) particle-reinforced A1 matrix composite prepared by the combination of a strong pulsed magnetic field and an ultrasonic field in Example 1.
  • Fig. 5 is a photograph showing the microstructure of the (Al 3 Zr( s ) + Z r B 2(s )) particle-reinforced A1 matrix composite prepared by the high-frequency oscillating magnetic field and the ultrasonic field coupling of Example 2.
  • FIG. 6 is a photograph showing the microstructure of the (Al 3 Zr( s ) + A1 2 0 3(S) ) particle-reinforced A1 matrix composite prepared by the low-frequency stirring magnetic field and the ultrasonic field coupling of Example 3.
  • 1 insulation refractory bath or crucible 2 composite melt; 3 ultrasonic horn; 4 magnetic field; 5 spray gun.
  • the ultrasonic field is concentrated in the central region of the melt and the edge region of the melt is weak.
  • the present invention proposes a new method for synthesizing particle-reinforced metal matrix composites by in-situ coupling of an electromagnetic field and an ultrasonic field. Summary of the invention
  • the object of the present invention is to provide a novel method for preparing an endogenous particle-reinforced metal matrix composite by melt reaction under the coupling of an electromagnetic field and an ultrasonic field, and preparing a high performance in-situ particle reinforced metal matrix composite.
  • the basic principle of the invention is to simultaneously apply a magnetic field and a high-energy ultrasonic field in the reaction synthesis process of the in-situ particle-reinforced metal matrix composite material, and use the magnetic field to generate electromagnetic force, magnetization and eddy current induction heat, and other high-energy ultrasonic fields.
  • the sonochemical principles such as acoustic cavitation and acoustic flow impact generated in the melt couple the synthetic synthesis process to achieve the control of particle phase distribution, inhibit particle growth and clusters, and change the thermodynamics and dynamics of in-situ synthesis reactions.
  • the purpose of the learning conditions is to realize the synthesis of particle-reinforced metal matrix composites under the sonochemical coupling of magnetic field magnetization and high-energy ultrasonic fields.
  • the principle of the new method is combined with the schematic diagram of the device for implementing the solution in FIG. 1 as follows:
  • the composite melt 2 is synthesized in a molten pool (or crucible) 1 made of a heat-insulating refractory material, and a high-energy ultrasonic horn 3 is inserted in the upper part of the molten pool (or crucible), and the melt is ultrasonically treated in the molten pool ( Or ⁇ ) Apply magnetic field 4 to the outside.
  • the applied magnetic field 4 can be three kinds of magnetic fields: a strong pulse magnetic field, a high frequency oscillating magnetic field, and a low frequency rotating magnetic field.
  • the applied magnetic field 4 is selected.
  • the strong pulsed magnetic field that is, the strong pulsed magnetic field and the ultrasonic field, the pulsed electromagnetic force, the pulsed magnetizing force and the induced current of the intense pulsed magnetic field in the melt are all in situ chemistry.
  • the reaction has an accelerating effect and can play the purpose of dispersing the particle phase.
  • the pulsed magnetic field has a certain attenuation in the metal melt, and the reaction in the edge region of the melt is strongly influenced by the magnetic field and the center portion is weak, so it is necessary to select and High-energy ultrasonic coupling, power ultrasonic through the cavitation effect in the melt and acoustic flow impact, cavitation effect allows the particle cluster to be controlled, the acoustic flow impact acts as a micro-region agitation, because the ultrasonic field is strong in the central region The edges are weak, and the two just complement each other.
  • the coupling effect accelerates the in-situ reaction, so that the particle phase is rapidly formed and dispersed.
  • the external magnetic field 4 can also be selected with a high-frequency oscillating magnetic field. Due to the skin effect in the melt, the high-frequency oscillating magnetic field concentrates on the edge of the molten pool and forms an oscillating electromagnetic force on the particles in the composite melt. , the particle cluster is controlled, and the ultrasonic field still mainly acts on the central region of the molten pool.
  • the magnetic field 4 can also be selected by using a low-frequency stirring magnetic field and power ultrasonic coupling.
  • the use of strong low-frequency stirring magnetic field and high-energy ultrasonic coupling can also achieve The ideal effect.
  • the principle is as follows: High-energy ultrasound passes the cavitation effect in the melt and the acoustic flow impact, the cavitation effect makes the particle clusters controlled, the acoustic flow impact acts as a micro-region stirring, and the additional low-frequency stirring magnetic field 4 pairs make the whole melting With the electromagnetic stirring of the pool, the ultrasonic treatment effect is more obvious, and the local effect or concentration effect of the ultrasonic treatment is controlled.
  • a method for synthesizing a metal matrix composite by a melt reaction of a magnetic field and an ultrasonic field is: adjusting a metal-based melt to a reaction starting temperature after refining, and adding a reactant powder capable of reacting in situ with the melt to form a particulate phase
  • the synthesis reaction is carried out, and a magnetic field and a high-energy ultrasonic field are applied during the reaction synthesis; after the reaction is completed, the casting is allowed to stand at the pouring temperature.
  • the applied magnetic field may be a strong pulsed magnetic field, a high frequency oscillating magnetic field or a low frequency alternating magnetic field.
  • a strong pulsed magnetic field a high frequency oscillating magnetic field or a low frequency alternating magnetic field.
  • a high frequency oscillating magnetic field or a low frequency alternating magnetic field.
  • a low frequency alternating magnetic field There are also three specific technical solutions for implementing the present invention in terms of different forms of applied magnetic fields.
  • the electromagnetic parameters of the strong pulse magnetic field are: pulse current frequency 0.1 Hz ⁇ 10 Hz, pulse current density lkA / m 2 ⁇ 10 kA / m 2 , charging voltage: lkV ⁇ 20kV, central magnetic field strength 0.5 ⁇ 20T. According to the size of the crucible and the type of melt, the electromagnetic parameters are selected so that the intensity of the pulsed magnetic field in the melt is above 1T, and the effect is obvious.
  • the specific steps are as follows: After the metal-based melt is refined, it is adjusted to the composite temperature, and a reagent capable of reacting with the melt in situ to form a particulate phase is added. After the magnetic field is stabilized, the ultrasonic horn is inserted into the liquid surface 5 to 6 mm, and the ultrasonic wave is turned on. The device, sonication time 60s ⁇ 600s, after the time is up, stop the ultrasonic device, turn off the magnetic field, and wait until the pouring temperature to wrap.
  • the method is particularly suitable for the preparation of composite materials having a small amount of metal matrix composite but requiring extremely high performance.
  • the electromagnetic parameters of the high-frequency oscillating magnetic field are: high-frequency reference wave frequency 10 kHz ⁇ 30 kHz, amplitude-modulated oscillating wave frequency 1 ⁇ 30 ⁇ , power range 0 ⁇ 100 kW, electromagnetic parameters adjusted according to melt amount, type, molten pool and stirring intensity
  • high-frequency reference wave frequency 10 kHz ⁇ 30 kHz
  • amplitude-modulated oscillating wave frequency 1 ⁇ 30 ⁇ power range 0 ⁇ 100 kW
  • a higher reference wave frequency can be used.
  • iron-based, nickel-based, and zinc-based melts a lower reference wave frequency is used.
  • the oscillation wave frequency is determined according to the melt agitation condition, and the reactor
  • the structure is related to the type of molten metal, and it is preferred that the melt does not exhibit strong turbulence.
  • the specific steps are as follows: After the metal melt is refined, it is adjusted to the reaction starting temperature, and a reactant powder which can react with the metal melt in situ to form a particle phase is added, and after the magnetic field is stabilized, the ultrasonic horn is inserted into the liquid surface. ⁇ 6mm, turn on the ultrasonic device, sonication time 60s ⁇ 600s , after the time is up, stop the ultrasonic equipment, turn off the magnetic field, and wait for the pouring temperature to carry out the pouring.
  • Example 1 Preparation of (Al 3 Zr( s )+ ZrB 2 ( s> ) particle reinforced A1 matrix composite by strong pulsed magnetic field and ultrasonic field coupling
  • Raw materials Base metal: Pure A1; Reaction salt: K 2 ZrF 6 + KBF 4 powder, refined deaerator and slag slag; The preparation process is divided into two steps:
  • 50Kg pure A1 was melted and heated to 900 ° C in a 60 kW resistance furnace to degas and slag.
  • the reagents used are all dried at 250 ° C ⁇ 300 ° C, wherein K 2 ZrF 6 + KBF 4 , ground into fine powder (particle size less than 200 mesh), weighed and coated with aluminum foil, K 2 ZrF 6
  • the +KBF 4 powder was added in an amount of 20% by weight of the metal.
  • the high-frequency magnetic field was continuously applied for 3 min, then the magnetic field power was turned off, the melt was allowed to stand, and the temperature was lowered to 720 Torr and poured into a water-cooled copper mold having a diameter of 200 mm to prepare a composite ingot.
  • the composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, and no solidification structure defects such as looseness and shrinkage, and the particle size is 0.2 ⁇ 0.6 ⁇ (Fig. 3).
  • Example 2 Preparation of Al 3 Zr( s> + ZrB 2 ( s )) particle reinforced A1 matrix composite by high frequency oscillating magnetic field and ultrasonic field coupling
  • Raw materials Base metal: Pure A1; Reaction salt: K 2 ZrF 6 + KBF 4 powder, refined deaerator and slag slag; The preparation process is divided into two steps:
  • 50Kg pure A1 is melted and heated to 900 ° C in a 60kW power frequency melting aluminum furnace, degassing and slag.
  • the reagents used are fully dried at 250 ° C ⁇ 300 ° C, wherein the K 2 ZrF 6 + BF 4 powder is ground into a fine powder (particle size less than 200 mesh), weighed and placed in a spray can, K 2 ZrF 6
  • the +KBF 4 powder was added in an amount of 20% by weight of the metal.
  • the device is shown in Fig. 2.
  • the molten metal which is refined and meets the reaction initiation temperature requirement (900 °C) is poured from the metal refining holding furnace into the insulated composite material molten pool 1, and is blown into the molten pool 1 by using the Ar gas spray gun 5.
  • K 2 ZrF 6 +KBF 4 powder after the powder is sprayed, the high-frequency oscillating magnetic field 4 is turned on, the high-frequency reference wave frequency is 20 kHz, the maximum current is 80 A, and the oscillation wave frequency is 25 Hz.
  • the undulating waveform is a sine wave.
  • the ultrasonic horn 3 is inserted into the molten pool to a depth of about 5 mm, and the ultrasonic device is turned on, the ultrasonic field frequency is 20 kHz, the ultrasonic intensity is 10 kW/m 2 , and the ultrasonic treatment time is 5 min.
  • the high-frequency magnetic field is continuously applied for 3 min, then the magnetic field power supply is turned off, the melt is allowed to stand, and the temperature is lowered to 730 ° C, and the slag is removed, and the round billet of 2 Q0 mm in diameter is semi-continuously cast at 720 ° C.
  • the composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, no looseness, shrinkage and other solidification, and structural defects, and the particle size is l ⁇ 5 m (Fig. 4).
  • Example 3 Preparation of low-amplitude stirring magnetic field and ultrasonic field coupling (Al 3 Zr( s )+ A1 2 0 3(S) ) particle reinforced A1 matrix composite
  • Raw materials base metal: pure A1; solid powder: industrial zirconium carbonate (Zr(C0 3 ) 2 ) powder, refined deaerator and slag slag;
  • the preparation process is divided into two steps:
  • 50Kg pure A1 is melted and heated to 900 ⁇ in a 60kW power frequency melting aluminum furnace, degassing and slag.
  • the reagents used are all dried at 250 °C ⁇ 30 (TC), wherein Zr(C0 3 ) 2 is ground into fine powder (particle size less than 200 mesh), weighed and put into the spray can, Zr(C0 3 ) 2 added The weight is 20% of the weight of the metal.
  • the composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, and no solidification structure defects such as looseness and shrinkage, and the particle size is l ⁇ 5 m (Fig. 5).

Abstract

A method of synthesizing metal-based composite material by melt reaction in coupling magnetic field and ultrasonic field comprises: adjusting metal-base melt to the reaction starting temperature after refining, then adding reactants which generate reinforced particles by in-situ synthesis reaction with melt, keeping the reacted melt stand until it is cooled to casting temperature after the reaction, and casting. Magnetic field and high-energy ultrasonic field are exerted simultaneously during the reaction. The magnetic field can be high-power pulse magnetic field, high-frequency oscillating magnetic field or low-frequency alternating magnetic field. The metal-based composite material produced by the above-mentioned method exhibits that reinforced particles are much finer, more uniformly distributed, and fit with metal matrix better.

Description

一种磁场与超声场耦合作用下熔体反应合成金属基复合材料的方法 技术领域  Method for synthesizing metal matrix composite material by melt reaction under coupling of magnetic field and ultrasonic field
本发明涉及新型复合材料合成制备技术领域， 特别涉及到一种在电磁场和超声场耦合 作用下熔体原位反应合成制备颗粒增强金属基复合材料的新方法。 背景技术  The invention relates to the technical field of novel composite material synthesis preparation, in particular to a novel method for preparing a particle reinforced metal matrix composite material by in-situ reaction of a melt under the coupling of an electromagnetic field and an ultrasonic field. Background technique
颗粒增强金属基复合材料由于具有复合的结构特征而兼备良好的力学性能和理化性能， 在先进的电工电子器件、 航空航天器、 机械、 桥梁隧道工程等领域具有广阔的应用前景， 已成为近年来金属基复合材料的研究热点之一。 原位反应合成法是目前制备颗粒增强金属 基复合材料的主要方法， 该方法的原理是在金属基体熔液中加入能生成第二相的合金元素 或化合物， 在一定温度下与金属熔液发生原位反应生成颗粒相而制得内生颗粒增强复合材 料。 该方法制备复合材料由于颗粒相原位生成， 其与基体金属结合界面干净， 润湿性好， 结合强度髙。 但是， 该技术还存在一系列问题， 反应过程难控制， 颗粒相易长大， 甚至团 聚， 分布也不均匀。  Particle-reinforced metal matrix composites have good mechanical properties and physical and chemical properties due to their composite structural features. They have broad application prospects in advanced electrical and electronic devices, aerospace, machinery, bridge and tunnel engineering, etc. One of the research hotspots of metal matrix composites. The in-situ reaction synthesis method is currently the main method for preparing particle-reinforced metal matrix composites. The principle of the method is to add an alloying element or compound capable of forming a second phase to the molten metal of the metal matrix, which occurs at a certain temperature with the molten metal. The in-situ reaction produces a particulate phase to produce an endogenous particle reinforced composite. The composite material prepared by the method has the interface of the particle phase in situ, and the interface with the matrix metal is clean, the wettability is good, and the bonding strength is 髙. However, this technology still has a series of problems, the reaction process is difficult to control, the particles are easy to grow, even agglomerate, and the distribution is not uniform.
利用外场作用可以改善原位合成反应的热力学与动力学条件，起到促进原位反应进行的 作用， 同时， 外场作用可以控制颗粒相的过分长大或偏聚团簇现象， 因此， 在外场下原位 合成金属基复合材料越来越受到研究者的重视。中国专利： CN 1676641A (公开日：2005.10.5, 发明名称： 制备金属基纳米复合材料的磁化学反应原位合成方法）提出在磁场 （稳恒磁场、 交变磁场和脉冲磁场） 下进行原位磁化学反应合成， 该专利介绍的方法在细化增强颗粒方 面具有非常好的效果。 中国专利： CN 1958816 (公开日： 2007.05.09, 发明名称： 功率超声 法制备内生颗粒增强铝基表面复合材料工艺） 提出利用功率超声制备内生颗粒增强 (Al3Ti 相)铝基表面复合材料， 使增强相在基体的表层分布均匀， 界面结合更好。 The use of the external field can improve the thermodynamic and kinetic conditions of the in-situ synthesis reaction, and promote the in-situ reaction. At the same time, the external field can control the excessive growth or segregation of the particle phase. Therefore, under the external field In-situ synthesis of metal matrix composites has received increasing attention from researchers. Chinese Patent: CN 1676641A (Publication Date: 2005.10.5, Title: In-situ Synthesis of Magnetic Chemical Reactions for Preparation of Metal-Based Nanocomposites) Proposed in situ in magnetic fields (steady magnetic field, alternating magnetic field and pulsed magnetic field) The magnetic chemical reaction synthesis, the method described in this patent has a very good effect in refining the reinforcing particles. Chinese Patent: CN 1958816 (Publication Date: 2007.05.09, Title: Process for Preparation of Endogenous Particle Reinforced Aluminum-Based Surface Composites by Power Ultrasonic Method) Preparation of Endogenous Particle Reinforced (Al 3 Ti Phase) Aluminum Matrix Surface Composite by Power Ultrasound The material makes the reinforcement phase evenly distributed on the surface of the substrate, and the interface is better.
但是，单一施加电磁场或超声场对原位反应合成颗粒增强金属基复合材料的作用仍不能 令人满意。 施加单一电磁场时， 由于电磁场在金属熔体内存在难以克服的集肤效应， 磁场 在金属内的作用强度按指数规律衰减， 因此电磁场对熔体的有效作用深度有限， 特别对于 大体积的熔池或采用较高频率的电磁场时， 熔体内电磁场作用的差异非常明显， 即电磁场 在熔体内作用出现严重的不均匀性， 中心区域电磁场作用微弱而边缘区域电磁场作用很强。 单一施加超声场时， 由于超声波是一种机械疏密震荡波， 属于纵波， 其作用有很显著的方 向性， 同时超声波在金属熔体中的衰减亦十分严重， 因此， 超声效应主要集中在变幅杆下 低频交变磁场的电磁参数范围， 频率： 0.1Hz〜60Hz， 工作电流： 1A〜10000A， 根据熔 体量、 种类和搅拌强度调节电磁参数， 对铝、 铜基熔体， 可采用较高频率， 对铁基、 镍基、. 锌基熔体， 采用较低频率。 However, the effect of a single applied electromagnetic field or ultrasonic field on the in-situ reaction synthesis of particle reinforced metal matrix composites is still unsatisfactory. When a single electromagnetic field is applied, due to the insurmountable skin effect of the electromagnetic field in the metal melt, the strength of the magnetic field in the metal is exponentially attenuated, so the effective depth of the electromagnetic field to the melt is limited, especially for large-volume molten pools. Or when a higher frequency electromagnetic field is used, the difference of the electromagnetic field in the melt is very obvious, that is, the electromagnetic field has a serious non-uniformity in the melt, the electromagnetic field in the central region is weak, and the electromagnetic field in the edge region is very strong. When a single ultrasonic field is applied, since the ultrasonic wave is a mechanically dense shock wave, it belongs to the longitudinal wave, and its action has a very significant directionality. At the same time, the attenuation of the ultrasonic wave in the metal melt is also very serious. Therefore, the ultrasonic effect is mainly concentrated in the change. Under the mast Electromagnetic parameter range of low-frequency alternating magnetic field, frequency: 0.1Hz~60Hz, working current: 1A~10000A, adjust electromagnetic parameters according to melt amount, type and stirring intensity. For aluminum and copper-based melt, higher frequency can be used. For iron-based, nickel-based, and zinc-based melts, lower frequencies are used.
超声场的频率 10kHz〜30kHz， 超声强度 0.5kW/m2〜60 kW/m2。 10kHz~30kHz frequency ultrasound field, the intensity of the ultrasound 0.5kW / m 2 ~60 kW / m 2.
具体步骤为： 金属基熔体精炼后调整到反应起始温度， 加入能与金属熔体原位反应生成 颗粒相的反应物粉剂， 开启磁场搅拌稳定后， 插入超声变幅杆到液面下 5〜6mm， 接通超声 装置， 超声处理时间 60s〜600s， 时间到后， 停止超声设备， 关掉磁场， 静置到浇注温度后 进行浇注。  The specific steps are as follows: After the metal-based melt is refined, it is adjusted to the reaction starting temperature, and a reactant powder which can react with the metal melt in situ to form a particulate phase is added, and after the magnetic field is stirred and stabilized, the ultrasonic horn is inserted into the liquid surface. ~6mm, turn on the ultrasonic device, the ultrasonic treatment time is 60s~600s. After the time is up, stop the ultrasonic equipment, turn off the magnetic field, and let it stand after the pouring temperature.
补充说明： 低频交变磁场也可采用上述参数范围内的旋转搅拌磁场或行波搅拌磁场， 旋 转搅拌磁场施加在熔池的侧面， 或行波磁场施加在熔池的底部， 均属本发明提出的方案。  Supplementary explanation: The low-frequency alternating magnetic field can also adopt the rotating stirring magnetic field or the traveling wave stirring magnetic field in the above parameter range, the rotating stirring magnetic field is applied to the side of the molten pool, or the traveling wave magnetic field is applied to the bottom of the molten pool, which is proposed by the present invention. Program.
该方法即可用于小批量生产， 也可用于大规模工业应用。  This method can be used for small batch production as well as for large scale industrial applications.
与现有技术相比本发明具有的优点是： The present invention has advantages over the prior art in that:
( 1 ) 复合材料在磁场和超声场耦合作用下合成， 磁场和超声场耦合作用使颗粒粒度细 化， 分散均匀；  (1) The composite material is synthesized under the coupling of magnetic field and ultrasonic field, and the magnetic field and the ultrasonic field are coupled to make the particle size finer and evenly dispersed;
(2) 超声波振动搅拌及电磁搅拌作用改善了复合的动力学条件， 且颗粒相与基体金属 界面复合更好；  (2) Ultrasonic vibration stirring and electromagnetic stirring improve the kinetic conditions of the composite, and the particle phase and the matrix metal interface are better composite;
(3 ) 磁化学与声化学共同作用， 改善原位反应的热力学条件， 即加速原位反应速度又 控制颗粒相的长大。 附图说明  (3) Magnetic chemistry and sonochemistry work together to improve the thermodynamic conditions of the in-situ reaction, that is, accelerate the in-situ reaction rate and control the growth of the particle phase. DRAWINGS
图 1 是本发明方法中使用的设备一示意图。  BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a schematic illustration of the apparatus used in the method of the present invention.
图 2是本发明方法中使用的设备二示意图。  Figure 2 is a schematic illustration of the second apparatus used in the method of the present invention.
图 3是实施例设备示意图。  Figure 3 is a schematic diagram of an embodiment apparatus.
图 4是实施例 1强脉冲磁场和超声场耦合作用下制备的（Al3Zr(s)+ ZrB2(s))颗粒增强 A1 基复合材料组织照片。 4 is a photograph showing the microstructure of an (Al 3 Zr( s )+ Z r B 2 ( s )) particle-reinforced A1 matrix composite prepared by the combination of a strong pulsed magnetic field and an ultrasonic field in Example 1.
图 5是实施例 2高频振荡磁场和超声场耦合作用下制备的 （Al3Zr(s)+ ZrB2(s)) 颗粒增强 A1基复合材料组织照片。 Fig. 5 is a photograph showing the microstructure of the (Al 3 Zr( s ) + Z r B 2(s )) particle-reinforced A1 matrix composite prepared by the high-frequency oscillating magnetic field and the ultrasonic field coupling of Example 2.
图 6是实施例 3低频搅拌磁场和超声场耦合作用下制备的（Al3Zr(s)+ A1203(S))颗粒增强 A1基复合材料组织照片。 6 is a photograph showing the microstructure of the (Al 3 Zr( s ) + A1 2 0 3(S) ) particle-reinforced A1 matrix composite prepared by the low-frequency stirring magnetic field and the ultrasonic field coupling of Example 3.
图中， 1 保温耐火材料熔池或坩埚； 2复合材料熔体； 3 超声变幅杆； 4磁场； 5 喷 枪。 的柱状区域范围内， 即超声场作用集中在熔体的中心区域， 熔体的边缘区域则很弱。 In the figure, 1 insulation refractory bath or crucible; 2 composite melt; 3 ultrasonic horn; 4 magnetic field; 5 spray gun. Within the columnar region, the ultrasonic field is concentrated in the central region of the melt and the edge region of the melt is weak.
为弥补单一施加电磁场或超声场的不足，本发明提出采用电磁场与超声场耦合作用下原 位合成颗粒增强金属基复合材料的新方法。 发明内容  In order to compensate for the shortage of a single applied electromagnetic field or ultrasonic field, the present invention proposes a new method for synthesizing particle-reinforced metal matrix composites by in-situ coupling of an electromagnetic field and an ultrasonic field. Summary of the invention
本发明的目的是：提供一种在电磁场与超声场耦合作用下熔体反应合成制备内生颗粒增 强金属基复合材料的新方法， 制备高性能原位颗粒增强金属基复合材料。  SUMMARY OF THE INVENTION The object of the present invention is to provide a novel method for preparing an endogenous particle-reinforced metal matrix composite by melt reaction under the coupling of an electromagnetic field and an ultrasonic field, and preparing a high performance in-situ particle reinforced metal matrix composite.
本发明的基本原理是：在原位颗粒增强金属基复合材料的反应合成过程同时施加磁场和 高能超声场， 利用磁场对熔体产生电磁力、 磁化及涡流感应热等磁化学原理和高能超声场 在熔体内产生的声空化和声流冲击等声化学原理对复合材料合成制备过程进行耦合作用， 达到控制颗粒相的分布、 抑制颗粒长大和团簇并改变原位合成反应的热力学和动力学条件 的目的， 实现磁场磁化学和高能超声场的声化学耦合作用下合成颗粒增强金属基复合材料。 该新方法的原理结合图 1实现本方案的装置示意图说明如下：  The basic principle of the invention is to simultaneously apply a magnetic field and a high-energy ultrasonic field in the reaction synthesis process of the in-situ particle-reinforced metal matrix composite material, and use the magnetic field to generate electromagnetic force, magnetization and eddy current induction heat, and other high-energy ultrasonic fields. The sonochemical principles such as acoustic cavitation and acoustic flow impact generated in the melt couple the synthetic synthesis process to achieve the control of particle phase distribution, inhibit particle growth and clusters, and change the thermodynamics and dynamics of in-situ synthesis reactions. The purpose of the learning conditions is to realize the synthesis of particle-reinforced metal matrix composites under the sonochemical coupling of magnetic field magnetization and high-energy ultrasonic fields. The principle of the new method is combined with the schematic diagram of the device for implementing the solution in FIG. 1 as follows:
在保温耐火材料制成的熔池（或坩埚） 1内合成制备复合材料熔体 2， 在熔池（或坩埚） 上部插入高能超声变幅杆 3， 对熔体施加超声处理， 在熔池 （或坩埚） 外侧施加磁场 4。 根 据复合材料熔体制备方法以及要求效果的不同， 可以选择不同的磁场施加形式。 因此外加 磁场 4可以是强脉冲磁场、 高频振荡磁场及低频旋转磁场三种磁场。  The composite melt 2 is synthesized in a molten pool (or crucible) 1 made of a heat-insulating refractory material, and a high-energy ultrasonic horn 3 is inserted in the upper part of the molten pool (or crucible), and the melt is ultrasonically treated in the molten pool ( Or 坩埚) Apply magnetic field 4 to the outside. Depending on the method of preparation of the composite melt and the desired effect, different forms of magnetic field application can be selected. Therefore, the applied magnetic field 4 can be three kinds of magnetic fields: a strong pulse magnetic field, a high frequency oscillating magnetic field, and a low frequency rotating magnetic field.
磁场与超声场耦合作用的原理是：  The principle of the coupling of the magnetic field and the ultrasonic field is:
( 1 ) 外加磁场 4选用.强脉冲磁场， 即强脉冲磁场与超声场稱合作用， 强脉冲磁场在熔 体内的脉冲电磁力、 脉冲磁化力和感应电流的焦耳热， 均对原位化学反应有加速作用， 并 能起到使颗粒相弥散分布的目的， 但脉冲磁场在金属熔体内有一定衰减， 熔体边缘区域的 反应受磁场的影响强而中心部位较弱， 因此要选择与高能超声耦合作用， 功率超声通过在 熔体内的空化效应和声流冲击， 空化效应使颗粒团簇得到控制， 声流冲击起到微区搅拌作 用， 由于超声场作用区域是中心区域强而边缘弱， 两者正好互相弥补不足， 耦合作用达到 加速原位反应， 使颗粒相快速生成并呈弥散分布的目的。  (1) The applied magnetic field 4 is selected. The strong pulsed magnetic field, that is, the strong pulsed magnetic field and the ultrasonic field, the pulsed electromagnetic force, the pulsed magnetizing force and the induced current of the intense pulsed magnetic field in the melt are all in situ chemistry. The reaction has an accelerating effect and can play the purpose of dispersing the particle phase. However, the pulsed magnetic field has a certain attenuation in the metal melt, and the reaction in the edge region of the melt is strongly influenced by the magnetic field and the center portion is weak, so it is necessary to select and High-energy ultrasonic coupling, power ultrasonic through the cavitation effect in the melt and acoustic flow impact, cavitation effect allows the particle cluster to be controlled, the acoustic flow impact acts as a micro-region agitation, because the ultrasonic field is strong in the central region The edges are weak, and the two just complement each other. The coupling effect accelerates the in-situ reaction, so that the particle phase is rapidly formed and dispersed.
(2) 外加磁场 4也可选用高频振荡磁场， 高频振荡磁场由于在熔体内存在集肤效应， 所以集中作用于熔池的边缘， 对复合材料熔体中的颗粒形成振荡的电磁力， 使颗粒团簇得 到控制， 超声场仍主要作用于熔池中部区域。  (2) The external magnetic field 4 can also be selected with a high-frequency oscillating magnetic field. Due to the skin effect in the melt, the high-frequency oscillating magnetic field concentrates on the edge of the molten pool and forms an oscillating electromagnetic force on the particles in the composite melt. , the particle cluster is controlled, and the ultrasonic field still mainly acts on the central region of the molten pool.
(3 ) 当对复合材料的颗粒大小及分布要求稍低时， 磁场 4也可以选择采用低频搅拌磁 场与功率超声耦合作用。 特别是当处理的金属量大到以吨位计量时， 由于目前高频振荡磁 场和强脉冲磁场设备的限制， 采用较强的低频搅拌磁场和高能超声耦合作用， 也能达到较 理想的效果。 其原理是： 高能超声通过在熔体内的空化效应和声流冲击， 空化效应使颗粒 团簇得到控制， 声流冲击起到微区搅拌作用， 外加的低频搅拌磁场 4对使整个熔池电磁搅 拌， 超声处理效果更加明显， 且超声处理的局部效应或集中效应得以控制。 (3) When the particle size and distribution requirements of the composite material are slightly lower, the magnetic field 4 can also be selected by using a low-frequency stirring magnetic field and power ultrasonic coupling. Especially when the amount of metal to be processed is large enough to be measured in tonnage, due to the limitations of the current high-frequency oscillating magnetic field and strong pulsed magnetic field equipment, the use of strong low-frequency stirring magnetic field and high-energy ultrasonic coupling can also achieve The ideal effect. The principle is as follows: High-energy ultrasound passes the cavitation effect in the melt and the acoustic flow impact, the cavitation effect makes the particle clusters controlled, the acoustic flow impact acts as a micro-region stirring, and the additional low-frequency stirring magnetic field 4 pairs make the whole melting With the electromagnetic stirring of the pool, the ultrasonic treatment effect is more obvious, and the local effect or concentration effect of the ultrasonic treatment is controlled.
基于上述原理， 实现本发明的技术方案是：  Based on the above principles, the technical solution for implementing the present invention is:
一种磁场与超声场耦合作用下熔体反应合成金属基复合材料的方法， 是： 金属基熔体精 炼后调整到反应起始温度， 加入能与熔体原位反应生成颗粒相的反应物粉剂进行合成反应， 在反应合成过程中 时施加磁场和高能超声场； 待反应结束， 静置到浇注温度后进行浇注。  A method for synthesizing a metal matrix composite by a melt reaction of a magnetic field and an ultrasonic field is: adjusting a metal-based melt to a reaction starting temperature after refining, and adding a reactant powder capable of reacting in situ with the melt to form a particulate phase The synthesis reaction is carried out, and a magnetic field and a high-energy ultrasonic field are applied during the reaction synthesis; after the reaction is completed, the casting is allowed to stand at the pouring temperature.
本发明方法中， 所说的外加磁场可以是强脉冲磁场、 高频振荡磁场或低频交变磁场。 针 对采用的外加磁场的不同形式， 实现本发明的具体的技术方案也有三种- In the method of the present invention, the applied magnetic field may be a strong pulsed magnetic field, a high frequency oscillating magnetic field or a low frequency alternating magnetic field. There are also three specific technical solutions for implementing the present invention in terms of different forms of applied magnetic fields.
( 1 ) 强脉冲磁场与高能超声耦合作用 (1) Strong pulsed magnetic field coupled with high-energy ultrasound
强脉冲磁场的电磁参数范围为：脉冲电流频率 0.1Hz 〜10Hz，脉冲电流密度为 lkA/m2〜 10kA/m2, 充电电压： lkV〜20kV,中心磁场强度 0.5〜20T。 根据坩埚尺寸及熔体种类选择电 磁参数， 使熔体内脉冲磁场强度在 1T以上， 效果明显。 The electromagnetic parameters of the strong pulse magnetic field are: pulse current frequency 0.1 Hz ~ 10 Hz, pulse current density lkA / m 2 ~ 10 kA / m 2 , charging voltage: lkV ~ 20kV, central magnetic field strength 0.5 ~ 20T. According to the size of the crucible and the type of melt, the electromagnetic parameters are selected so that the intensity of the pulsed magnetic field in the melt is above 1T, and the effect is obvious.
超声场的频率 10kHz〜30kHz, 超声强度 0.5kW/m2〜60 kW/m2。 10kHz~30kHz frequency ultrasound field, the intensity of the ultrasound 0.5kW / m 2 ~60 kW / m 2.
具体步骤为： 金属基熔体精炼后调整到复合温度， 加入能与熔体原位反应生成颗粒相的 试剂， 开启磁场稳定后， 插入超声变幅杆到液面下 5〜6mm， 接通超声装置， 超声处理时间 60s〜600s， 时间到后， 停止超声设备， 关掉磁场， 静置到浇注温度后进行绕注。  The specific steps are as follows: After the metal-based melt is refined, it is adjusted to the composite temperature, and a reagent capable of reacting with the melt in situ to form a particulate phase is added. After the magnetic field is stabilized, the ultrasonic horn is inserted into the liquid surface 5 to 6 mm, and the ultrasonic wave is turned on. The device, sonication time 60s~600s, after the time is up, stop the ultrasonic device, turn off the magnetic field, and wait until the pouring temperature to wrap.
该方法特别适用于制备金属基复合材料量少但要求性能极高的复合材料。  The method is particularly suitable for the preparation of composite materials having a small amount of metal matrix composite but requiring extremely high performance.
(2) 高频振荡磁场与高能超声耦合作用  (2) High-frequency oscillating magnetic field and high-energy ultrasonic coupling
高频振荡磁场的电磁参数范围为： 高频基准波频率 10 kHz〜30kHz， 调幅振荡波频率为 1Ηζ〜30Ηζ， 功率范围 0〜100kW， 根据熔体量、 种类、 熔池和搅拌强度调节电磁参数， 对 铝、 铜基熔体， 可采用较高基准波频率， 对铁基、 镍基、 锌基熔体， 采用较低基准波频率， 振荡波频率根据熔体搅动情况确定， 与反应器的结构和金属熔体的种类有关， 以熔体不出 现强烈紊流为宜。  The electromagnetic parameters of the high-frequency oscillating magnetic field are: high-frequency reference wave frequency 10 kHz~30 kHz, amplitude-modulated oscillating wave frequency 1 Ηζ~30 Ηζ, power range 0~100 kW, electromagnetic parameters adjusted according to melt amount, type, molten pool and stirring intensity For aluminum and copper-based melts, a higher reference wave frequency can be used. For iron-based, nickel-based, and zinc-based melts, a lower reference wave frequency is used. The oscillation wave frequency is determined according to the melt agitation condition, and the reactor The structure is related to the type of molten metal, and it is preferred that the melt does not exhibit strong turbulence.
超声场的频率 10kHz〜30kHz, 超声强度 0.5kW/m2〜60 kW/m2。 10kHz~30kHz frequency ultrasound field, the intensity of the ultrasound 0.5kW / m 2 ~60 kW / m 2.
具体步骤为： 金属熔体精炼后调整到反应起始温度， 加入能与金属熔体原位反应生成颗 粒相的反应物粉剂， 幵启磁场稳定后 ·， 插入超声变幅杆到液面下 5〜6mm， 接通超声装置， 超声处理时间 60s〜600s， 时间到后， 停止超声设备， 关掉磁场， 静置到浇注温度后进行浇 注。 The specific steps are as follows: After the metal melt is refined, it is adjusted to the reaction starting temperature, and a reactant powder which can react with the metal melt in situ to form a particle phase is added, and after the magnetic field is stabilized, the ultrasonic horn is inserted into the liquid surface. ~6mm, turn on the ultrasonic device, sonication time 60s ~ 600s , after the time is up, stop the ultrasonic equipment, turn off the magnetic field, and wait for the pouring temperature to carry out the pouring.
(3 ) 低频交变磁场与高能超声耦合作用 具体实施方式 (3) Low-frequency alternating magnetic field and high-energy ultrasonic coupling detailed description
实施例 1: 强脉冲磁场和超声场耦合作用下制备（Al3Zr(s)+ ZrB2(s>)颗粒增强 A1基复合 材料 Example 1: Preparation of (Al 3 Zr( s )+ ZrB 2 ( s> ) particle reinforced A1 matrix composite by strong pulsed magnetic field and ultrasonic field coupling
原材料： 基体金属： 纯 A1; 反应盐： K2ZrF6+KBF4粉剂， 精炼脱气剂及扒渣剂； 制备过程分两步: Raw materials: Base metal: Pure A1; Reaction salt: K 2 ZrF 6 + KBF 4 powder, refined deaerator and slag slag; The preparation process is divided into two steps:
(一）： 金属熔炼及粉体制备：  (1): Metal smelting and powder preparation:
50Kg纯 A1在 60kW电阻炉中熔化升温到 900°C， 脱气、 扒渣。 所用试剂均在 250'C〜 300°C下充分烘干， 其中 K2ZrF6+KBF4， 研磨成细粉 （粒度小于 200 目）， 称量后用铝箔包 覆待用， K2ZrF6+KBF4粉剂加入的重量为金属重量的 20%。 50Kg pure A1 was melted and heated to 900 ° C in a 60 kW resistance furnace to degas and slag. The reagents used are all dried at 250 ° C ~ 300 ° C, wherein K 2 ZrF 6 + KBF 4 , ground into fine powder (particle size less than 200 mesh), weighed and coated with aluminum foil, K 2 ZrF 6 The +KBF 4 powder was added in an amount of 20% by weight of the metal.
(二）： 原位反应合成制备复合材料熔体- 精炼好且符合反应起始温度要求（900 °C ) 的金属液， 用钟罩将 K2ZrF6+KBF4压入到坩 埚内的铝液中， 将坩埚放入强脉冲磁场中， 开启强脉冲磁场， 脉冲磁场的充电电压 lkV， 脉冲频率 1Ηζ。 然后将超声变幅杆插入铝液， 深度 3mm左右， 开启超声装置， 超声场频率 20kHz, 超声强度 2kW/m2， 超声处理时间 5min。 超声结束后， 高频磁场继续施加 3min， 然 后关闭磁场电源， 熔体静置， 待温度降到 720Ό浇入直径 200mm的水冷铜模， 制得复合材 料铸锭。 (2): In-situ reaction synthesis to prepare composite melt - refining metal liquid that meets the reaction initiation temperature requirement (900 °C), press K 2 ZrF 6 + KBF 4 into the crucible aluminum with a bell jar In the liquid, put the helium into a strong pulsed magnetic field, turn on the strong pulsed magnetic field, the charging voltage of the pulsed magnetic field is lkV, and the pulse frequency is 1Ηζ. Then, the ultrasonic horn is inserted into the aluminum liquid, the depth is about 3 mm, the ultrasonic device is turned on, the ultrasonic field frequency is 20 kHz, the ultrasonic intensity is 2 kW/m 2 , and the ultrasonic treatment time is 5 min. After the end of the ultrasonic wave, the high-frequency magnetic field was continuously applied for 3 min, then the magnetic field power was turned off, the melt was allowed to stand, and the temperature was lowered to 720 Torr and poured into a water-cooled copper mold having a diameter of 200 mm to prepare a composite ingot.
复合材料熔体具有很好的流动性， 制得的复合材料铸坯外表面光洁， 内部组织致密， 无 疏松、 缩孔等凝固组织缺陷， 颗粒尺寸 0.2~0.6 ΠΙ (图 3)。  The composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, and no solidification structure defects such as looseness and shrinkage, and the particle size is 0.2~0.6 ΠΙ (Fig. 3).
实施例 2: 高频振荡磁场和超声场耦合作用下制备（Al3Zr(s>+ ZrB2(s))颗粒增强 A1基复 合材料 Example 2: Preparation of Al 3 Zr( s> + ZrB 2 ( s )) particle reinforced A1 matrix composite by high frequency oscillating magnetic field and ultrasonic field coupling
原材料： 基体金属： 纯 A1; 反应盐： K2ZrF6+KBF4粉剂， 精炼脱气剂及扒渣剂； 制备过程分两步： Raw materials: Base metal: Pure A1; Reaction salt: K 2 ZrF 6 + KBF 4 powder, refined deaerator and slag slag; The preparation process is divided into two steps:
( -)： 金属熔炼及粉体制备：  ( -): Metal melting and powder preparation:
50Kg纯 A1在 60kW工频熔铝炉中熔化升温到 900°C， 脱气、 扒渣。 所用试剂均在 250 °C〜300°C下充分烘干， 其中， K2ZrF6+ BF4粉剂研磨成细粉（粒度小于 200目）， 称量后装 入喷吹罐， K2ZrF6+KBF4粉剂加入的重量为金属重量的 20%。 50Kg pure A1 is melted and heated to 900 ° C in a 60kW power frequency melting aluminum furnace, degassing and slag. The reagents used are fully dried at 250 ° C ~ 300 ° C, wherein the K 2 ZrF 6 + BF 4 powder is ground into a fine powder (particle size less than 200 mesh), weighed and placed in a spray can, K 2 ZrF 6 The +KBF 4 powder was added in an amount of 20% by weight of the metal.
(二）： 原位反应合成制备复合材料熔体：  (2): In-situ reaction synthesis to prepare composite melt:
装置如图 2， 精炼好且符合反应起始温度要求 （900°C ) 的金属液从金属精炼保温炉倾 入保温的复合材料熔池 1， 向熔池 1内用用 Ar气喷枪 5吹入 K2ZrF6+KBF4粉末， 喷粉结束 后， 开启高频振荡磁场 4, 高频基准波频率 20kHz， 最大电流 80A， 振荡波频率 25Hz， 振 荡波波形为正弦波。 然后将超声变幅杆 3插入熔池， 深度 5mm左右， 开启超声装置， 超声 场频率 20kHz, 超声强度 10kW/m2， 超声处理时间 5min。 超声结束后， 高频磁场继续施加 3min, 然后关闭磁场电源， 熔体静置， 待温度降到 730°C， 除渣， 720°C时通过半连铸成直 径 2Q0mm的圆坯。 The device is shown in Fig. 2. The molten metal which is refined and meets the reaction initiation temperature requirement (900 °C) is poured from the metal refining holding furnace into the insulated composite material molten pool 1, and is blown into the molten pool 1 by using the Ar gas spray gun 5. K 2 ZrF 6 +KBF 4 powder, after the powder is sprayed, the high-frequency oscillating magnetic field 4 is turned on, the high-frequency reference wave frequency is 20 kHz, the maximum current is 80 A, and the oscillation wave frequency is 25 Hz. The undulating waveform is a sine wave. Then, the ultrasonic horn 3 is inserted into the molten pool to a depth of about 5 mm, and the ultrasonic device is turned on, the ultrasonic field frequency is 20 kHz, the ultrasonic intensity is 10 kW/m 2 , and the ultrasonic treatment time is 5 min. After the end of the ultrasonic wave, the high-frequency magnetic field is continuously applied for 3 min, then the magnetic field power supply is turned off, the melt is allowed to stand, and the temperature is lowered to 730 ° C, and the slag is removed, and the round billet of 2 Q0 mm in diameter is semi-continuously cast at 720 ° C.
复合材料熔体具有很好的流动性， 制得的复合材料铸坯外表面光洁， 内部组织致密， 无 疏松、 缩孔等凝固,组织缺陷， 颗粒尺寸 l~5 m (图 4)。  The composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, no looseness, shrinkage and other solidification, and structural defects, and the particle size is l~5 m (Fig. 4).
实施例 3: 低频搅拌磁场和超声场耦合作用下制备 （Al3Zr(s)+ A1203(S)) 颗粒增强 A1基 复合材料 Example 3: Preparation of low-amplitude stirring magnetic field and ultrasonic field coupling (Al 3 Zr( s )+ A1 2 0 3(S) ) particle reinforced A1 matrix composite
原材料： 基体金属： 纯 A1; 固体粉末： 工业碳酸锆 (Zr(C03)2)粉剂， 精炼脱气剂及扒渣 剂； Raw materials: base metal: pure A1; solid powder: industrial zirconium carbonate (Zr(C0 3 ) 2 ) powder, refined deaerator and slag slag;
制备过程分两步：  The preparation process is divided into two steps:
(一）： 金属熔炼及粉体制备- (1): Metal smelting and powder preparation -
50Kg纯 A1在 60kW工频熔铝炉中熔化升温到 900Ό， 脱气、 扒渣。 所用试剂均在 250 °C〜30(TC下充分烘干， 其中 Zr(C03)2研磨成细粉（粒度小于 200目）， 称量后装入喷吹罐， Zr(C03)2加入的重量为金属重量的 20%。 50Kg pure A1 is melted and heated to 900 Ό in a 60kW power frequency melting aluminum furnace, degassing and slag. The reagents used are all dried at 250 °C~30 (TC), wherein Zr(C0 3 ) 2 is ground into fine powder (particle size less than 200 mesh), weighed and put into the spray can, Zr(C0 3 ) 2 added The weight is 20% of the weight of the metal.
(二）： 原位反应合成制备复合材料熔体- 精炼好且符合反应起始温度要求（900Ό ) 的金属液从金属精炼保温炉倾入保温的复合 材料熔池 3, 向熔池内用用 Ar气喷枪吹入 Zr(C03)2粉末， 同时开启低频搅拌磁场， 磁场的 电磁参数为 10Hz， 电流 280A， 喷粉结束后， 将超声变幅杆插入熔池， 深度 5mm左右， 开 启超声装置， 超声场频率 20kHz， 超声强度 10kW/m2， 超声处理时间 5min。 超声结束后， 继续搅拌 3min， 然后静置， 待温度降到 730°C， 除渣， 720°C通过半连铸制得直径 200mm 的复合材料圆坯。 (2): In-situ reaction synthesis to prepare composite melt - refining and meeting the reaction initiation temperature requirement (900 Ό) of molten metal from the metal refining holding furnace into the insulated composite material pool 3, using Ar in the molten pool The air spray gun blows into the Zr(C0 3 ) 2 powder and simultaneously turns on the low-frequency stirring magnetic field. The electromagnetic parameter of the magnetic field is 10Hz, and the current is 280A. After the powder is sprayed, the ultrasonic horn is inserted into the molten pool, the depth is about 5mm, and the ultrasonic device is turned on. The ultrasonic field frequency is 20 kHz, the ultrasonic intensity is 10 kW/m 2 , and the sonication time is 5 min. After the end of the ultrasonication, stirring was continued for 3 min, and then allowed to stand, until the temperature was lowered to 730 ° C, and the slag was removed, and a round billet of 200 mm in diameter was obtained by semi-continuous casting at 720 ° C.
复合材料熔体具有很好的流动性， 制得的复合材料铸坯外表面光洁， 内部组织致密， 无 疏松、 缩孔等凝固组织缺陷， 颗粒尺寸 l~5 m (图 5)。  The composite melt has good fluidity, and the prepared composite slab has a smooth outer surface, compact internal structure, and no solidification structure defects such as looseness and shrinkage, and the particle size is l~5 m (Fig. 5).

Claims

权利 要求 、 一种磁场与超声场耦合作用下制备金属基原位复合材料的方法， 包括将金属基熔体精炼 后调整到反应起始温度， 加入能与熔体原位反应生成颗粒相的反应物进行合成反应， 待 反应结束， 静置到浇注温度后进行浇注； 其特征在于： 在反应合成过程中同时施加磁场 和高能超声场， 实现磁场磁和高能超声场耦合作用下合成内生颗粒增强金属基复合材 料。  Claims, a method for preparing a metal-based in-situ composite material by coupling a magnetic field and an ultrasonic field, comprising refining a metal-based melt to a reaction initiation temperature, and adding a reaction capable of reacting with the melt in situ to form a particulate phase The synthesis reaction is carried out, and after the reaction is completed, the casting is allowed to stand at the pouring temperature; the characteristic is: simultaneous application of a magnetic field and a high-energy ultrasonic field during the reaction synthesis to realize the synthesis of endogenous particles under the coupling of the magnetic field magnetic field and the high-energy ultrasonic field Metal matrix composites.
、 根据权利要求 1所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 在反应合成过程中同时施加磁场和高能超声场的方式为： 在保温耐火材料制成的熔 池（1 ) 内合成制备复合材料熔体 （2)， 在熔池 （1 ) 上部插入高能超声变幅杆 （3)， 对 熔体 （2 ) 施加超声处理， 在熔池 （1 ) 外侧施加磁场 （4)。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 1, wherein the method of simultaneously applying a magnetic field and a high-energy ultrasonic field during the reaction synthesis process is: The composite melt (2) is synthesized in the molten pool (1), the high-energy ultrasonic horn (3) is inserted in the upper part of the molten pool (1), and the melt (2) is ultrasonically treated on the outside of the molten pool (1). Apply a magnetic field (4).
、 根据权利要求 2所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 操作过程具体是： 金属基熔体精炼后调整到反应起始温度， 加入能与熔体原位反应 生成颗粒相的反应物粉剂， 开启磁场稳定后， 插入超声变幅杆到液面下 5〜6mm， 接通超 声装置， 超声处理时间 60s〜600s， 超声处理时间到后， 停止超声设备， 然后关掉磁场， 静置熔体到浇注温度后进行浇注。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 2, wherein the operation process is specifically: adjusting the metal-based melt to a reaction starting temperature after refining, adding energy and a melt In-situ reaction to form a particulate phase reactant powder. After the magnetic field is stabilized, insert the ultrasonic horn into the liquid surface 5~6mm, turn on the ultrasonic device, and the ultrasonic treatment time is 60s~600s. After the ultrasonic treatment time, stop the ultrasonic equipment. , then turn off the magnetic field, leave the melt to the pouring temperature and pour.
、 根据权利要求 1所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 其中所说的磁场是强脉冲磁场、 高频振荡磁场或低频交变磁场。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 1, wherein the magnetic field is a strong pulse magnetic field, a high frequency oscillating magnetic field or a low frequency alternating magnetic field.
、 根据权利要求 4所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 是在强脉冲磁场与高能超声场耦合作用下制备复合材料， 强脉冲磁场的电磁参数范 围为：脉冲电流频率 0. 1Hz 〜10Hz，脉冲电流密度为 lkA/m2〜10kA/m2， 充电电压： lkV〜 20 kV,线圈中心磁场强度 0. 5〜20 T;超声场的频率 10kHz〜30kHz，超声强度 0. 5kW/m2〜 60 kW/m2。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 4, wherein the composite material is prepared by coupling a strong pulse magnetic field and a high-energy ultrasonic field, and the electromagnetic parameter range of the strong pulse magnetic field is For the pulse current frequency 0. 1Hz ~ 10Hz, the pulse current density is lkA / m 2 ~ 10kA / m 2 , the charging voltage: lkV ~ 20 kV, the coil center magnetic field strength 0. 5~20 T; the frequency of the ultrasonic field 10kHz ~ 30 kHz, ultrasonic intensity 0. 5 kW / m 2 ~ 60 kW / m 2 .
、 根据权利要求 4所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 是在高频振荡磁场与高能超声场耦合作用下制备复合材料， 高频振荡磁场的电磁参 数范围为：高频基准波频率 10kHz 〜30kHz,调幅振荡波频率为 1Ηζ〜30Ηζ，功率范围 0〜 lOOkW, 超声场的频率 10kHz〜30kHz, 超声强度 0. 5kW/m2〜60 kW/m2。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 4, wherein the composite material is prepared by coupling a high frequency oscillating magnetic field and a high energy ultrasonic field, and the electromagnetic field of the high frequency oscillating magnetic field is The range of the parameters is: high frequency reference wave frequency 10 kHz ~ 30 kHz, amplitude modulation oscillating wave frequency is 1 Ηζ ~ 30 Ηζ, power range 0 ~ lOOkW, ultrasonic field frequency 10 kHz ~ 30 kHz, ultrasonic intensity 0. 5 kW / m2 ~ 60 kW / m2.
、 根据权利要求 4所说的磁场与超声场耦合作用下制备金属基复合材料的方法， 其特征在 于， 是在低频交变磁场与高能超声场耦合作用下制备复合材料； 低频交变磁场的电磁参 数范围： 频率： 0. 1Ηζ〜60Ηζ， 工作电流： 1A〜10000A， 超声场的频率 10kHz〜30kHz， 超声强度 0. 5kW/m2〜60 kW/m2。 The method for preparing a metal matrix composite material by coupling a magnetic field and an ultrasonic field according to claim 4, wherein the composite material is prepared by coupling a low frequency alternating magnetic field and a high energy ultrasonic field; electromagnetic of a low frequency alternating magnetic field Parameter range: Frequency: 0. 1Ηζ~60Ηζ, working current: 1A~10000A, frequency of ultrasonic field 10kHz~30kHz, ultrasonic intensity 0. 5kW/m2~60 kW/m2.
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CN106967940B (en) * 2017-05-02 2023-05-30 贵州理工学院 Method and device for preparing arc-shaped special-shaped steel
US20220282356A1 (en) * 2020-01-19 2022-09-08 Jiangsu University Method and apparatus for preparing aluminum matrix composite with high strength, high toughness, and high neutron absorption
US11643709B2 (en) * 2020-01-19 2023-05-09 Jiangsu University Method and apparatus for preparing aluminum matrix composite with high strength, high toughness, and high neutron absorption
CN114182352A (en) * 2021-12-13 2022-03-15 西北工业大学 Preparation method of multi-stage directional growth metal material under multi-field action
CN114182352B (en) * 2021-12-13 2023-01-17 西北工业大学 Preparation method of multi-stage directional growth metal material under multi-field action
CN116372188A (en) * 2023-03-01 2023-07-04 汕头大学 Method and device for regulating and controlling residual stress of additive manufacturing
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