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WO2010051675A1 - Procédé de synthèse d'un matériau composite à base de métal par réaction à l'état fondu dans un champ magnétique et un champ d'ultrasons couplés - Google Patents

Procédé de synthèse d'un matériau composite à base de métal par réaction à l'état fondu dans un champ magnétique et un champ d'ultrasons couplés 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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Prior art keywords
magnetic field
ultrasonic
field
melt
reaction
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Ceased
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PCT/CN2009/000252
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English (en)
Chinese (zh)
Inventor
赵玉涛
陈刚
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Jiangsu University
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Jiangsu University
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Priority to US13/126,510 priority Critical patent/US20110247778A1/en
Publication of WO2010051675A1 publication Critical patent/WO2010051675A1/fr
Anticipated expiration legal-status Critical
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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).

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

L'invention concerne un procédé de synthèse d'un matériau composite à base de métal par réaction à l'état fondu dans un champ magnétique et un champ d'ultrasons couplés, qui comprend : amener le métal de base fondu à la température de début de réaction après affinage, ajouter ensuite des réactifs qui, par une réaction de synthèse in situ, forment avec le bain de fusion des particules renforcées, laisser reposer le bain de fusion qui réagit jusqu'à ce qu'il se soit refroidi jusqu'à la température de coulée après la réaction, et couler. Pendant la réaction, un champ magnétique et un champ d'ultrasons à haute énergie sont appliqués simultanément. Le champ magnétique peut être un champ magnétique pulsé à haute puissance, un champ magnétique oscillant à haute fréquence ou un champ magnétique alternatif à basse fréquence. Le matériau composite à base de métal produit par le procédé décrit ci-dessus présente des particules renforcées plus fines, réparties plus uniformément et mieux mariées avec la matrice métallique.
PCT/CN2009/000252 2008-11-05 2009-03-10 Procédé de synthèse d'un matériau composite à base de métal par réaction à l'état fondu dans un champ magnétique et un champ d'ultrasons couplés Ceased WO2010051675A1 (fr)

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US13/126,510 US20110247778A1 (en) 2008-11-05 2009-03-10 Method of synthesizing metal -based composite material by melt reaction in coupling magnetic field and ultrasonic field

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CN2008102349789A CN101391290B (zh) 2008-11-05 2008-11-05 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
CN200810234978.9 2008-11-05

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