CN113388752B - Preparation method of metal-based composite material - Google Patents

Preparation method of metal-based composite material Download PDF

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CN113388752B
CN113388752B CN202110438409.1A CN202110438409A CN113388752B CN 113388752 B CN113388752 B CN 113388752B CN 202110438409 A CN202110438409 A CN 202110438409A CN 113388752 B CN113388752 B CN 113388752B
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CN113388752A (en
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曾小勤
谷立东
应韬
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Shanghai Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B22D17/007Semi-solid pressure die casting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention relates to a preparation method of a metal matrix composite, which comprises the following steps: processing a base metal material into millimeter-sized base alloy particles with uniform particle size, and carrying out solid-state mixing on the millimeter-sized base alloy particles and small-sized non-metallic reinforcing phase particles to form a state that a non-metallic reinforcing phase wraps the metal particles; quantitatively conveying the mixed material obtained by solid mixing into a cylinder of a metal thixotropic injection machine, and spirally shearing and propelling the mixed material through a conveying rod to heat the matrix metal to a semi-solid melt to form semi-solid composite slurry; the metal matrix composite material member was obtained by performing high-speed injection by an injection machine, molding in a mold, and cooling. Compared with the prior art, the metal-based composite material prepared by the method has the advantages of uniform addition of the reinforcing phase, less oxidation and inclusion in the semi-solid process, remarkable improvement on mechanical property and heat-conducting property, full play of the performance advantage of material compositing, and suitability for continuous preparation and production.

Description

Preparation method of metal matrix composite material
Technical Field
The invention belongs to the field of metal matrix composite preparation and molding, and particularly relates to a preparation method of a metal matrix composite.
Background
The structural material is an important component of social production and life, wherein the metal material has the characteristics of excellent mechanical property, thermal conductivity, durability and the like, so that the metal material is widely applied to the fields of home building materials, traffic automobiles, electronic communication, aerospace and the like, but along with the rapid development of modern society, particularly when the 5G era comes and the new energy industry is prosperous, the performance requirement of an advanced component on the structural material is gradually improved, and the traditional metal material cannot meet the new requirement gradually.
Alloying is a main method for improving the performance of metal materials, and through development for many years, researchers develop a great deal of research work, develop many grades of aluminum alloy, magnesium alloy, zinc alloy and copper alloy, basically establish a perfect alloying theory and recognize the mutual influence mechanism of common alloy elements. However, under the condition that the traditional alloying means is difficult to greatly improve the material performance, the compounding provides a new possibility: the non-metal reinforced phases such as SiC and diamond are added in the metal, and the prepared metal matrix composite material has higher mechanical property and improved physical property. Although the metal matrix composite has the potential of obtaining excellent performance, the preparation method is always a difficulty limiting the production and application of the metal matrix composite. The good metal matrix composite material should have the fine dispersed reinforcement distributed in the matrix, and the microstructure not only can effectively improve the strength of the material, but also can ensure the plasticity of the material. At present, the relatively mature preparation process of the metal matrix composite mainly comprises a stirring casting method, a powder metallurgy method, a pressure infiltration method and the like, but the methods generally have the defects of complex flow, more oxidation impurities, easy agglomeration of a reinforcement, high process cost and the like, and are difficult to adapt to the requirements of low-cost and high-efficiency production. Therefore, the development of a novel metal matrix composite material preparation method with low cost and high efficiency is urgently needed.
Through retrieval, the invention is a Chinese patent with publication number 103789590A, and the invention relates to a preparation method of a particle reinforced magnesium-based composite material, wherein: the preparation method comprises the following steps: firstly, preparing a magnesium alloy semi-solid melt; secondly, preparing a particle-magnesium alloy melt: firstly, heating the particles to 550-600 ℃ to obtain preheated particles; secondly, adding the preheated particles into the magnesium alloy semi-solid melt at the rotating speed of 800 r/min-1000 r/min, and stirring for 3 min-10 min at the rotating speed of 1200 r/min-2000 r/min; thirdly, ultrasonic treatment is carried out for 10min to 35min under the conditions that the temperature is 700 ℃ to 720 ℃ and the stirring speed is 200r/min to 500 r/min; fourthly, stirring for 5 to 10 minutes under the conditions that the temperature is 700 to 720 ℃ and the stirring speed is 200 to 300r/min to obtain particle-magnesium alloy melt; thirdly, pouring the particle-magnesium alloy melt into a mould, pressurizing, solidifying and forming. The technology of the invention utilizes a semi-solid state stirring process, can dope a reinforcing phase into a metal melt, but has the following defects: the melt is easy to have dead zones during mechanical stirring, the reinforcement is difficult to be dispersed uniformly in whole after entering, and the local part is easy to agglomerate; oxide inclusions are easily introduced during stirring, so that the material performance is unstable; complex components and thin-walled parts are difficult to directly form, and subsequent extrusion is often needed to improve density and machining.
Disclosure of Invention
The invention aims to develop a preparation method of a metal-based composite material, wherein a matrix metal is one of magnesium alloy, aluminum alloy, zinc alloy and copper alloy, a non-metal reinforcement can be one or more of mixed materials, and a metal-based composite material component is prepared by premixing, semi-solid heating, shearing, mixing and injection molding of different particle sizes.
The purpose of the invention can be realized by the following technical scheme: a preparation method of a metal matrix composite material comprises the following steps:
step 1: preparing raw materials according to the design proportion of the composite material, processing a base metal material into millimeter-sized base alloy particles with uniform particle size, and simultaneously preparing small-sized non-metallic reinforcing phase particles, and drying the particles;
step 2: carrying out solid-state mixing on the matrix alloy particles and the nonmetal reinforcing phase particles to form a state that the nonmetal reinforcing phase wraps the metal particles;
and step 3: quantitatively conveying the mixed material obtained by solid mixing into a cylinder of a metal thixotropic injection machine, and carrying out gradual heating and heat preservation (the heating temperature and the heat preservation time are set according to the performance of raw materials, aiming at heating and stirring the mixed material to form a semi-solid state with a certain liquid fraction) by spiral shearing propulsion of a conveying rod, so that the matrix metal is heated to a semi-solid melt, the reinforcing phase is also heated and forcibly stirred, and semi-solid composite slurry in which a matrix liquid phase, a matrix spherical solid phase and reinforcing solid phase particles are uniformly distributed is prepared;
and 4, step 4: and when the composite slurry in the semi-solid accumulator is accumulated to a certain volume, ejecting the semi-solid composite slurry at a high speed through an injection machine, and forming and cooling in a mould to obtain the metal matrix composite material component.
The base metal material is one of magnesium alloy, aluminum alloy, zinc alloy and copper alloy.
The granularity of the base alloy particles in the step 1 is 0.5-5 mm, and the granularity is preferably 1-3 mm.
The non-metallic reinforcing phase particles in step 1 comprise: SiC and B 3 N 4 、Al 2 O 3 One or more of TiC, diamond and graphene, the particle size of the diamond is less than or equal to 100 mu m, and the preferable nonmetal isThe particle size of the reinforcing phase is 0.5-20 μm.
The time for solid-state mixing in the step 2 is 15-45 minutes, preferably 30 minutes.
The solid-state mixing mode in the step 2 is three-dimensional mechanical stirring and mixing, so that the raw materials are subjected to three-dimensional motion mixing.
The screw shearing and propelling speed of the conveying rod in the step 3 is 100 r/min-350 r/min, preferably 150 r/min-300 r/min.
And (3) controlling the liquid fraction in the semi-solid composite slurry in the step 3 to be between 40 and 80 percent, and preferably between 50 and 70 percent.
And 4, the speed of the semi-solid composite slurry ejected by the injection machine is 1-10 m/s.
And 4, controlling the temperature of the die to be 200-400 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) the matrix metal and the reinforcing body with different orders of magnitude of particle size are selected for premixing, small-sized reinforcing body particles with larger specific surface area are utilized, and the small-sized reinforcing body particles can be fully adhered to large-sized metal particles through proper three-dimensional mechanical mixing to form a wrapping state, so that initial conditions are provided for uniform addition of the reinforcing body. The granularity of the selected metal can not exceed 5mm, so that the particles are heated uniformly in the semi-solid heating process and the efficiency is higher. The particle size of the reinforcement is selected to be below 100 mu m, so that the adhesion capability of the reinforcement is ensured.
(2) The mixed granules are heated in the closed charging barrel and are stirred at high speed by the shearing screw, after the mixed granules reach a semi-solid state, the reinforcing bodies are further dispersed in the matrix by utilizing the thixotropic property of the semi-solid metal melt and the larger apparent viscosity, and the oxidation and agglomeration are avoided in the stirring process. The liquid fraction is controlled to be between 40% and 80%, so that on one hand, the subsequent forming capability of the semi-solid slurry is ensured, on the other hand, the viscosity of the melt cannot be too low, and otherwise, the reinforcement is easy to agglomerate.
(3) Because the fluidity of the melt is reduced after the reinforcing body is added, the prepared semisolid composite slurry is directly injected and molded at high speed, and the conveying and molding processes are integrated, so that impurities are prevented from being introduced in the composite material pouring process, the density of the composite material is improved by using certain injection pressure, and the filling integrity of a complex component is ensured by matching with higher injection speed.
Drawings
FIG. 1 is a photograph of the microstructure of the composite material obtained in example 1;
FIG. 2 is a photograph of the microstructure of the composite material obtained in comparative example 1;
fig. 3 is a schematic diagram of the principle of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the invention.
The metal-based composite material prepared by the method is an existing metal-based material, and the existing metal-based material is prepared by a special method, and aims to improve the mechanical property and the heat-conducting property of the material. The material comprises a base metal material and a non-metal reinforcement, and the proportion of the material is that the existing non-metal reinforcement reinforces the composite material of the base metal,
the preparation method of the metal matrix composite material comprises the following steps as shown in figure 3:
step 1: according to the composite material mixing theorem, raw materials are prepared according to the requirements of modulus, heat conduction and the like (the proportion is the conventional proportion of a target metal-based composite material), the base metal can be one of magnesium alloy, aluminum alloy, zinc alloy and copper alloy, wherein the base metal material 1 is processed into millimeter-sized particles with uniform particle size, and the particle size is 0.5-5 mm; meanwhile, preparing small-sized non-metallic reinforcing phase particles 2, wherein the non-metallic reinforcing phase comprises one or more of SiC, B3N4, Al2O3, TiC, diamond, graphene and the like, and the particle size is micron-sized or below (less than or equal to 100 mu m), and drying.
Step 2: and (3) carrying out solid-state mixing on the matrix alloy particles and the nonmetal reinforcing phase particles, wherein three-dimensional motion mixing and other methods can be adopted, the mixing time is not less than 15min, and finally, a small-size nonmetal reinforcing phase wrapped in a large-size metal particle state 3 is formed.
And 3, step 3: quantitatively conveying the mixed material into a cylinder of a metal thixotropic injection machine (a JSW 280T MGlle type semi-solid forming machine product can be adopted), spirally shearing and propelling the mixed material through a conveying rod, wherein the rotating speed of a shearing screw rod is not lower than 100r/min, after gradual heating and heat preservation (the temperature is determined by the semi-solid interval of a specific material), heating the matrix metal to a semi-solid melt, heating and forcibly stirring a reinforcing phase, and preparing the semi-solid composite slurry with uniformly distributed matrix liquid phase, matrix spherical solid phase and reinforcing solid phase particles, wherein the liquid fraction is controlled to be 40-80%.
And 4, step 4: and when the composite slurry in the semi-solid accumulator is accumulated to the volume meeting the size of a casting product, the composite slurry is injected at a high speed by an injection machine, the injection speed is not lower than 1m/s, and the composite slurry is molded and cooled in a mold at the temperature of not lower than 200 ℃ to obtain the metal matrix composite material member.
Example 1
The composition of the reinforcement in the composite material is 5 wt% by mass, the matrix metal is AZ91 magnesium alloy, and the particle size is 1.2 mmx1.2mmx4mm; meanwhile, preparing small-sized non-metal reinforced phase SiC particles with the particle size of 10 mu m, and drying the particles. The two are subjected to solid three-dimensional mixing for 30min, then the mixed materials are quantitatively conveyed into a cylinder of a metal thixotropic injection machine, the mixed materials are spirally sheared and pushed by a conveying rod, the rotating speed of a shearing screw rod is 150r/min, semi-solid composite slurry with uniformly distributed matrix liquid phase, matrix spherical solid phase and reinforcement solid phase particles is prepared after gradual heating and heat preservation, and the liquid fraction is controlled at 60%. When the composite slurry in the semi-solid accumulator is accumulated to a certain volume, the composite slurry is injected at a high speed of 2m/s by an injection machine and the temperature of a mould is 250 ℃, so that the metal matrix composite material component is obtained, as shown in figure 1. The mechanical properties are shown in table 1. As can be seen, the yield strength of the alloy is 194MPa, the tensile strength is 264MPa, and the elongation is 5.9%.
Example 2
The composition of the reinforcement in the composite material is 5 wt% by mass, the matrix metal is AM60 magnesium alloy, and the processed particle size is 1.2 mmx1.2mmx4mm; meanwhile, preparing small-sized non-metal reinforced phase SiC particles with the particle size of 10 mu m, and drying the particles. The two are subjected to solid three-dimensional mixing for 30min, then the mixed materials are quantitatively conveyed into a cylinder of a metal thixotropic injection machine, the mixed materials are spirally sheared and pushed by a conveying rod, the rotating speed of a shearing screw rod is 150r/min, semi-solid composite slurry with uniformly distributed matrix liquid phase, matrix spherical solid phase and reinforcement solid phase particles is prepared after gradual heating and heat preservation, and the liquid fraction is controlled at 60%. And when the composite slurry in the semi-solid accumulator is accumulated to a certain volume, the composite slurry is injected at a high speed of 2m/s by an injection machine and the temperature of a mould is 250 ℃, so that the metal matrix composite material component is obtained. The mechanical properties are shown in table 1. As can be seen, the yield strength of the alloy was 160MPa, the tensile strength was 244MPa, and the elongation was 7.3%.
Comparative example 1
The composition of the reinforcement in the composite material is 5 wt% by mass, the matrix metal is AZ91 magnesium alloy, and the composite material is processed into 6mmx6mmx8mm of granularity; meanwhile, preparing small-sized non-metal reinforced phase SiC particles with the particle size of 10 mu m, and drying the particles. The two are subjected to solid three-dimensional mixing for 30min, then the mixed materials are quantitatively conveyed into a cylinder of a metal thixotropic injection machine, the mixed materials are spirally sheared and pushed by a conveying rod, the rotating speed of a shearing screw rod is 150r/min, semi-solid composite slurry with uniformly distributed matrix liquid phase, matrix spherical solid phase and reinforcement solid phase particles is prepared after gradual heating and heat preservation, and the liquid fraction is controlled at 60%. When the composite slurry in the semi-solid accumulator is accumulated to a certain volume, the composite slurry is injected at a high speed of 2m/s by an injection machine and the temperature of a mould is 250 ℃, so that the metal matrix composite material component is obtained, as shown in figure 2. The mechanical properties are shown in table 1. As can be seen, the yield strength of the alloy was 170MPa, the tensile strength was 250MPa, and the elongation was 2.1%.
TABLE 1
Figure BDA0003034109340000061
As can be seen from the above table 1 and the attached figures 1-2, under the process method of the invention, the metal matrix composite material with uniform tissue can be obtained by reasonably mixing and matching the metal particles and the reinforcement body, and through semi-solid shear stirring and molding, the metal matrix composite material has obviously improved elastic modulus, mechanical property and heat conductivity.
Example 3
A preparation method of a metal matrix composite material comprises the following steps:
step 1: preparing raw materials according to the design proportion of the composite material, processing the zinc alloy into matrix alloy particles with uniform particle size of 0.5-1 mm, and preparing non-metal reinforcing phase particles B with particle size of 0.5-1 mu m 3 N 4 Drying the materials;
and 2, step: carrying out solid-state mixing on the matrix alloy particles and the nonmetal reinforcing phase particles for 15 minutes to form a state that the nonmetal reinforcing phase is wrapped in the metal particles;
and step 3: quantitatively conveying the mixed material obtained by solid mixing into a cylinder of a metal thixotropic injection machine, carrying out spiral shearing propulsion through a conveying rod at the propulsion speed of 100r/min, gradually heating and preserving heat to heat matrix metal to a semi-solid melt, heating and forcibly stirring a reinforcing phase to prepare semi-solid composite slurry in which a matrix liquid phase, a matrix spherical solid phase and reinforcing solid phase particles are uniformly distributed, wherein the liquid fraction is controlled at 40%;
and 4, step 4: and when the composite slurry in the semi-solid accumulator is accumulated to a certain volume, ejecting the semi-solid composite slurry at a high speed of 1m/s through an injection machine, and forming and cooling in a mold at 200 ℃ to obtain the metal matrix composite material member.
The yield strength of the obtained metal matrix composite material member is 250MPa, the tensile strength is 305MPa, the elongation is 4.5%, and the thermal conductivity is 80.
Example 4
A preparation method of a metal matrix composite material comprises the following steps:
step 1: preparing raw materials according to the design proportion of the composite material, processing the copper alloy into 4-5 mm matrix alloy particles with uniform particle size, and simultaneously preparing 10-20 mu m of non-metal reinforced phase particle graphene, and drying the particles;
and 2, step: carrying out solid-state mixing on the matrix alloy particles and the nonmetal reinforcing phase particles for 45 minutes to form a state that the nonmetal reinforcing phase is wrapped in the metal particles;
and 3, step 3: quantitatively conveying the mixed material obtained by solid mixing into a cylinder of a metal thixotropic injection machine, carrying out spiral shearing propulsion through a conveying rod at the propulsion speed of 350r/min, gradually heating and preserving heat to heat matrix metal to a semi-solid melt, heating and forcibly stirring a reinforcing phase to prepare semi-solid composite slurry in which a matrix liquid phase, a matrix spherical solid phase and reinforcing solid phase particles are uniformly distributed, wherein the liquid fraction is controlled at 80%;
and 4, step 4: and when the composite slurry in the semi-solid accumulator is accumulated to a certain volume, ejecting the semi-solid composite slurry at a high speed of 10m/s by an injection machine, and forming and cooling in a die at 400 ℃ to obtain the metal matrix composite material member.
The yield strength of the obtained metal matrix composite material member is 250MPa, the tensile strength is 330MPa, the elongation is 5.3 percent, and the thermal conductivity is 280.

Claims (7)

1. The preparation method of the metal matrix composite material is characterized by comprising the following steps:
step 1: preparing raw materials according to the design proportion of the composite material, processing a base metal material into millimeter-sized base alloy particles with uniform particle size, and simultaneously preparing small-sized non-metallic reinforcing phase particles, and drying the particles; the granularity of the base alloy particles is between 1.1 and 5 mm; the non-metallic reinforcing phase particles comprise: SiC and B 3 N 4 、Al 2 O 3 One or more of TiC and diamond, wherein the particle size is 0.5-100 mu m;
step 2: carrying out solid-state mixing on the matrix alloy particles and the nonmetal reinforcing phase particles to form a state that the nonmetal reinforcing phase wraps the metal particles;
and step 3: quantitatively conveying the mixed material obtained by solid mixing into a cylinder of a metal thixotropic injection machine, and carrying out spiral shearing propulsion through a conveying rod to gradually heat and preserve heat so as to heat the matrix metal to a semisolid melt, thereby preparing semisolid composite slurry in which a matrix liquid phase, a matrix spherical solid phase and reinforcement solid phase particles are uniformly distributed; the liquid fraction in the semi-solid composite slurry is controlled to be between 40 and 80 percent;
and 4, step 4: and (3) injecting the semi-solid composite slurry at a high speed through an injection machine, forming and cooling in a mould to obtain the metal matrix composite material component.
2. The method of claim 1, wherein the base metal material is one of a magnesium alloy, an aluminum alloy, a zinc alloy, and a copper alloy.
3. The method for preparing a metal matrix composite according to claim 1, wherein the time for solid state mixing in step 2 is 15 to 45 minutes.
4. The method of claim 1, wherein the solid-state mixing in step 2 is three-dimensional mechanical stirring.
5. The method for preparing a metal matrix composite according to claim 1, wherein the screw shearing advancing speed of the conveying rod in the step 3 is 100r/min to 350 r/min.
6. The method for preparing a metal matrix composite according to claim 1, wherein the speed of the semi-solid composite slurry injected by the injection machine in the step 4 is 1m/s to 10 m/s.
7. The method for preparing a metal matrix composite according to claim 1, wherein the temperature of the mold in step 4 is 200 ℃ to 400 ℃.
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JPH0320424A (en) * 1989-06-19 1991-01-29 Kobe Steel Ltd Manufacture of particle-dispersed composite
JPH09118945A (en) * 1995-10-26 1997-05-06 Ishikawajima Harima Heavy Ind Co Ltd Copper alloy base wear resistant composite material and its manufacture
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CN108396167B (en) * 2018-04-29 2019-09-20 中北大学 A kind of method that injection moulding prepares graphene reinforced aluminum matrix composites
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