CN112210688A - Copper-based composite material and preparation method thereof - Google Patents

Copper-based composite material and preparation method thereof Download PDF

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Publication number
CN112210688A
CN112210688A CN202010592349.4A CN202010592349A CN112210688A CN 112210688 A CN112210688 A CN 112210688A CN 202010592349 A CN202010592349 A CN 202010592349A CN 112210688 A CN112210688 A CN 112210688A
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copper
composite material
based composite
powder
alloy
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CN112210688B (en
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宋克兴
冯江
国秀花
周延军
李韶林
赵培峰
王旭
张朝民
林焕然
张祥峰
杨豫博
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Henan University of Science and Technology
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Henan University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D13/00—Centrifugal casting; Casting by using centrifugal force
    • B22D13/08—Centrifugal casting; Casting by using centrifugal force in which a stationary mould is fed from a rotating mass of liquid metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/03—Press-moulding apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C22C32/0057—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
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Abstract

The invention relates to a copper-based composite material and a preparation method thereof, belonging to the technical field of metal-based composite materials. The invention provides a copper-based composite material, which comprises a reinforcing material and a copper matrix, wherein the copper-based composite material is in a cylinder shape, and the content of the reinforcing material is in gradient distribution from inside to outside along a direction vertical to the central axis of the cylinder; wherein the reinforcing material is a metal oxide, a metal carbide, a metal boride or a refractory metal. The copper-based composite material has the advantages of both the copper matrix and the copper-based composite material, has excellent comprehensive performance, good electrical conductivity and thermal conductivity, high strength, and good heat resistance and wear resistance.

Description

Copper-based composite material and preparation method thereof
Technical Field
The invention relates to a copper-based composite material and a preparation method thereof, belonging to the technical field of metal-based composite materials.
Background
Copper is widely applied to industrial production as a material with electric and heat conducting functions. However, copper has low strength, poor heat resistance and abrasion resistance, and is easily softened and deformed at high temperatures.
Although the copper-based composite material prepared by adding the reinforcing material into copper can improve the strength, heat resistance and wear resistance of the copper-based composite material and relieve the defect of easy softening and deformation of copper at high temperature, the copper-based composite material has poor electric conductivity or thermal conductivity, and along with the continuous development of information technology, the requirement on the copper-based composite material in a special environment is increasingly improved, and the requirement on the performance of the common copper-based composite material under a severe condition is difficult to meet by the common copper-based composite material.
Disclosure of Invention
A first object of the present invention is to provide a copper-based composite material having excellent electrical conductivity, thermal conductivity and wear resistance.
The second purpose of the invention is to provide a preparation method of the copper-based composite material, which is simple to operate and has controllability.
The copper-based composite material comprises a reinforcing material and a copper matrix, wherein the copper-based composite material is in a cylinder shape, and the content of the reinforcing material is in gradient distribution from inside to outside along a direction perpendicular to the central axis of the cylinder;
wherein the reinforcing material is a metal oxide, a metal carbide, a metal boride or a refractory metal.
It should be understood that, along the direction perpendicular to the central axis of the column, the content of the reinforcing material may be in a gradient distribution from inside to outside, wherein, along the direction perpendicular to the central axis of the column, the content of the reinforcing material is increased in a gradient manner from inside to outside, and in this case, the content of the reinforcing material in the innermost material of the copper-based composite material is the smallest, and the content of the reinforcing material in the innermost material of the copper-based composite material may be 0 wt%, or more than 0 wt%, such as 2 wt%, and the content of the reinforcing material in the outermost material of the copper-based composite material is the highest.
The content of the reinforcing material in the copper-based composite material is distributed in a gradient manner from inside to outside, the reinforcing material in the gradient layer material with higher content of the reinforcing material in the copper-based composite material improves the strength, heat resistance, wear resistance and other properties of the copper matrix, and relieves the defect that the copper matrix is easy to soften and deform at high temperature, and the copper-based composite material has better electrical conductivity and thermal conductivity in the gradient layer material with lower content of the reinforcing material and even without the reinforcing material. The copper-based composite material has the advantages of both the copper matrix and the copper-based composite material, has excellent comprehensive performance, good electrical conductivity and thermal conductivity, high strength, and good heat resistance and wear resistance.
Preferably, the distribution is in a gradient from inside to outside, and the gradient from inside to outside is increased.
Along the direction vertical to the central axis of the column, the content of the reinforcing material is increased in a gradient manner from inside to outside, the content of the reinforcing material in the external material of the copper-based composite material is higher, so that the copper-based composite material has higher strength, heat resistance and wear resistance, and the content of the reinforcing material in the internal material of the copper-based composite material is lower, so that the copper-based composite material has better electrical conductivity and thermal conductivity. In practical application, the copper-based composite material with the gradient distribution of the specific reinforcing material can be selected according to the requirement.
Preferably, the cylinder is a cylinder. Preferably, the annular gradient copper-based composite material is used.
Preferably, the maximum content of the reinforcing material in the copper-based composite material is 25 wt%. The maximum content of the reinforcing material in the copper-based composite material of 25 wt% is beneficial to ensuring that the copper-based composite material has good strength, heat resistance and wear resistance, and the processability of the copper-based composite material is not influenced.
It should be understood that the maximum content of the reinforcing material in the copper-based composite material is 25 wt%, which means that the content of the reinforcing material in the material at any position of the copper-based composite material is below 25 wt%. The content of the reinforcing material is increased in a gradient manner from inside to outside along the direction vertical to the central axis of the column, and the content of the reinforcing material in the outermost material of the copper-based composite material is below 25 wt%.
Preferably, the metal oxide is Al2O3、ZrO2、TiO2、MgO、CeO2Or La2O3；
The metal carbide is TiC, WC and B4C or Cr3C2；
The metal boride is CrB2、TiB2Or ZrB2；
The refractory metal is W or Mo.
The metal oxide, the metal carbide, the metal boride or the refractory metal is a copper-based composite material reinforcing phase, has a good reinforcing effect, and is beneficial to improving the strength, the heat resistance and the wear resistance of the copper-based composite material.
Preferably, the copper matrix is Cu or a copper alloy consisting of Cu and at least one metal selected from Cr, Zr, Ti and Fe.
Preferably, the copper alloy is a Cu-Cr alloy, a Cu-Zr alloy, a Cu-Cr-Zr alloy, a Cu-Ti alloy or a Cu-Fe alloy;
wherein the mass ratio of Cu to Cr in the Cu-Cr alloy is 100: 0.4-1.2;
the mass ratio of Cu to Cr to Zr in the Cu-Cr-Zr alloy is 100: 0.4-1.2: 0.03-0.3;
the mass ratio of Cu to Zr in the Cu-Zr alloy is 100: 0.03-0.3;
the mass ratio of Cu to Ti in the Cu-Ti alloy is 100: 0.5-5;
the mass ratio of Cu to Fe in the Cu-Fe alloy is 100: 0.3-4.
A preparation method of a copper-based composite material comprises the following steps:
filling mixed powder containing a reinforcing material and a copper base material into a cylindrical mold provided with an annular partition plate, enabling the content of the reinforcing material in the mixed powder to be distributed in a gradient manner from inside to outside along a direction vertical to the central shaft of the mold, removing the partition plate, and then pressing and sintering to obtain the composite material;
wherein the reinforcing material is a metal oxide, a metal carbide, a metal boride or a refractory metal.
It can be understood that, the axis coincidence of the annular partition plate and the cylindrical mold is an optimized scheme, the thickness of the annular partition plate should be as small as possible, the requirement that the cylindrical mold can be divided into a plurality of spaces is met, and the influence on the mixed powder in the gradient distribution is small or negligible after the annular partition plate is removed.
The quantity of the annular partition plates can be 1, 2, 3, 4, 5, 6 or 7, or more partition plates, the quantity of the partition plates is increased, so that the content difference of the reinforcing materials in the mixed powder at the two sides of the partition plates is reduced, the uniformity of the transition layer is improved, and the quantity of the partition plates can be adjusted according to the requirements of production and cost.
It is understood that when the number of the partition plates is plural, the spacing between the adjacent annular partition plates is not limited, and may be equally spaced, for example, the diameter of 3 annular partition plates may be 0.9 times, 0.8 times and 0.7 times the diameter of the cylindrical mold in sequence, or may be unequally spaced, for example, the diameter of 3 annular partition plates may be 0.9 times, 0.75 times and 0.7 times the diameter of the cylindrical mold in sequence.
It is understood that when the number of the partition plates is more than 2, the content difference of the reinforcing materials in the mixed powder on both sides of each partition plate may be the same, for example, the content of the reinforcing materials in the mixed powder charged into the cylindrical mold provided with 3 annular partition plates is 15%, 10%, 5%, 0% in order from the outer annular space to the inner annular space, or may be different, for example, the content of the reinforcing materials in the mixed powder charged into the cylindrical mold provided with 3 annular partition plates is 12%, 8%, 5%, 0% in order from the outer annular space to the inner annular space.
The preparation method of the copper-based composite material only needs to carry out gradient powder loading on mixed powder containing different reinforcing materials, and then the mixed powder is pressed and sintered to prepare the copper-based composite material.
Preferably, the content difference of the reinforcing materials in the mixed powder filled into the two sides of the annular partition plate is within 5 percent. When the content difference of the reinforcing materials in the mixed powder filled into the two sides of the annular partition plate is within 5%, the content difference of the reinforcing materials in the mixed powder of the two adjacent layers is smaller, and the transition layer is smoother.
Preferably, the distribution is in a gradient from inside to outside, and the gradient from inside to outside is increased.
Preferably, the cylindrical mold is a cylindrical mold.
Preferably, the maximum content of reinforcing material in the mixed powder is 25 wt%.
Preferably, the metal oxide is Al2O3、ZrO2、TiO2、MgO、CeO2Or La2O3；
The metal carbide is TiC, WC and B4C or Cr3C2；
The metal boride is CrB2、TiB2Or ZrB2；
The refractory metal is W or Mo.
Preferably, the copper base material is Cu powder or alloy powder consisting of Cu powder and at least one metal powder of Cr powder, Zr powder, Ti powder and Fe powder.
Preferably, the alloy powder is Cu-Cr alloy powder, Cu-Zr alloy powder, Cu-Cr-Zr alloy powder, Cu-Ti alloy powder or Cu-Fe alloy powder;
wherein the mass ratio of Cu powder to Cr powder in the Cu-Cr alloy powder is 100: 0.4-1.2;
the mass ratio of Cu powder, Cr powder and Zr powder in the Cu-Cr-Zr alloy powder is 100: 0.4-1.2: 0.03-0.3;
the mass ratio of Cu powder to Zr powder in the Cu-Zr alloy powder is 100: 0.03-0.3;
the mass ratio of Cu powder to Ti powder in the Cu-Ti alloy powder is 100: 0.5-5;
the mass ratio of Cu powder to Fe powder in the Cu-Fe alloy powder is 100: 0.3-4.
Preferably, the pressing pressure is 180-300 MPa, and the pressing time is 6-8 min. Pressing for 6-8 min under the pressure of 180-300 MPa, which is beneficial to improving the densification of the blank, and the requirement of overhigh pressure on equipment is higher and the energy consumption is higher. The most economical at this pressure and time.
Preferably, the sintering temperature is 950-1060 ℃, the sintering time is 1-5 h, and the sintering vacuum degree is 1 x 10-3～1×10-1Pa. At 950-1060 ℃ and 1 × 10-3～1×10-1And Pa sintering for 1-5 h is favorable for obtaining the high-densification copper-based composite material, and sintering under a vacuum condition is favorable for reducing the gas content in the composite material and improving the density of the composite material.
Preferably, the preparation method of the copper-based composite material further comprises the following steps:
and smelting the copper-based composite material blank obtained by sintering as a consumable electrode by a vacuum consumable arc smelting method, wherein a melt formed by melting the consumable electrode in the smelting process vertically drips under the action of electromagnetic force to form a molten pool, the molten pool rotates under the action of the electromagnetic force, and the copper-based composite material blank is obtained after cooling.
After the copper-based composite material is smelted by a vacuum consumable arc smelting method, the uniformity of a transition layer is further improved, and in the smelting process, a centrifugal force is formed under the action of electromagnetic force, so that a molten pool rotates directionally, reinforcing material particles are increased at the edges of a casting blank, the center of the casting blank is reduced, the transition is more uniform, the connection is smoother, and the comprehensive performance of the material is improved. Vacuum arc melting melts and recrystallizes the consumable electrode bar, and under the action of vacuum and electromagnetic force, negative pressure is kept in the melting process, so that gas is discharged out of the melting furnace, the densification of the cast ingot is ensured, meanwhile, the impurities are generally lighter, and can float above the melt or be distributed on the edge under the action of centrifugal force, so that the purity of the cast ingot is ensured.
Preferably, the smelting current is 2500-4500A, and the smelting voltage is 23-28V. Smelting under the current of 2500-4500A and the voltage of 23-28V, which is beneficial to matching of electrode feeding amount and melting speed, and obtaining the ingot with uniform structure.
Preferably, the electromagnetic force is generated by arc stabilizing current, and the arc stabilizing current is 5-18A. 5 ~ 18A's steady arc current makes the molten bath rotatory, forms centrifugal force for reinforcing material granule increases at the limit portion of casting blank, and the core reduces, makes the transition more even, links up more smoothly, improves the comprehensive properties of material.
Preferably, the arc stabilizing current is 7-15A. The arc stabilizing current of 7-15A is more beneficial to the fact that the content difference of the reinforcing materials in the mixed powder of the two adjacent layers is small, and the transition layer is more smooth.
Preferably, the arc stabilizing current is 7-12A.
Preferably, the arc stabilizing current is 7-10A.
Drawings
Fig. 1 is a schematic view of a cylindrical mold provided with an annular partition plate of example 1;
FIG. 2 is a schematic view of the copper-based composite material obtained by melting in example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments.
In the preparation method of the copper-based composite material, after the partition plate is removed, vibration, material rolling and reverse material upsetting are carried out, and then pressing is carried out.
Preferably, the vibration is mechanical vibration. The vibration time is 30-70 s.
Preferably, the material rolling time is 4-8 min.
Preferably, the reverse material upsetting times are 4-6.
In the preparation method of the copper-based composite material, the pressing method is a cold isostatic pressing method.
In the preparation method of the copper-based composite material, the particle size of the copper base material is 1-200 mu m. The particle size of the reinforcing material is 0.5-100 mu m.
In the preparation method of the copper-based composite material, the preparation method of the mixed powder of the reinforcing material and the copper base material comprises the following steps: and mixing the reinforcing material and the copper base material in a mixer for 2-16 h.
In the method for producing a copper-based composite material of the present invention, the melting is performed in a protective gas. The protective gas is helium.
The specific embodiment of the preparation method of the copper-based composite material is as follows:
example 1
The preparation method of the copper-based composite material of the embodiment takes the copper-based composite material composed of TiC and pure copper as an example, the mass percentage content of TiC is 10%, 5% and 0% in sequence from the outer ring to the inner ring along the direction perpendicular to the central axis of the copper-based composite material of the column, and the steps are as follows:
powder filling
(1) The diameter of the cylindrical mold is 80mm, the diameters of the two partition plates are 60 and 40 in sequence, the two partition plates are placed into the mold, and the mold is divided into three annular spaces, as shown in fig. 1, 1 is the mold, 2 is the partition plate, 3 is the outer annular space, 4 is the middle annular space between the two partition plates, and 5 is the inner annular space.
(2) And (3) weighing TiC and copper powder to enable the weight ratio of the TiC to the copper powder to be 10:90, and mixing the powder in a mixer for 3 hours to obtain mixed powder I.
And (3) weighing TiC and copper powder to enable the weight ratio of the TiC to the copper powder to be 5:95, and mixing the powder in a mixer for 3 hours to obtain mixed powder II.
And weighing copper powder, and marking as mixed powder III.
(3) Filling the mixed powder I into the outer ring space shown in figure 1, filling the mixed powder II into the middle ring space shown in figure 1, filling the mixed powder III into the inner ring space shown in figure 1, then drawing out the partition plate, vibrating for 40s, rolling for 5min, and upsetting materials reversely for 4 times.
(II) pressing
And (3) pressing the gradient mixed powder obtained in the step (I) by using a cold isostatic press, wherein the pressing pressure is 250MPa, and the pressing time is 7min, so that the annular gradient blank is obtained.
(III) sintering
Sintering the blank obtained in the step (II) with the sintering vacuum degree of 1 multiplied by 10-2Pa, the gas content in the composite material is effectively reduced by vacuum sintering, the density of the composite material is favorably improved, the temperature of the vacuum sintering is 1000 ℃, and the time of the vacuum sintering is 3 hours, so that the copper-based composite material is obtained.
Example 2
The difference between the preparation method of the copper-based composite material of the embodiment and the embodiment 1 is that the copper-based composite material obtained in the step (three) of the embodiment 1 is used as a consumable electrode to be smelted, and the steps are as follows:
taking the copper-based composite material obtained in the step (III) in the example 1 as a consumable electrode, putting the consumable electrode into a vacuum consumable electric arc furnace, closing a furnace door, vacuumizing the vacuum consumable electric arc furnace, then filling protective gas helium, and carrying out vacuum consumable electric arc furnace smelting, wherein the smelting current is 3500A, the smelting voltage is 25V, under the action of the electric arc, the consumable electrode is molten and then drops into a water-cooled copper crucible to be rapidly solidified into an ingot, the arc stabilizing current is 10A, the rotation of a molten pool is ensured, the centrifugal force is formed, the reinforcing material particles are increased at the edge part of a casting blank, the core part is reduced, the transition is more uniform and smooth, and the copper-based composite material is obtained, as shown in fig. 2, the schematic diagram of the copper-based composite material obtained by smelting is shown in fig. 2, the black points in fig. 2 are reinforcing phase particles, and the reinforcing phases are distributed from high to low.
Example 3
The copper-based composite material of this example was prepared using Al2O3Copper-based composite material composed of Cu-Ti alloy powder, Al2O3The mass percentage of the copper-based composite material is 16 percent, 12 percent, 8 percent, 4 percent and 1 percent from the outer ring to the inner ring in sequence along the direction vertical to the central axis of the copper-based composite material of the column, and the steps are as follows:
powder filling
(1) The diameter of the cylindrical mold is 80mm, the diameters of the four partition plates are 70, 60, 50 and 40 in sequence, the four partition plates are placed into the mold, and the mold is divided into five annular spaces.
(2) Mixing Cu powder and Ti powder according to the mass ratio of 100:2, and mixing the powder in a mixer for 3 hours to obtain Cu-Ti alloy powder.
Weighing Al2O3With Cu-Ti alloy powder to make Al2O3Mixing the powder and Cu-Ti alloy powder for 5 hours in a mixer at a weight ratio of 16:84, and marking as mixed powder I.
Weighing Al2O3With Cu-Ti alloy powder to make Al2O3The weight ratio of the mixed powder to the Cu-Ti alloy powder is 12:88, and the mixed powder is mixed for 3 hours in a mixer and marked as mixed powder II.
Weighing Al2O3With Cu-Ti alloy powder to make Al2O3Mixing the powder with Cu-Ti alloy powder for 5h in a mixer at a weight ratio of 8:92, and marking as mixed powder III.
Weighing Al2O3With Cu-Ti alloy powder to make Al2O3The weight ratio of the Cu-Ti alloy powder to the Cu-Ti alloy powder is 4:96, and the mixed powder is mixed for 3 hours in a mixer and is marked as mixed powder IV.
Weighing Al2O3With Cu-Ti alloy powder to make Al2O3The weight ratio of the mixed powder to the Cu-Ti alloy powder is 1:99, and the mixed powder is mixed for 3 hours in a mixer and marked as mixed powder V.
(3) Respectively filling the mixed powder I, the mixed powder II, the mixed powder III, the mixed powder IV and the mixed powder V into five annular spaces to ensure that Al in the mixed powder2O3The content of the inorganic acid is distributed in a gradient decreasing way from the outer ring space to the inner ring space, then the clapboard is pulled out, and the materials are vibrated for 40s, rolled for 5min and reversely piled for 4 times.
(II) pressing
And (3) pressing the gradient mixed powder obtained in the step (I) by using a cold isostatic press, wherein the pressing pressure is 180MPa, and the pressing time is 8min, so that the annular gradient blank is obtained.
(III) sintering
Sintering the blank obtained in the step (II) with the sintering vacuum degree of 1 multiplied by 10-3Pa, the gas content in the composite material is effectively reduced by vacuum sintering, the density of the composite material is favorably improved, the temperature of the vacuum sintering is 950 ℃, the time of the vacuum sintering is 2.5h, and the consumable electrode of the copper-based composite material is obtained.
(IV) melting
And (3) putting the consumable electrode of the copper-based composite material obtained in the step (three) into a vacuum consumable electric arc furnace, vacuumizing the vacuum consumable electric arc furnace after a furnace door is closed, then filling protective gas helium, and smelting in the vacuum consumable electric arc furnace at the smelting current of 4500A and the smelting voltage of 23V, dropping the consumable electrode into a water-cooled copper crucible after the consumable electrode is molten under the action of an electric arc, quickly solidifying into an ingot, and obtaining the copper-based composite material at the arc stabilizing current of 13A.
Example 4
The preparation method of the copper-based composite material of the embodiment uses TiB2Copper-based composite materials with Cu-Fe alloy powder, TiB2The mass percentage of the copper-based composite material is 25 percent, 20 percent, 15 percent, 10 percent, 5 percent and 0 percent from the outer ring to the inner ring in sequence along the direction vertical to the central axis of the copper-based composite material of the column, and the steps are as follows:
powder filling
(1) The diameter of the cylindrical mold is 80, the diameters of the five partition plates are 70, 60, 50, 40 and 30 in sequence, the five partition plates are placed into the mold, and the mold is divided into six annular spaces.
(2) Mixing Cu powder and Fe powder according to a mass ratio of 100:4, and mixing the powder in a mixer for 3 hours to obtain Cu-Fe alloy powder.
Weighing TiB2With Cu-Fe alloy powder to make TiB2Mixing the powder with Cu-Fe alloy powder for 5 hours in a mixer at a weight ratio of 25:75, and marking as mixed powder I.
Weighing TiB2With Cu-Fe alloy powder to make TiB2The weight ratio of the Cu-Fe alloy powder to the Cu-Fe alloy powder is 20:80, and the powder is mixed for 3 hours in a mixer and is marked as mixed powder II.
Weighing TiB2With Cu-Fe alloy powder to make TiB2The weight ratio of the Cu-Fe alloy powder to the Cu-Fe alloy powder is 15:85, and the powder is mixed for 5 hours in a mixer and is marked as mixed powder III.
Weighing TiB2With Cu-Fe alloy powder to make TiB2The weight ratio of the Cu-Fe alloy powder to the Cu-Fe alloy powder is 10:90, and the powder is mixed for 3 hours in a mixer and is marked as mixed powder IV.
Weighing TiB2With Cu-Fe alloy powder to make TiB2The weight ratio of the Cu-Fe alloy powder to the Cu-Fe alloy powder is 5:95, and the powder is mixed for 3 hours in a mixer, and is marked as mixed powder V.
Weighing Cu-Fe alloy powder and marking as mixed powder VI.
(3) Respectively filling the mixed powder I, the mixed powder II, the mixed powder III, the mixed powder IV, the mixed powder V and the mixed powder VI into six annular spaces to ensure that TiB in the mixed powder2The content of the diaphragm is distributed in a gradient way from the outer ring space to the inner ring space, and then the diaphragm is drawn out for vibrationMoving for 40s, rolling for 5min, and reversely upsetting for 4 times.
(II) pressing
And (3) pressing the gradient mixed powder obtained in the step (I) by using a cold isostatic press, wherein the pressing pressure is 300MPa, and the pressing time is 6min, so that the annular gradient blank is obtained.
(III) sintering
Sintering the blank obtained in the step (II) with the sintering vacuum degree of 1 multiplied by 10-1Pa, the gas content in the composite material is effectively reduced by vacuum sintering, the density of the composite material is favorably improved, the temperature of the vacuum sintering is 1060 ℃, the time of the vacuum sintering is 3h, and the consumable electrode of the copper-based composite material is obtained.
(IV) melting
And (3) putting the consumable electrode of the copper-based composite material obtained in the step (three) into a vacuum consumable electric arc furnace, vacuumizing the vacuum consumable electric arc furnace after a furnace door is closed, then filling protective gas helium, and smelting in the vacuum consumable electric arc furnace at the smelting current of 2500A and the smelting voltage of 28V, dropping the consumable electrode into a water-cooled copper crucible after the consumable electrode is molten under the action of an electric arc, quickly solidifying into an ingot, and obtaining the copper-based composite material at the arc stabilizing current of 10A.
Example 5
In the preparation method of the copper-based composite material of the embodiment, taking the copper-based composite material composed of W and Cu-Cr-Zr alloy powder as an example, the mass percentage content of W is 12%, 9%, 6%, 3% and 0% in sequence from the outer ring to the inner ring along the direction perpendicular to the central axis of the copper-based composite material of the column, and the steps are as follows:
powder filling
(1) The diameter of the cylindrical mold is 80, the diameters of the four partition plates are 70, 60, 50 and 40 in sequence, the four partition plates are placed into the mold, and the mold is divided into five annular spaces.
(2) Mixing Cu powder, Cr powder and Zr powder according to the mass ratio of 100:1:0.2, and mixing the powder in a mixer for 3 hours to obtain Cu-Cr-Zr alloy powder.
Weighing W and Cu-Cr-Zr alloy powder to ensure that the weight ratio of the W to the Cu-Cr-Zr alloy powder is 12:88, and mixing the powder for 5 hours in a mixer to obtain mixed powder I.
Weighing W and Cu-Cr-Zr alloy powder to ensure that the weight ratio of the W to the Cu-Cr-Zr alloy powder is 9:91, and mixing the powder in a mixer for 3 hours to obtain mixed powder II.
Weighing W and Cu-Cr-Zr alloy powder to ensure that the weight ratio of the W to the Cu-Cr-Zr alloy powder is 6:94, and mixing the powder for 5 hours in a mixer to obtain mixed powder III.
Weighing W and Cu-Cr-Zr alloy powder to ensure that the weight ratio of the W to the Cu-Cr-Zr alloy powder is 3:97, and mixing the powder for 3 hours in a mixer to obtain mixed powder IV.
Weighing Cu-Cr-Zr alloy powder and marking as mixed powder V.
(3) And respectively filling the mixed powder I, the mixed powder II, the mixed powder III, the mixed powder IV and the mixed powder V into five annular spaces, so that the content of W in the mixed powder is in gradient decreasing distribution from an outer annular space to an inner annular space, then drawing out the partition plate, vibrating for 40s, rolling for 5min and reversely upsetting for 4 times.
(II) pressing
And (3) pressing the gradient mixed powder obtained in the step (I) by using a cold isostatic press, wherein the pressing pressure is 220MPa, and the pressing time is 7.5min, so that the annular gradient blank is obtained.
(III) sintering
Sintering the blank obtained in the step (II) with the sintering vacuum degree of 1 multiplied by 10-2Pa, the gas content in the composite material is effectively reduced by vacuum sintering, the density of the composite material is favorably improved, the temperature of the vacuum sintering is 1020 ℃, the time of the vacuum sintering is 3h, and the consumable electrode of the copper-based composite material is obtained.
(IV) melting
And (3) putting the consumable electrode of the copper-based composite material obtained in the step (three) into a vacuum consumable electric arc furnace, vacuumizing the vacuum consumable electric arc furnace after a furnace door is closed, then filling protective gas helium, and smelting in the vacuum consumable electric arc furnace at the smelting current of 3000A and the smelting voltage of 25V, dropping the consumable electrode into a water-cooled copper crucible after the consumable electrode is molten under the action of an electric arc, quickly solidifying into an ingot, and obtaining the copper-based composite material at the arc stabilizing current of 14A.
Example 6
In the preparation method of the copper-based composite material of the embodiment, taking the copper-based composite material composed of WC and Cu-Zr alloy powder as an example, the mass percentage of WC is 5%, 3% and 0% in sequence from the outer ring to the inner ring along the direction perpendicular to the central axis of the copper-based composite material of the column, and the steps are as follows:
powder filling
(1) The diameter of the cylindrical mold is 80, the diameters of the two partition plates are 60 and 40 in sequence, the two partition plates are placed into the mold, and the mold is divided into three annular spaces.
(2) And mixing the Cu powder and the Zr powder according to the mass ratio of 100:0.3, and mixing the powder in a mixer for 3 hours to obtain the Cu-Zr alloy powder.
And weighing WC and Cu-Zr alloy powder to ensure that the weight ratio of the WC to the Cu-Zr alloy powder is 5:95, and mixing the powder for 5 hours in a mixer to obtain mixed powder I.
And weighing WC and Cu-Zr alloy powder to enable the weight ratio of the WC to the Cu-Zr alloy powder to be 3:97, and mixing the powder in a mixer for 3 hours to obtain mixed powder II.
Weighing Cu-Zr alloy powder and marking as mixed powder III.
(3) And respectively filling the mixed powder I, the mixed powder II and the mixed powder III into three annular spaces to ensure that the content of WC in the mixed powder is in gradient decreasing distribution from the outer annular space to the inner annular space, then drawing out the partition plate, and vibrating for 40s, rolling for 5min and reversely upsetting for 4 times.
(II) pressing
And (3) pressing the gradient mixed powder obtained in the step (I) by using a cold isostatic press, wherein the pressing pressure is 220MPa, and the pressing time is 7.5min, so that the annular gradient blank is obtained.
(III) sintering
Sintering the blank obtained in the step (II) with the sintering vacuum degree of 1 multiplied by 10-2Pa, the gas content in the composite material is effectively reduced by vacuum sintering, the density of the composite material is favorably improved, the temperature of the vacuum sintering is 1020 ℃, the time of the vacuum sintering is 2.5h, and the consumable electrode of the copper-based composite material is obtained.
(IV) melting
And (3) putting the consumable electrode of the copper-based composite material obtained in the step (three) into a vacuum consumable electric arc furnace, vacuumizing the vacuum consumable electric arc furnace after a furnace door is closed, then filling protective gas helium, and smelting in the vacuum consumable electric arc furnace at the smelting current of 3000A and the smelting voltage of 25V, dropping the consumable electrode into a water-cooled copper crucible after the consumable electrode is molten under the action of an electric arc, quickly solidifying into an ingot, and obtaining the copper-based composite material at the arc stabilizing current of 9A.
Examples 7 to 16
Examples 7 to 16 differ from example 3 only in that the reinforcing material or the copper substrate was different, and the remaining steps were the same as those of example 3 and examples 7 to 16 shown in Table 1.
TABLE 1 reinforcing materials and copper substrates for example 3 and examples 7-16
Reinforcing material Copper base material
Example 3 Al2O3 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 7 ZrO2 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 8 TiO2 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 9 TiC Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 10 WC Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 11 B4C Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 12 TiB2 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 13 Mo Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:2)
Example 14 Al2O3 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:1)
Example 15 Al2O3 Cu-Ti alloy powder (the mass ratio of Cu powder to Ti powder is 100:5)
Example 16 Al2O3 Cu-Fe alloy powder (the mass ratio of Cu powder to Fe powder is 100:4)
Examples 17 to 20
Examples 17-20 differ from example 2 only in that the reinforcing material or copper substrate is different, and the remaining steps are as shown in table 2 for the reinforcing material and copper substrate of example 2 and examples 17-20.
TABLE 2 arc stabilization Current for examples 17-20 and example 2
Figure BDA0002556098600000111
Figure BDA0002556098600000121
Examples 21 to 28
Examples 21-28 differ from example 3 only in the reinforcing material or copper substrate, and the remaining steps are as shown in table 3 for the reinforcing material and copper substrate of example 3 and examples 21-28.
TABLE 3 ARC STABILIZING CURRENT FOR EXAMPLES 21-28 AND EXAMPLE 3
Arc stabilizing current (A)
Example 3 13
Example 21 5
Example 22 6
Example 23 7
Example 24 8
Example 25 9
Example 26 10
Example 27 11
Example 28 12
Examples 29 to 36
Examples 29-36 differ from example 4 only in the reinforcing material or copper substrate, and the remaining steps are as shown in table 4 for the reinforcing material and copper substrate of example 4 and examples 29-36.
TABLE 4 ARC STABILIZING CURRENT FOR EXAMPLES 29-36 AND EXAMPLE 4
Figure BDA0002556098600000122
Figure BDA0002556098600000131
Examples 37 to 41
Examples 37 to 41 differ from example 4 only in that the reinforcing material or the copper substrate was different, and the remaining steps were the same as those of example 4 and the reinforcing materials and the copper substrates of examples 37 to 41 are shown in Table 4.
TABLE 5 arc stabilization Current for examples 37-41 and example 5
Arc stabilizing current (A)
Example 5 9
Example 37 4
Example 38 5
Example 39 6
Example 40 7
EXAMPLE 41 8
Example 42
The copper-based composite material of example 42 was prepared in the same manner as in example 2 except that the arc stabilizing current was 5A.
Second, the examples of the copper-based composite material of the present invention correspond to the final products of the copper-based composite material production methods examples 1 to 42, respectively.
Third, Experimental example
The copper-based composite material of the above exemplary embodiment was subjected to performance tests, which included electric conductivity, hardness, and friction rate. Specifically, the conductivity is detected according to the GB/T32791-2016 copper and copper alloy conductivity eddy current test method; detecting the hardness according to a GB/T231.1-2009 metal Brinell hardness test method; the detection of the wear resistance is tested by adopting a high-speed current-carrying friction wear testing machine under the following test conditions: the pressure 60N and the current 70A were measured, and the results are shown in Table 6.
TABLE 6 results of performance test of copper-based composite materials of exemplary examples
Material Conductivity/% IACS hardness/HWB Friction rate/mg/m
Example 1: TiC/Cu 50 55 25
Example 2: TiC/Cu 67 83 15
Example 6: WC/Cu-Cr 83 92 12
Example 42: TiC/Cu 65 79 17
(Note: 1) when the substrate is an alloy substrate, such as the Cu-Cr alloy substrate of example 6, the article obtained by melting is subjected to aging treatment at 475 ℃ for 4 hours, and then subjected to conductivity, hardness and current-carrying frictional rate tests. 2) Conductivity, hardness and current carrying friction rate tests were all conducted to measure the maximum end/face of the reinforcing phase content, which in the present example is the outer circumferential surface of the cylinder. )
The conductivity of the sintered pure copper is 75% IACS, and the hardness is 42 HWB; the as-cast pure copper has an electrical conductivity of 99% IACS and a hardness of 51 HWB. . As can be seen from the experimental results in Table 6, the copper-based composite material of the present invention exhibits different properties at the pure copper end and the end having the largest content of the reinforcing phase, and thus can be adapted to the connection requirements in a particular field.

Claims (10)

1. The copper-based composite material is characterized by comprising a reinforcing material and a copper matrix, wherein the copper-based composite material is in a cylinder shape, and the content of the reinforcing material is in gradient distribution from inside to outside along a direction perpendicular to the central axis of the cylinder;
wherein the reinforcing material is a metal oxide, a metal carbide, a metal boride or a refractory metal.
2. Copper-based composite material according to claim 1, characterized in that said gradient profile from the inside to the outside is a gradient increasing from the inside to the outside.
3. Copper-based composite material according to claim 1, characterized in that said columns are cylindrical.
4. Copper-based composite material according to claim 1, characterized in that the maximum content of reinforcing material in the copper-based composite material is 25% by weight.
5. Copper-based composite material according to claim 1, characterized in that the metal oxide is Al2O3、ZrO2、TiO2、MgO、CeO2Or La2O3；
The metal carbide is TiC, WC and B4C or Cr3C2；
The metal boride is CrB2、TiB2Or ZrB2；
The refractory metal is W or Mo.
6. Copper-based composite material according to claim 1, characterized in that the copper matrix is Cu or a copper alloy of Cu with at least one metal of Cr, Zr, Ti and Fe.
7. Copper-based composite material according to claim 6, characterized in that said copper alloy is a Cu-Cr alloy, a Cu-Zr alloy, a Cu-Cr-Zr alloy, a Cu-Ti alloy or a Cu-Fe alloy;
wherein the mass ratio of Cu to Cr in the Cu-Cr alloy is 100: 0.4-1.2;
the mass ratio of Cu to Cr to Zr in the Cu-Cr-Zr alloy is 100: 0.4-1.2: 0.03-0.3;
the mass ratio of Cu to Zr in the Cu-Zr alloy is 100: 0.03-0.3;
the mass ratio of Cu to Ti in the Cu-Ti alloy is 100: 0.5-5;
the mass ratio of Cu to Fe in the Cu-Fe alloy is 100: 0.3-4.
8. The preparation method of the copper-based composite material is characterized by comprising the following steps of:
filling mixed powder containing a reinforcing material and a copper base material into a cylindrical mold provided with an annular partition plate, enabling the content of the reinforcing material in the mixed powder to be distributed in a gradient manner from inside to outside along a direction vertical to the central shaft of the mold, removing the partition plate, and then pressing and sintering to obtain the composite material;
wherein the reinforcing material is a metal oxide, a metal carbide, a metal boride or a refractory metal.
9. The method for producing a copper-based composite material according to claim 8, further comprising the steps of:
and smelting the copper-based composite material blank obtained by sintering as a consumable electrode by a vacuum consumable arc smelting method, wherein a melt formed by melting the consumable electrode in the smelting process vertically drips under the action of electromagnetic force to form a molten pool, the molten pool rotates under the action of the electromagnetic force, and the copper-based composite material blank is obtained after cooling.
10. The method for preparing the copper-based composite material according to claim 8 or 9, wherein the sintering temperature is 950 to 1060 ℃, the sintering time is 1 to 5 hours, and the sintering vacuum degree is 1 x 10-3～1×10-1Pa。
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