CN112322922A - Powder metallurgy preparation method of dispersion copper-copper laminated composite material - Google Patents

Powder metallurgy preparation method of dispersion copper-copper laminated composite material Download PDF

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CN112322922A
CN112322922A CN202011273666.6A CN202011273666A CN112322922A CN 112322922 A CN112322922 A CN 112322922A CN 202011273666 A CN202011273666 A CN 202011273666A CN 112322922 A CN112322922 A CN 112322922A
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powder
copper
layer
sintering
compaction
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CN112322922B (en
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郑顺奇
郑阳升
贺勇
汪祥余
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China Weapon Science Academy Ningbo Branch
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China Weapon Science Academy Ningbo Branch
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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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/001Non-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
    • C22C32/0015Non-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
    • C22C32/0021Matrix based on noble metals, Cu or alloys thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C2204/00End product comprising different layers, coatings or parts of cermet

Abstract

The invention discloses a powder metallurgy preparation method of a dispersed copper-copper laminated composite material, which comprises the following steps: (1) preparing raw materials: the raw materials are copper powder and internal oxidation Cu-Al2O3And (3) pulverizing. (2) Cold-press forming: a cold-pressing die is adopted, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu-Al is laid2O3Powder ofCompacting; and so on. (3) And (3) sintering: sintering the cold pressed compact in vacuum or reducing atmosphere at 800-1050 ℃ for 0.5-6 h. The method can improve the plastic deformation capability of the aluminum oxide dispersion strengthened copper material, simultaneously keep the good electric conduction and heat conduction performance of the aluminum oxide dispersion strengthened copper material, and solve the problem that the material is applied to Al2O3When the content is high, cracks are likely to occur during the deformation.

Description

Powder metallurgy preparation method of dispersion copper-copper laminated composite material
Technical Field
The invention belongs to the field of metal matrix composite materials. In particular to a powder metallurgy preparation method of a dispersion copper-copper laminated composite material.
Background
The aluminum oxide particle reinforced copper material has the characteristics of good strength, electrical conductivity, thermal conductivity and the like. Due to Al2O3The wettability of the particles and the copper matrix is poor, and Al is adopted2O3The composite material prepared by the powder metallurgy preparation method by mixing the particles and the copper powder has poor performance. Therefore, the aluminum oxide particle reinforced copper material is generally prepared by adopting an internal oxidation method with higher cost and more complex process. Al material obtained by internal oxidation method2O3The copper material has fine and dispersed particles, uniform distribution and good performance, is called as a dispersed copper material, and can be used in the fields of electrode materials, electrical contact materials, lead frames and other various electrical engineering. But the material is in Al2O3When the content is higher, the plastic forming capability is poorer, cracks are easy to generate in the deformation processes of extrusion, rolling and the like, and in order to ensure that the composite material has good deformation capability and simultaneously keep good electric and heat conduction characteristics, the composite material is improved in a layered composite mode.
Disclosure of Invention
The invention aims to solve the problem that the aluminum oxide dispersion strengthened copper material is in Al in the prior art2O3When the content is higher, the plastic formability is poorer, and cracks are easy to generate in the deformation processes of extrusion, rolling and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
(1) preparing raw materials: the raw materials are copper powder and internal oxidation Cu-Al2O3And (3) pulverizing. The copper powder includes electrolytic copper powder or atomized copper powder, Cu-Al2O3Al in powder2O3The proportion of (B) is 1-4%.
(2) Cold-press forming: a flat-bottom cold-pressing die is adopted, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu is laid-Al2O3Powder and compaction; and so on until the desired thickness is reached.
(3) Hot-pressing and sintering: and hot-pressing and sintering the cold-pressed compact in vacuum or reducing atmosphere at the sintering temperature of 800-1050 ℃ for 0.5-6 h.
Preferably, Cu-Al in step (1)2O3The powder is prepared by the following method: preparing Cu-Al alloy powder by an atomization powder preparation method, wherein the mass fraction of Al is 0.5-2.2%. Oxidizing Cu-Al alloy powder in an air furnace at the temperature of 250-450 ℃ for 40-60h to obtain CuO-Al2O3And (3) powder. Then the alloy powder is kept warm for 3-5h in a nitrogen atmosphere furnace with the temperature of 650 plus 900 ℃ to prepare Cu2O-Al2O3And (3) powder. Then preserving the heat for 1 to 4 hours in a hydrogen atmosphere furnace with the temperature of 700-900 ℃, and reducing excessive oxygen to obtain Cu-Al2O3And (3) powder.
Preferably, the compaction pressure in step (2) is 100-300 MPa.
Preferably, in step (2), the thickness of each layer after compaction is between 0.5 and 3mm, and the thicknesses of the two components are not necessarily the same.
Preferably, in the step (3), hot-pressing sintering or plasma sintering can be adopted, and the sintering pressure is 20-70 MPa.
Preferably, in the step (3), pressureless sintering can also be adopted, and rolling or extrusion is carried out after sintering to improve the density.
Compared with the prior art, the invention has the beneficial effects that:
the invention is prepared by mixing Al2O3The mode of forming the layered composite material by dispersing copper and copper improves Al2O3The deformability of the dispersed copper material is maintained, and the good electric and heat conducting properties of the dispersed copper material are maintained. The material can be used in the electrical engineering fields of electrical contacts, electrodes, lead frames and the like.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
A powder metallurgy preparation method of a dispersion copper-copper laminated composite material comprises the following steps:
(1) preparing raw materials: the raw materials are electrolytic copper powder and internal oxidation Cu-Al2O3And (3) pulverizing.
Wherein Cu-Al2O3The powder is prepared by the following method: 100-200-mesh water is adopted to atomize Cu-Al alloy powder, wherein the mass fraction of Al is 1 percent. Oxidizing Cu-Al alloy powder in an air furnace at the temperature of 300 ℃ for 40h to obtain CuO-Al2O3And (3) powder. Then keeping the alloy powder in a nitrogen atmosphere furnace at 800 ℃ for 3h to prepare Cu2O-Al2O3Powder is then preserved for 3 hours in a hydrogen atmosphere furnace at 800 ℃ to reduce excessive oxygen to obtain Cu-1.9 percent Al2O3And (3) powder.
(2) Cold-press forming: adopting a flat-bottom cold-pressing die, and alternately spreading electrolytic copper powder and Cu-Al2O3Powder is compacted under the pressure of 200MPa, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu-Al is laid2O3Powder and compaction; by analogy, 11 layers are paved, and the thickness of each layer after compaction is 1 mm.
(3) And (3) sintering: placing the cold pressed blank in H2Hot-pressing and sintering in the atmosphere, wherein the sintering pressure is 50MPa, the temperature is 1000 ℃, and the time is 2 hours, so that the dispersed copper-copper laminated composite material is obtained.
In this example, the elongation of the dispersed copper-copper laminated composite material was 6.2%, while the elongation of the dispersed copper of the same composition not laminated with the copper layer was 3.5%. The method can improve the plastic deformation capability of the aluminum oxide dispersion strengthened copper material, simultaneously keep the good electric conduction and heat conduction performance of the aluminum oxide dispersion strengthened copper material, and solve the problem that the material is applied to Al2O3When the content is high, cracks are likely to occur during the deformation.
Example two
A powder metallurgy preparation method of a dispersion copper-copper laminated composite material comprises the following steps:
(1) preparing raw materials: the raw materials are electrolytic copper powder and internal oxidation Cu-Al2O3And (3) pulverizing.
Wherein Cu-Al2O3The powder is prepared by the following method: 100-200-mesh water is adopted to atomize Cu-Al alloy powder, wherein the mass fraction of Al is 0.5 percent. Oxidizing Cu-Al alloy powder in an air furnace at the temperature of 300 ℃ for 40h to obtain CuO-Al2O3And (3) powder. Then the alloy powder is kept warm for 2h in a nitrogen atmosphere furnace at 800 ℃ to prepare Cu2O-Al2O3Powder is then preserved for 3 hours in a hydrogen atmosphere furnace at 800 ℃ to reduce excessive oxygen to obtain Cu-0.94 percent Al2O3And (3) powder.
(2) Cold-press forming: adopting a flat-bottom cold-pressing die, and alternately spreading electrolytic copper powder and Cu-Al2O3Powder is compacted under the compaction pressure of 100MPa, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu-Al is laid2O3Powder and compaction; by analogy, 11 layers are paved, and the thickness of each layer after compaction is 2 mm.
(3) And (3) sintering: and hot-pressing and sintering the cold pressed compact in a reducing atmosphere at the sintering pressure of 50MPa and the temperature of 1000 ℃ for 2 hours to obtain the dispersed copper-copper laminated composite material.
In this example, the elongation of the dispersed copper-copper laminated composite material was 12.8%. While the elongation of the same composition dispersed copper not composited with the copper layer was 8.7%. The method can improve the plastic deformation capability of the aluminum oxide dispersion strengthened copper material, simultaneously keep the good electric conduction and heat conduction performance of the aluminum oxide dispersion strengthened copper material, and solve the problem that the material is applied to Al2O3When the content is high, cracks are likely to occur during the deformation.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
EXAMPLE III
A powder metallurgy preparation method of a dispersion copper-copper laminated composite material comprises the following steps:
(1) preparing raw materials: the raw materials are electrolytic copper powder and internal oxidation Cu-Al2O3And (3) pulverizing. Wherein Cu-Al2O3The powder is prepared by the following method: 100-200-mesh water is adopted to atomize Cu-Al alloy powder, wherein the mass fraction of Al is 2.2 percent. Oxidizing Cu-Al alloy powder in an air furnace at the temperature of 300 ℃ for 40h to obtain CuO-Al2O3And (3) powder. Then keeping the alloy powder in a nitrogen atmosphere furnace at 800 ℃ for 3h to prepare Cu2O-Al2O3Powder is then preserved for 3 hours in a hydrogen atmosphere furnace at 800 ℃ to reduce excessive oxygen to obtain Cu-4% Al2O3And (3) powder.
(2) Cold-press forming: adopting a flat-bottom cold-pressing die, and alternately spreading electrolytic copper powder and Cu-Al2O3Powder is compacted under the pressure of 200MPa, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu-Al is laid2O3Powder and compaction; by analogy, 11 layers are paved, and the thickness of each layer after compaction is 0.5 mm.
(3) And (3) sintering: and (3) performing vacuum plasma sintering on the cold-pressed blank, wherein the sintering pressure is 30MPa, the temperature is 950 ℃, and the time is 0.5 hour, so that the dispersed copper-copper laminated composite material is obtained.
In this example, the elongation of the dispersed copper-copper laminated composite material was 4.2%, while the elongation of the dispersed copper of the same composition not laminated with the copper layer was 1.8%. The method can improve the plastic deformation capability of the aluminum oxide dispersion strengthened copper material, simultaneously keep the good electric conduction and heat conduction performance of the aluminum oxide dispersion strengthened copper material, and solve the problem that the material is applied to Al2O3When the content is high, cracks are likely to occur during the deformation.

Claims (6)

1. A powder metallurgy preparation method of a dispersed copper-copper laminated composite material is characterized by comprising the following steps:
(1) Preparing raw materials: the raw materials are copper powder and internal oxidation Cu-Al2O3And (3) pulverizing. The copper powder includes electrolytic copper powder or atomized copper powder, Cu-Al2O3Al in powder2O3The proportion of (B) is 1-4%.
(2) Cold-press forming: a flat-bottom cold-pressing die is adopted, and a layer of copper powder is firstly paved and compacted; then a layer of Cu-Al is laid2O3Powder and compaction; then spreading a layer of copper powder and compacting; then a layer of Cu-Al is laid2O3Powder and compaction; and so on until the desired thickness is reached.
(3) And (3) sintering: sintering the cold pressed compact in vacuum or reducing atmosphere at 800-1050 ℃ for 0.5-6 h.
2. The method of claim 1, wherein: Cu-Al in step (1)2O3The powder is prepared by the following method: preparing Cu-Al alloy powder by an atomization powder preparation method, wherein the mass fraction of Al is 0.5-2.2%. Oxidizing Cu-Al alloy powder in an air furnace at the temperature of 250-450 ℃ for 40-60h to obtain CuO-Al2O3And (3) powder. Then the alloy powder is preserved for 3-5h in a nitrogen atmosphere furnace with the temperature of 650-900 ℃ to prepare Cu2O-Al2O3And (3) powder. Then preserving the heat for 1 to 4 hours in a hydrogen atmosphere furnace with the temperature of 700-900 ℃, and reducing excessive oxygen to obtain Cu-Al2O3And (3) powder.
3. The method of claim 1, wherein: the compaction pressure in the step (2) is 100-300 MPa.
4. The method of claim 1, wherein: in the step (2), the thickness of each layer after compaction is 0.5-3mm, and the layer thickness of the two components is not necessarily the same.
5. The method of claim 1, wherein: in the step (3), hot-pressing sintering or plasma sintering can be adopted, and the sintering pressure is 20-70 MPa.
6. The method of claim 1, wherein: in the step (3), pressureless sintering can also be adopted, and rolling or extrusion is carried out after sintering to improve the density.
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Cited By (4)

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CN113441724A (en) * 2021-07-07 2021-09-28 燕山大学 Method for preparing aluminum alloy/aluminum-based composite material composite board through powder metallurgy-rolling
CN114309615A (en) * 2021-12-17 2022-04-12 合肥波林新材料股份有限公司 Iron-based double-layer sintered material and preparation method thereof
CN114959343A (en) * 2022-05-30 2022-08-30 河南科技大学 Forging forming method of aluminum oxide dispersion strengthening copper-based composite material and composite blank
CN115502404A (en) * 2022-11-09 2022-12-23 西安理工大学 Method for preparing heterogeneous layered metal material by powder metallurgy

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN113441724A (en) * 2021-07-07 2021-09-28 燕山大学 Method for preparing aluminum alloy/aluminum-based composite material composite board through powder metallurgy-rolling
CN114309615A (en) * 2021-12-17 2022-04-12 合肥波林新材料股份有限公司 Iron-based double-layer sintered material and preparation method thereof
CN114959343A (en) * 2022-05-30 2022-08-30 河南科技大学 Forging forming method of aluminum oxide dispersion strengthening copper-based composite material and composite blank
CN114959343B (en) * 2022-05-30 2024-03-29 河南科技大学 Forging forming method of aluminum oxide dispersion strengthening copper-based composite material and composite blank
CN115502404A (en) * 2022-11-09 2022-12-23 西安理工大学 Method for preparing heterogeneous layered metal material by powder metallurgy
CN115502404B (en) * 2022-11-09 2024-01-19 西安理工大学 Method for preparing heterogeneous layered metal material by powder metallurgy

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