CN111145960A - High-strength high-conductivity copper-based composite material and preparation method thereof - Google Patents
High-strength high-conductivity copper-based composite material and preparation method thereof Download PDFInfo
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to the field of metal composite materials, in particular to a high-strength high-conductivity copper-based composite material and a preparation method thereof. The preparation method comprises the following steps: (1) laminating more than two layers of copper foil layers deposited with graphene, and then carrying out hot press molding to prepare a graphene-copper composite material; (2) and (3) applying a pressure of 80-120MPa to the graphene-copper composite material through inert gas at the temperature of 700-900 ℃ to carry out hot isostatic pressing densification treatment. The metal high-strength high-conductivity copper-based layered composite material prepared by the invention has good composite effect, high strength and high conductivity. In addition, the preparation method has short flow and high efficiency, is beneficial to reducing the production cost and saving resources, and is environment-friendly and convenient for popularization and application.
Description
Technical Field
The invention relates to the field of metal composite materials, in particular to a high-strength high-conductivity copper-based composite material and a preparation method thereof.
Background
With the rapid development of modern industrial fields, the requirements of the industrial fields such as aerospace, traffic, mechanical industry, energy and chemical industry, communication, electrical, power electronics, national defense and the like on the electrical conductivity and mechanical properties of copper or copper alloy are higher and higher. In order to obtain high-strength and high-conductivity materials, high-strength and high-conductivity copper alloy materials and composite materials such as Cu-Ag, Cu-Al, Cu-Cr-Fe and the like have been developed at home and abroad scientific circles. However, most of the developed materials are remained in the experimental stage, and cannot be widely applied due to the problems of high cost of production raw materials, complex processing and preparation process and the like. The demand of copper alloy or composite material thereof with excellent high-strength conductivity and preparation technology in various large industrial fields is more and more urgent.
Graphene is a carbonaceous material with a monolayer two-dimensional honeycomb lattice structure formed by closely packing sp2 hybridized carbon atoms, has excellent comprehensive performance, and has the advantages of 125Gpa of tensile strength, 1.0Tpa of elastic modulus, 5300W/(m.k) of thermal conductivity and 2 x 105cm2 (v.s) of electron mobility, so that the graphene is often used as an ideal filler for preparing a composite material.
The research and development of the existing graphene-copper composite material mostly focuses on the improvement of the electrical conductivity, and neglects the improvement of the mechanical property of the graphene-copper composite material to cause the unsatisfactory subsequent forming and processing properties of the graphene-copper composite material, so that the application bottleneck of the high-strength high-conductivity copper-based composite material is formed; meanwhile, the existing preparation method inevitably brings in nickel impurities, and influences the chemical components and the microstructure of the high-strength and high-conductivity copper-based composite material, thereby influencing the comprehensive performance of the composite material.
In addition, CN106548831A discloses a method for preparing a graphene-copper composite wire, in which a copper strip coated with a graphene film is wound on a copper rod and placed in a copper sheath to obtain a pre-assembled body; and carrying out hot extrusion on the pre-assembled body to obtain the graphene copper rod. Although the obtained material has certain strength, the strength of the material is mostly determined by the strength of the copper rod, and the graphene has low component ratio in the whole material, so that the comprehensive strength is not greatly improved, and the conductivity of the material is also slightly improved. Meanwhile, the purity of the generated graphene is low by a method of firstly generating the graphene oxide and then adding the reducing agent to convert the graphene oxide into the graphene, and a large amount of the graphene oxide is not reduced and is left on the surface of the copper strip, so that the conductivity of the material is further influenced. The special strong acid oxidation preparation process causes the graphene sheet layers to have more defects and more functional groups, and the conduction of electrons and phonons is influenced, thereby causing the reduction of the electric and heat conductivity of the material.
Disclosure of Invention
In order to solve the technical problems, the invention firstly provides a preparation method of a high-strength high-conductivity copper-based composite material with good composite effect, which comprises the following steps:
(1) taking a copper foil deposited with graphene as a unit material, laminating more than two layers of copper foils deposited with graphene on the unit material, and then carrying out hot press molding to prepare a graphene-copper composite material;
(2) and (3) applying a pressure of 80-120MPa (preferably 90-110MPa) to the graphene-copper composite material by inert gas at the temperature of 700-900 ℃ to carry out hot isostatic pressing densification treatment.
The invention finds that the hot-pressing molding is carried out firstly, and then the hot isostatic pressing densification treatment is carried out under the specific condition, so that the performance advantages of the copper foil and the graphene are well exerted, a good electron exchange migration channel is formed in the composite material, and the composite material also has good advantages in strength.
Preferably, when the thickness of the copper foil is 20-50 μm and the graphene is single-layer graphene, the combination of the above methods can further improve the comprehensive performance of the material.
Preferably, the graphene is grown and deposited on the surface of the copper foil by a CVD method.
Preferably, the graphene is deposited to form graphene layers, and the graphene layer of one unit material is disposed in contact with the copper foil of the other unit material during the lamination.
In order to further improve the effect of hot isostatic pressing densification treatment, the temperature of hot press molding is preferably 500-900 ℃, the pressure is preferably 10-30MPa, and the dwell time is preferably 3-10 min.
As a preferable technical scheme, the temperature of the hot-press forming is 700 ℃, the pressure is 20MPa, and the pressure maintaining time is 8 min.
Preferably, in the hot press forming, when the degree of vacuum is less than 1.0-1After Pa, the temperature was raised to 500-900 ℃. Preferably, in the hot isostatic pressing densification treatment, the dwell time is 1 to 3 hours.
Preferably, the inert gas is argon.
Preferably, after the hot isostatic pressing densification treatment is finished, the prepared semi-finished product is cooled to room temperature along with the furnace under the inert gas environment.
In some embodiments, the preparation method further comprises processing the graphene-copper composite into a plate, a strip or a wire after hot press forming, and then performing the hot isostatic pressing densification treatment. Thus, the compactness, the conductivity and the mechanical property of the material can be further improved.
The above-described preferred embodiments can be combined by one skilled in the art to provide preferred embodiments of the present invention.
The invention further provides the copper-based composite material prepared by the preparation method.
The invention has the following beneficial effects:
(1) the metal high-strength high-conductivity copper-based layered composite material prepared by the invention has good composite effect, high strength and high conductivity.
(2) The preparation method has the advantages of short flow, high efficiency, contribution to reducing the production cost and saving resources, environmental friendliness and convenience for popularization and application.
Drawings
FIG. 1 is a flow chart of the preparation process in example 1.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
In order to compare the influence of the preparation process on the high-strength and high-conductivity copper-based composite material in the invention more intuitively, the copper foil and the graphene used in the following embodiments belong to the same batch, wherein the thickness of the copper foil is 35 +/-2 μm; graphene is a single layer graphene.
Example 1
The embodiment provides a copper-based composite material, and the specific preparation method is as follows (see the flow chart in fig. 1):
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 700 ℃, pressing the composite material at 700 ℃ under the pressure of 20MPa for 8min, and pressing to obtain the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 90Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Example 2
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 100 Mpa.
Example 3
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 110 Mpa.
Example 4
This example provides a copper-based composite material, which is prepared by the following steps: the temperature in step (2) was 800 ℃.
Example 5
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 100 Mpa.
Example 6
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 110 Mpa.
Example 7
This example provides a copper-based composite material, which is prepared by the following steps: the temperature in step (2) was 900 ℃.
Example 8
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 100 Mpa.
Example 9
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (2) is 110 Mpa.
Example 10
The embodiment provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 400 ℃, pressing the composite material at 400 ℃ under the pressure of 20MPa for 8min, and pressing to obtain the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 90Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Example 11
The embodiment provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 300 ℃, pressing the material at 300 ℃ under the pressure of 20MPa for 8min, and pressing to form the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 90Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Example 12
The embodiment provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 700 ℃, pressing the composite material at the temperature of 700 ℃ under the pressure of 40MPa for 8min, and pressing to form the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 90Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Example 13
The embodiment provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 700 ℃, pressing the composite material at 700 ℃ under the pressure of 5MPa for 8min, and pressing to obtain the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 90Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Comparative example 1
The comparative example provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1After 0Pa, the temperature is raised to 700 ℃, and the composite material is pressed into the composite material to be processed under the pressure of 5MPa and the pressure for 8min at the temperature of 700 ℃. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 800 ℃, pumping argon (i.e. pressure transmission medium) to 80Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Comparative example 2
The comparative example provides a copper-based composite material, which is prepared by the following steps:
(1) laminating 30 high-orientation metal copper foils with single-layer graphene grown by CVD method in a stacking hot-pressing mode by using a vacuum hot-pressing furnace, and when the vacuum degree is lower than 1.0-1And after Pa, heating to 700 ℃, pressing the composite material at 700 ℃ under the pressure of 5MPa for 8min, and pressing to obtain the composite material to be processed. The copper foil deposited with graphene is used as a unit material, and when the unit materials are stacked, the graphene layer of one unit material is in contact with the copper foil of the other unit material.
(2) Putting the composite material to be processed into a ceramic sheath, placing the ceramic sheath in a hot-pressing sintering furnace of a high-pressure container with hot isostatic pressure, sealing the pressure container, heating the inside of the container to 700 ℃, pumping argon (namely a pressure transmission medium) to 130Mpa, and maintaining the pressure for 3 hours;
(3) and (5) after the hot pressing is finished, cooling the processing material to room temperature along with the furnace in the inert gas environment.
Test examples
The test examples were conducted to examine the properties of the copper-based layered composite materials in the examples and comparative examples.
The detection method comprises the following steps: taking a compression-molded sample, preparing the compression-molded sample into a test standard sample, and detecting the tensile strength, the specified plastic elongation strength, the actual compression force, the Vickers hardness and the conductivity, wherein the detection results are shown in tables 1-2 below.
Wherein the detection method of the tensile strength Rm and the specified plastic elongation strength Rp0.2 refers to GB/T228.1-2010
The detection method of the actual compression force refers to GB/T7314-;
the detection method of Vickers hardness HV0.2 refers to 4340.1-2009;
the conductivity detection adopts a four-probe detection method.
TABLE 1
TABLE 2
From the result, the copper-based-graphene composite material in the embodiment of the invention has high conductivity and excellent mechanical property.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a copper-based composite material is characterized by comprising the following steps:
(1) taking the copper foil deposited with the graphene as a unit material, laminating more than two layers of unit materials, and then carrying out hot press molding to prepare a graphene-copper composite material;
(2) and (3) applying a pressure of 80-120MPa to the graphene-copper composite material through inert gas at the temperature of 700-900 ℃ to carry out hot isostatic pressing densification treatment.
2. The preparation method according to claim 1, wherein the copper foil has a thickness of 20 to 50 μm, and the graphene is single-layer graphene; the graphene is preferably grown and deposited on the surface of the copper foil by a CVD method.
3. The method according to claim 1 or 2, wherein the graphene is deposited to form graphene layers, and the graphene layers of one of the unit materials are disposed in contact with the copper foil of the other unit material during the lamination.
4. The preparation method according to any one of claims 1 to 3, wherein the hot press forming temperature is 500 ℃ and 900 ℃, the pressure is 10 to 30MPa, and the dwell time is 3 to 10 min.
5. The production method according to any one of claims 1 to 4, wherein, in the hot press forming, when the degree of vacuum is less than 1.0-1After Pa, the temperature was raised to 500-900 ℃.
6. The production method according to any one of claims 1 to 5, wherein in the hot isostatic compaction treatment, a dwell time is 1 to 3 hours.
7. The method according to any one of claims 1 to 6, wherein the inert gas is argon.
8. The preparation method according to any one of claims 1 to 7, wherein after the hot isostatic pressing densification treatment is finished, the prepared semi-finished product is furnace-cooled to room temperature in an inert gas environment.
9. The preparation method according to any one of claims 1 to 8, further comprising processing the graphene-copper composite material into a plate, a strip or a wire after hot press forming, and then performing the hot isostatic pressing densification treatment.
10. The copper-based composite material prepared by the preparation method of any one of claims 1 to 9.
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| CN111844953A (en) * | 2020-06-12 | 2020-10-30 | 中车工业研究院有限公司 | High-strength high-conductivity copper-based composite material and preparation method thereof |
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| WO2022081113A1 (en) * | 2020-10-14 | 2022-04-21 | Atatürk Üni̇versi̇tesi̇ Bi̇li̇msel Araştirma Projeleri̇ Bi̇ri̇mi̇ | Method and system for production of layered cu-graphene ultra conductor wire |
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| CN113954461A (en) * | 2021-10-29 | 2022-01-21 | 松山湖材料实验室 | Graphene reinforced copper-aluminum laminated composite material and preparation method thereof |
| CN114213706A (en) * | 2021-12-02 | 2022-03-22 | 北京石墨烯技术研究院有限公司 | Graphene composite material, preparation method thereof, heat dissipation member and electronic device |
| CN114388167A (en) * | 2022-01-18 | 2022-04-22 | 远东电缆有限公司 | Graphene copper wire, preparation method thereof and cable |
| CN114388167B (en) * | 2022-01-18 | 2024-01-26 | 远东电缆有限公司 | Graphene copper wire, preparation method thereof and cable |
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| CN114474897A (en) * | 2022-01-26 | 2022-05-13 | 重庆墨希科技有限公司 | Large-scale production method and device of high-conductivity graphene metal composite material |
| CN115652129A (en) * | 2022-11-01 | 2023-01-31 | 合肥工业大学 | Preparation method of Cu-graphene laminated composite material |
| CN115652129B (en) * | 2022-11-01 | 2024-03-19 | 合肥工业大学 | Preparation method of Cu-graphene lamellar composite material |
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