CN111844953A - High-strength high-conductivity copper-based composite material and preparation method thereof - Google Patents
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- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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- 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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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) the method comprises the following steps of taking a copper foil deposited with graphene as a unit material, firstly stacking more than two layers of unit materials, then placing the unit materials into a ceramic tool, then coating a metal sheath on the outer surface of the ceramic tool, and packaging the unit materials by vacuumizing so that the metal sheath is tightly coated on the outer surface of the ceramic tool; (2) and applying pressure of 90-200MPa to the encapsulated composite material through inert gas at 800-1000 ℃ to perform hot isostatic pressing densification treatment. The copper-based composite material prepared by the preparation method has the advantages of good composite effect, high density, high forming rate, high strength and high conductivity. Meanwhile, the preparation method further reduces the working procedures, improves the processing efficiency, and is more beneficial to reducing the production cost and saving resources.
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
The existing processing technology of the raw material of the graphene-copper composite material is mature continuously, but a plurality of problems exist in the processing and preparation of a formed workpiece.
For example, CN108145169A and CN110157932A both refer to a powder forming method, but the pores inside the compact formed by pressing the powder cannot be completely eliminated, which easily results in insufficient internal compactness of the product and further adversely affects the electrical conductivity of the product. Meanwhile, the method also has the problems of long production process, complicated working procedures, high production cost and the like.
CN111145960A proposes a preparation method, in which two or more layers of copper foil with deposited graphene are stacked and then hot-pressed to form, and then hot isostatic pressing densification is performed, so as to solve the problems caused by the above grinding and forming method to a greater extent. However, the mechanical hot pressing method is easy to cause the problems of adhesion between the hot-pressed copper foil and the gasket, copper foil deformation and the like, so that the copper foil is irregularly stacked and formed, the process efficiency is greatly reduced, and the size of the shape of the workpiece is limited.
Therefore, it is desirable to provide a more superior graphene-copper composite material and a method for preparing a finished workpiece thereof.
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 and high molding efficiency, which comprises the following steps:
(1) the method comprises the following steps of taking a copper foil deposited with graphene as a unit material, firstly stacking more than two layers of unit materials, then placing the unit materials into a ceramic tool, then coating a metal sheath on the outer surface of the ceramic tool, and packaging the unit materials by vacuumizing so that the metal sheath is tightly coated on the outer surface of the ceramic tool;
(2) and applying pressure of 90-200MPa to the encapsulated composite material through inert gas at 800-1000 ℃ to perform hot isostatic pressing densification treatment.
In the field, ceramic tools are generally used in hot pressing, and the invention finds that the process can be reduced and the problems of adhesion between copper foil and gasket, copper foil deformity and the like can be avoided after the ceramic tools are used in the hot isostatic pressing densification treatment in the manner. In addition, the method is also beneficial to pressure stabilization, and the density of the pressed finished graphene-copper composite material is improved by 10-20% compared with the density of the process without the ceramic tool, and the corresponding electric conductivity is improved by 2-10%.
Preferably, in the step (1), when the thickness of the copper foil is 20-100 μm and the graphene is single-layer graphene, the performance of the graphene-copper composite material is better.
Graphene is preferably grown and deposited on the surface of the copper foil by chemical vapor deposition.
Preferably, in the step (1), the graphene layer of one of the unit materials is provided in contact with the copper foil of the other unit material at the time of the lamination.
Preferably, in the step (1), the ceramic tool is pressed in a manner that: radial pressureless and axial pressuring.
Preferably, in the step (1), when the unit materials are laminated by 20-50 layers, the composite effect of the materials can be ensured, the structural stability and uniformity of the materials can be favorably maintained, and the performance of the composite materials in all aspects can be further favorably improved. Within the above range, when the number of laminations is increased, it is necessary to appropriately increase the pressure (within 90 to 200 MPa) at the time of the hot isostatic pressing densification treatment.
Preferably, in the hot isostatic compaction process, a pressure of 140MPa to 200MPa is applied.
Preferably, in the step (1), the metal sheath is a stainless steel sheath.
Preferably, in step (1), the degree of vacuum in the metal sheath is less than 1X 10 -1And packaging is started after Pa.
Preferably, the ceramic tool and the stainless steel sheath are processed in a 3D printing mode.
Preferably, in the step (2), the time of the hot isostatic pressing densification treatment is 1-3 h.
Preferably, in step (2), the inert gas is argon.
Preferably, after the hot isostatic pressing densification treatment is finished, the manufactured finished workpiece is cooled to room temperature along with the furnace in an inert gas environment and then taken out.
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 a copper-based composite material prepared by the preparation method.
The invention has the following beneficial effects:
(1) the metal high-strength high-conductivity graphene-copper finished product material prepared by the invention has the advantages of good compounding effect, high density, high forming rate, high strength and high conductivity.
(2) The preparation method further reduces the working procedures, improves the processing efficiency, is more favorable for reducing the production cost and saving resources, and is environment-friendly and convenient 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.
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 50 +/-5 μm; graphene is a single layer graphene.
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.
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) stacking 50 layers of copper foil with graphene deposited in a chemical vapor phase manner, and then putting the copper foil into a hot isostatic pressing ceramic tool which is processed in advance;
(2) carrying out metal sheathing on the ceramic tool with the graphene copper foil, and carrying out vacuumizing and sealing treatment;
(3) and (3) performing hot isostatic pressing densification (HIP) by applying 100MPa pressure to the graphene-copper composite materials (1) and (2) through inert gas at 800 ℃.
According to statistics, the forming rate of the preparation method is 92.5%.
Example 2
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (3) is 120 Mpa.
According to statistics, the forming rate of the preparation method is 95.2%.
Example 3
This example provides a copper-based composite material, which is prepared by the following steps: the temperature in step (3) was 900 ℃.
According to statistics, the forming rate of the preparation method is 95.6%.
Example 4
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (3) is 120 Mpa.
According to statistics, the forming rate of the preparation method is 95.8%.
Example 5
This example provides a copper-based composite material, which is prepared by the following steps: the temperature in step (3) was 1000 ℃.
According to statistics, the forming rate of the preparation method is 96.4%.
Example 6
This example provides a copper-based composite material, which is prepared by the following steps: the pressure in the step (3) is 120 Mpa.
According to statistics, the forming rate of the preparation method is 98.5%.
Example 7
This example provides a copper-based composite material, which is prepared by the following steps: in the step (3), the temperature is 1000 ℃ and the pressure is 200 MPa.
According to statistics, the forming rate of the preparation method is 98.2%.
Example 8
This example provides a copper-based composite material, which is prepared by the following steps: in the step (3), the temperature is 800 ℃ and the pressure is 140 MPa.
According to statistics, the forming rate of the preparation method is 99.1%.
Example 9
This example provides a copper-based composite material, which is prepared by the following steps: in the step (3), the temperature is 900 ℃ and the pressure is 170 MPa.
According to statistics, the forming rate of the preparation method is 99.3%.
Comparative example 1
This comparative example provides a copper-based composite material, which was prepared in the same manner as in example 1 of CN 111145960A.
According to statistics, the forming rate of the preparation method is 62.1%.
Comparative example 2
This comparative example provides a copper-based composite material, which was prepared by a process different from that of example 1: except that the heating temperature was 600 ℃ and the pressure was 80 MPa.
According to statistics, the forming rate of the preparation method is 13.0%.
Comparative example 3
This comparative example provides a copper-based composite material, which was prepared by a process different from that of example 1: except that the heating temperature was 1100 deg.C and the pressure was 80 MPa.
According to statistics, the forming rate of the preparation method is 50.4%.
Comparative example 4
This comparative example provides a copper-based composite material, which was prepared by a process different from that of example 1: except that the heating temperature was 600 deg.c and the pressure was 210 MPa.
According to statistics, the forming rate of the preparation method is 15.7%.
Comparative example 5
This comparative example provides a copper-based composite material, which was prepared by a process different from that of example 1: except that the heating temperature was 1100 deg.c and the pressure was 210 MPa.
According to statistics, the forming rate of the preparation method is 40.2%.
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) the method comprises the following steps of taking a copper foil deposited with graphene as a unit material, firstly stacking more than two layers of unit materials, then placing the unit materials into a ceramic tool, then coating a metal sheath on the outer surface of the ceramic tool, and packaging the unit materials by vacuumizing so that the metal sheath is tightly coated on the outer surface of the ceramic tool;
(2) and applying pressure of 90-200MPa to the encapsulated composite material through inert gas at 800-1000 ℃ to perform hot isostatic pressing densification treatment.
2. The preparation method according to claim 1, wherein in the step (1), the copper foil has a thickness of 20 to 100 μm, and the graphene is single-layer graphene; graphene is preferably grown and deposited on the surface of the copper foil by chemical vapor deposition.
3. The production method according to claim 1 or 2, characterized in that in step (1), the graphene layer of one of the unit materials is disposed in contact with the copper foil of the other unit material at the time of the lamination.
4. The preparation method according to any one of claims 1 to 3, wherein in the step (1), the ceramic tool is pressed in a manner that: radial pressureless and axial pressuring.
5. The production method according to any one of claims 1 to 4, wherein in the step (1), the unit material is laminated by 20 to 50 layers.
6. The method according to any one of claims 1 to 5, wherein in the step (1), the metal sheath is a stainless steel sheath.
7. The method according to any one of claims 1 to 6, wherein in the step (1), the degree of vacuum in the metal casing is less than 1 x 10-1And packaging is started after Pa.
8. The production method according to any one of claims 1 to 7, wherein in the step (2), the hot isostatic pressing densification treatment is performed for 1 to 3 hours.
9. The method according to any one of claims 1 to 8, wherein in the step (2), the inert gas is argon; preferably, after the hot isostatic pressing densification treatment is finished, the manufactured finished workpiece is cooled to room temperature along with the furnace in an inert gas environment and then taken out.
10. A copper-based composite material characterized by being produced by the production method according to any one of claims 1 to 9.
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CN108672249A (en) * | 2018-04-04 | 2018-10-19 | 北京石墨烯技术研究院有限公司 | A kind of anisotropic graphite alkene composite material and preparation method thereof |
CN109735826A (en) * | 2019-02-14 | 2019-05-10 | 中车工业研究院有限公司 | A kind of graphene/copper composite material and its preparation method and application |
CN111145960A (en) * | 2019-12-19 | 2020-05-12 | 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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CN105000891A (en) * | 2015-06-01 | 2015-10-28 | 北京控制工程研究所 | MnCoNi oxide ceramic infrared sensitive element densifying method |
CN108672249A (en) * | 2018-04-04 | 2018-10-19 | 北京石墨烯技术研究院有限公司 | A kind of anisotropic graphite alkene composite material and preparation method thereof |
CN109735826A (en) * | 2019-02-14 | 2019-05-10 | 中车工业研究院有限公司 | A kind of graphene/copper composite material and its preparation method and application |
CN111145960A (en) * | 2019-12-19 | 2020-05-12 | 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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