CN111331127A - Preparation method of graphene/copper composite wire - Google Patents

Preparation method of graphene/copper composite wire Download PDF

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Publication number
CN111331127A
CN111331127A CN201811550044.6A CN201811550044A CN111331127A CN 111331127 A CN111331127 A CN 111331127A CN 201811550044 A CN201811550044 A CN 201811550044A CN 111331127 A CN111331127 A CN 111331127A
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China
Prior art keywords
graphene
copper
copper composite
powder
composite wire
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Pending
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CN201811550044.6A
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Chinese (zh)
Inventor
冯雪
杨振
解浩峰
黄国杰
米绪军
彭丽军
尹向前
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GRIMN Engineering Technology Research Institute Co Ltd
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GRIMN Engineering Technology Research Institute Co Ltd
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Priority to CN201811550044.6A priority Critical patent/CN111331127A/en
Publication of CN111331127A publication Critical patent/CN111331127A/en
Pending legal-status Critical Current

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    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F3/20Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/12Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/026Alloys based on copper
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a preparation method of a graphene/copper composite wire, and belongs to the field of composite material processing and preparation. The method comprises the following steps: (1) mixing graphene and copper powder in a solid phase to obtain composite powder; (2) carrying out reduction treatment on the composite powder; (3) preparing a graphene/copper composite material wire blank by adopting a continuous extrusion technology; (4) and preparing the graphene/copper composite wire by adopting a multi-pass cold drawing technology. The method adopts the continuous extrusion technology to prepare the composite material wire blank, realizes the continuous production of the wire blank, simultaneously adopts the multi-pass drawing technology to realize the further dispersion and orientation of the graphene in the copper matrix, and improves the performance of the composite wire. The graphene/copper composite wire prepared by the method has higher electrical conductivity while obviously improving the tensile strength; the method has the advantages of less procedures, continuous production and high production efficiency.

Description

Preparation method of graphene/copper composite wire
Technical Field
The invention relates to a preparation method of a composite material wire, in particular to a preparation method of a graphene/copper composite wire, and belongs to the field of composite material processing and preparation.
Background
With the development of aerospace, mechanical and electronic industries, the demand for cables with light weight, high strength and high conductivity is more and more urgent. The graphene provides possibility for improving the performance of light, high-strength and high-wire cables.
The graphene is a two-dimensional nano material composed of carbon atoms, is a nano material with the highest specific strength in the world, is known at present, has the strength of 130GPa, and is more than 100 times that of steel; the thermal conductivity can reach 5000W/(m.K), which is 3 times of that of diamond; its resistivity is also only about 10n Ω · m. Compared with other nano carbon materials, the graphene has a larger specific surface area and a large contact area with a substrate; although graphene is also agglomerated by van der waals forces, it can slip relatively under external forces, and further dispersion and orientation distribution in the matrix can be achieved during large deformation. Therefore, the graphene is compounded with copper to prepare a light, high-strength and high-wire cable by utilizing the high strength and high conductivity of the graphene, and the requirements of the aerospace and electronic information fields on high-end cables can be expected to be met.
The preparation method of the graphene/copper composite wire comprises a melt casting method and a powder metallurgy method. When a melt casting method is adopted, due to the fact that the density difference between graphene and copper is large, an interface is not wet, and graphene is difficult to uniformly disperse in a copper matrix; when the powder metallurgy method is adopted, a plurality of processes such as hot extrusion after hot-pressing sintering are required, the process is complex, and continuous preparation cannot be realized. Therefore, there is a need to develop a new process for continuously producing graphene/copper composite wires.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a novel method for preparing the graphene/copper composite wire by adopting continuous extrusion and multi-pass drawing, the continuous preparation of the composite material wire blank can be realized by adopting the continuous extrusion technology, and the further dispersion and orientation of the graphene in the copper matrix can be realized by adopting the multi-pass drawing, so that the performance of the wire is improved.
The purpose of the invention can be realized by the following technical scheme:
a continuous preparation method of a graphene/copper composite wire comprises the following steps:
(1) mixing graphene and copper powder in a solid phase to obtain composite powder;
(2) carrying out reduction treatment on the composite powder;
(3) preparing a graphene/copper composite material wire blank by adopting a continuous extrusion technology;
(4) and preparing the graphene/copper composite wire by adopting a multi-pass cold drawing technology.
In the step (1), the addition amount of the graphene is less than 5 wt%, and the addition amount of the graphene is preferably less than 3 wt%; the minimum addition amount of the graphene is preferably more than 0.005 wt%; more preferably from 0.005% to 1% by weight.
In the step (1), the particle size of the copper powder is 50 to 500 μm, and the particle size of the copper powder is preferably 200 to 400 μm.
In the step (1), the solid phase mixing method comprises: mechanical mixing and pneumatic mixing.
In the step (2), the composite powder reduction treatment method comprises the following steps: reducing for 1-4 h under the condition of hydrogen at the temperature of 400-600 ℃.
In the step (3), a continuous extruder is adopted to prepare the graphene/copper composite material wire blank, and the composite powder is continuously added through a vibration funnel at a speed of 20-40 g/s.
In the step (3), continuous extrusion is carried out under the conditions that the temperature is 650-750 ℃, the rotating speed of an extrusion wheel is 5-15 rpm, and the extrusion ratio is 10-30. The diameter of the prepared graphene/copper composite material wire blank is 1 cm-3 cm.
In the step (4), the composite material wire blank is subjected to multi-pass cold drawing, and the deformation rate is 60-99%. The diameter of the prepared graphene/copper composite wire is 0.1 cm-2 cm.
The invention adopts the continuous extrusion technology to prepare the composite material wire blank, realizes the continuous production of the wire blank, simultaneously adopts the multi-pass drawing technology to realize the further dispersion and orientation of the graphene in the copper matrix, and improves the performance of the composite wire. The graphene/copper composite wire prepared by the method has higher electrical conductivity while obviously improving the tensile strength; the method has the advantages of less procedures, continuous production and high production efficiency.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The invention discloses a continuous preparation method of a graphene/copper composite wire, which comprises the following steps:
(1) mixing graphene and copper powder by adopting a solid phase; the mass ratio of the graphene is less than 5 wt%; the particle size of the copper powder is 50-500 mu m; the solid phase mixing method comprises mechanical mixing and pneumatic mixing;
(2) the composite powder is subjected to reduction treatment, and the reduction treatment method comprises the following steps: reducing for 1-4 h under the condition of hydrogen at the temperature of 400-600 ℃;
(3) preparing a graphene/copper composite material wire blank by adopting a continuous extruder, adding composite powder into a feed chute of the continuous extruder through a vibration funnel, continuously adding mixed powder through the vibration funnel at a speed of 20-40 g/s, and continuously extruding at 650-750 ℃, an extrusion wheel rotating speed of 5-15 rpm and an extrusion ratio of 10-30;
(4) and preparing the graphene/copper composite wire by adopting a multi-pass cold drawing technology. And (3) performing multi-pass cold drawing on the composite material wire blank, wherein the deformation rate is 60-99%.
Example 1
(1) 995g of copper powder with the particle size of 200-400 mu m and 5g of graphene powder (the mass ratio of graphene is 0.5 wt%) are weighed and put into a roller stirrer to be mixed, and the rotation speed is 12rpm and the mixture is mixed for 1 hour.
(2) And taking out the mixed powder, putting the powder into a reduction box filled with hydrogen, reducing the powder for 2 hours at 600 ℃, cooling and taking out the powder.
(3) And adding the composite powder into a feed chute of a continuous extruder through a vibrating funnel, wherein the adding speed is 20g/s, the rotating speed of an extrusion wheel is 7rpm, the temperature is about 650 ℃, the extrusion ratio is 10, and continuously extruding to obtain a composite wire blank with the diameter of 3 mm.
(4) And (3) carrying out multi-pass fine drawing on the obtained 3mm composite wire blank until the wire diameter is 1mm, wherein the deformation rate is 89%, so as to obtain the graphene/copper composite material wire.
The tensile strength of the lead can reach 450MPa, and the conductivity can reach 98.5% IACS.
Example 2
The difference from the embodiment 1 is that the mass ratio of the graphene in the step (1) is 1 wt%, the tensile strength of the composite wire prepared by the method can reach 500MPa, and the conductivity can reach 96.7% IACS.
Example 3
The difference from example 1 is that in step (3), the addition rate was 40g/s, the rotation speed of the extrusion wheel was 12rpm, the temperature was around 700 ℃, and the extrusion ratio was 20. The tensile strength of the lead can reach 430MPa, and the conductivity can reach 98% IACS.
Example 4
The difference from example 1 is that in step (4), fine drawing was carried out until the final wire diameter was 0.5mm and the deformation ratio was 97%. The tensile strength of the lead can reach 462MPa, and the conductivity can reach 98% IACS.
The embodiment shows that the graphene/copper composite wire prepared by the method has higher electrical conductivity while obviously improving the tensile strength; the method has the advantages of less procedures, continuous production and high production efficiency.

Claims (10)

1. A continuous preparation method of a graphene/copper composite wire comprises the following steps:
(1) mixing graphene and copper powder in a solid phase to obtain composite powder;
(2) carrying out reduction treatment on the composite powder;
(3) preparing a graphene/copper composite material wire blank by adopting a continuous extrusion technology;
(4) and preparing the graphene/copper composite wire by adopting a multi-pass cold drawing technology.
2. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the addition amount of the graphene is less than 5 wt%.
3. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the particle size of the copper powder is 50-500 mu m.
4. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the solid phase mixing method comprises mechanical mixing and pneumatic mixing.
5. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the reduction treatment method of the composite powder comprises the following steps: reducing for 1-4 h under the condition of hydrogen at the temperature of 400-600 ℃.
6. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the graphene/copper composite material wire blank is prepared by adopting a continuous extruder, and composite powder is continuously added through a vibration funnel at the speed of 20-40 g/s.
7. The continuous preparation method of the graphene/copper composite wire according to claim 6, wherein: and continuously extruding at 650-750 ℃, the rotating speed of the extrusion wheel is 5-15 rpm, and the extrusion ratio is 10-30.
8. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the diameter of the prepared graphene/copper composite material wire blank is 1 cm-3 cm.
9. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: and (3) performing multi-pass cold drawing on the composite material wire blank, wherein the deformation rate is 60-99%.
10. The continuous preparation method of the graphene/copper composite wire according to claim 1, wherein: the diameter of the prepared graphene/copper composite wire is 0.1 cm-2 cm.
CN201811550044.6A 2018-12-18 2018-12-18 Preparation method of graphene/copper composite wire Pending CN111331127A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112359244A (en) * 2020-10-21 2021-02-12 有研工程技术研究院有限公司 High-strength high-conductivity graphene copper composite wire and preparation method thereof

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