CN111161903B - Graphene-aluminum composite wire and preparation method thereof - Google Patents

Graphene-aluminum composite wire and preparation method thereof Download PDF

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CN111161903B
CN111161903B CN201911415192.1A CN201911415192A CN111161903B CN 111161903 B CN111161903 B CN 111161903B CN 201911415192 A CN201911415192 A CN 201911415192A CN 111161903 B CN111161903 B CN 111161903B
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graphene
metal layer
layer
intermediate metal
aluminum
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CN111161903A (en
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陈长科
卢科伟
李辰鹏
王成军
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Xinjiang Xijin Graphene Technology Co ltd
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Xinjiang Xijin Graphene Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/023—Alloys based on aluminium
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention discloses a graphene-aluminum composite wire which is a core-shell structure, wherein the core-shell structure comprises an aluminum substrate, a middle metal layer and a graphene layer, the middle metal layer is arranged around the aluminum substrate, the graphene layer is arranged around the middle metal layer, and the metal in the middle metal layer is one or two of copper and nickel. The invention also discloses a preparation method of the graphene aluminum composite wire, which comprises the following steps: forming the intermediate metal layer on the surface of the aluminum substrate, wherein the intermediate metal layer wraps the aluminum substrate to obtain a double-layer structure; and forming the graphene layer on the intermediate metal layer by using a plasma chemical vapor deposition method.

Description

Graphene-aluminum composite wire and preparation method thereof
Technical Field
The invention relates to the technical field of wires, in particular to a graphene-aluminum composite wire and a preparation method thereof.
Background
At present, the overhead high-voltage transmission conductor which is more commonly used at home and abroad comprises a copper conductor and an aluminum matrix. Compared with aluminum matrix, the copper wire has good conductivity and high strength. However, the cost of copper wire is high, copper belongs to strategic resource, and aluminum resource is abundant, widely distributed and low in cost. In recent years, as the suspension span of overhead high voltage transmission lines becomes larger, higher requirements are made on the performance of aluminum matrix cables.
The graphene has higher strength and good conductivity, so that the graphene is compounded with pure aluminum or an aluminum composite material to prepare the graphene/aluminum alloy composite material, and the graphene/aluminum alloy composite material is expected to be used for improving the strength and the conductivity of an aluminum cable and better matching the mechanical property and the electrical property of an aluminum matrix. The graphene is uniformly distributed in the aluminum matrix to become the biggest difficulty in the preparation process of the graphene-aluminum composite material, so that the enhancement effect of the graphene is seriously influenced, and the graphene powder is distributed in the aluminum matrix in a powder metallurgy method, so that the mechanical property enhancement advantage of the graphene can be exerted, but the conductivity cannot be effectively improved. In addition, in the preparation of the graphene-aluminum composite material by adopting a powder metallurgy method, due to the large specific surface area of graphene, agglomeration phenomenon is easy to occur in an aluminum matrix, mechanical ball milling adopted in a powder metallurgy process is only used for uniformly mixing powder of a reinforcing phase and powder of a matrix phase, and interface bonding is difficult to form between the powder in the ball milling process, so that the overall conductivity of the graphene-aluminum composite material is influenced.
Disclosure of Invention
Therefore, it is necessary to provide a graphene aluminum composite wire and a preparation method thereof, aiming at the technical problem that the graphene aluminum composite material prepared by the conventional method has poor conductivity.
A graphene-aluminum composite wire is a core-shell structure, the core-shell structure comprises an aluminum matrix, an intermediate metal layer and a graphene layer, the intermediate metal layer is arranged around the aluminum matrix, the graphene layer is arranged around the intermediate metal layer, and the metal in the intermediate metal layer is one or two of copper and nickel.
In one embodiment, the aluminum substrate is cylindrical.
In one embodiment, the aluminum matrix is a solid structure.
In one embodiment, the aluminum matrix has a diameter of 0.4mm to 1 mm.
In one embodiment, the thickness of the intermediate metal layer is 0.1 μm to 10 μm.
In one embodiment, the thickness of the graphene layer is 0.334 nm-3 nm.
A preparation method of the graphene-aluminum composite wire comprises the following steps:
forming the intermediate metal layer on the surface of the aluminum substrate, wherein the intermediate metal layer wraps the aluminum substrate to obtain a double-layer structure; and
and forming the graphene layer on the intermediate metal layer by adopting a plasma chemical vapor deposition method.
In one embodiment, the method for forming the intermediate metal layer is electroplating or magnetron sputtering.
In one embodiment, the step of forming the graphene layer on the intermediate metal layer includes:
introducing working gas and introducing gaseous carbon source in vacuum and plasma atmosphere;
forming the graphene layer on the intermediate metal layer at 450-400 ℃.
In one embodiment, the working gas comprises hydrogen, and optionally one or more of an inert gas and nitrogen.
In one embodiment, the gaseous carbon source is selected from one or more of methane, methanol, ethanol, methyl formate, acetylene.
In one embodiment, the working gas is introduced at a flow rate of 100sccm to 300sccm, and the gaseous carbon source is introduced at a flow rate of 5sccm to 30 sccm.
According to the graphene-aluminum composite wire, the intermediate metal layer is arranged between the aluminum substrate and the graphene layer, and copper or nickel is introduced as an intermediate metal to play a transition role, so that the binding property of graphene on the aluminum substrate can be improved, the lattice matching of each layer is improved, the lattice mismatch rate between each layer is reduced, a continuous structure can be formed, and the conductivity and the mechanical property of the graphene-aluminum composite wire are further improved.
Drawings
Fig. 1 is a schematic structural diagram of a graphene aluminum composite wire according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the present invention provides a graphene-aluminum composite wire, which is a core-shell structure, the core-shell structure includes, from inside to outside, an aluminum substrate 10, an intermediate metal layer 20 disposed around the aluminum substrate 10, and a graphene layer 30 disposed around the intermediate metal layer 20, where a metal in the intermediate metal layer 20 is one or both of copper and nickel.
According to the graphene-aluminum composite wire provided by the embodiment of the invention, the intermediate metal layer 20 is arranged between the aluminum substrate 10 and the graphene layer 30, and copper or nickel is introduced as an intermediate metal, so that a transition effect is achieved, the binding property of graphene on the aluminum substrate 10 can be improved, the lattice matching of each layer is improved, the lattice mismatch rate between each layer is reduced, a continuous structure can be formed, and the conductivity and the mechanical property of the graphene-aluminum composite wire are further improved.
In one embodiment, the aluminum substrate 10 is cylindrical, and may be, for example, a square cylinder or a cylinder. Preferably, the aluminum substrate 10 is cylindrical, the cylindrical shape more conforming to the general shape of a wire, and the curved outer surface of the cylindrical shape more facilitating the deposition of graphene or an intermediate metal and the formation of a uniform and continuous graphene layer 30.
In an embodiment, the aluminum substrate 10 is a solid structure, so that the graphene-aluminum composite wire is a solid structure, and the solid structure provides more stable conductivity and stronger mechanical properties for the graphene-aluminum composite wire.
In one embodiment, the aluminum matrix 10 may have a diameter of 0.4mm to 1 mm. In one embodiment, the thickness of the middle metal layer 20 may be 0.1 μm to 10 μm. In one embodiment, the graphene layer 30 is a two-dimensional graphene, such that the hexagonal honeycomb lattice of graphene can be maintained. In one embodiment, the thickness of the graphene layer 30 may be 0.334nm to 3 nm. Each layer can be matched with each other within the size range, and the lattice coherent rate of each layer and the conductivity and mechanical property of the whole graphene aluminum composite wire are achieved.
In one embodiment, the intermediate metal layer 20 and the graphene layer 30 form a superlattice structure. Preferably, the lattice matching rate of the interface between the intermediate metal layer 20 and the graphene layer 30 may be 85% or more.
The embodiment of the invention also provides a preparation method of the graphene-aluminum composite wire, which comprises the following steps:
s100, forming the intermediate metal layer 20 on the surface of the aluminum substrate 10, wherein the intermediate metal layer 20 wraps the aluminum substrate 10 to obtain a double-layer structure; and
and S200, forming the graphene layer 30 on the intermediate metal layer 20 by using a plasma chemical vapor deposition method.
In step S100, a method for forming the intermediate metal layer 20 may be an electroplating method or a magnetron sputtering method. The electroplating method is a process of plating an intermediate metal thin layer on the surface of the aluminum substrate 10 by using electrolysis, and during electroplating, a plating metal (i.e., the intermediate metal) is used as an anode, a workpiece to be plated (i.e., the aluminum substrate 10) is used as a cathode, and cations of the plating metal are reduced on the surface of the workpiece to be plated to form a plating layer. In order to eliminate the interference of other cations and make the coating uniform and firm, a solution containing the metal cations of the coating is used as an electroplating solution to keep the concentration of the metal cations of the coating constant. The magnetron sputtering method is to fill a proper amount of argon gas into high vacuum, apply direct current voltage between a cathode (the metal of the intermediate metal layer 20 is used as a cathode material) and an anode, and generate magnetic control type abnormal glow discharge in a coating chamber to ionize the argon gas. The argon ions are accelerated by the cathode and bombard the cathode surface, sputtering out the cathode surface atoms to deposit an intermediate metal layer 20 on the surface of the aluminum substrate 10.
In one embodiment, the electroplating solution used to form the intermediate metal layer 20 by electroplating may include nickel sulfate with a concentration of 30g/L to 40g/L, sodium hypophosphite with a concentration of 20g/L to 30g/L, and lactic acid with a concentration of 25mg/L to 35 g/L. In one embodiment, the temperature of the plating may be 45 ℃ to 65 ℃. Or the electroplating solution can comprise 30 g/L-40 g/L copper sulfate, 20 g/L-30 g/L sodium hypophosphite and 25 mg/L-35 g/L lactic acid.
In step S200, the step of forming the graphene layer 30 may be performed in a vacuum tube furnace, which may be provided with a plasma device.
In an embodiment, the double-layer structure formed by the aluminum substrate 10 and the intermediate metal layer 20 may be set to be a winding shape in a vacuum tube furnace, the graphene aluminum composite wire on which the graphene layer 30 has been formed is drawn out of the vacuum tube furnace at a constant speed, and the double-layer structure on which the graphene layer 30 is not formed at the other end of the winding shape is drawn into the vacuum tube furnace from the other end of the vacuum tube furnace to perform graphene growth, so that the formation thickness of the graphene layer 30 can be controlled more easily.
In an embodiment, the step of forming the graphene layer 30 on the intermediate metal layer 20 may include:
introducing working gas and introducing gaseous carbon source in vacuum and plasma atmosphere;
forming the graphene layer 30 on the intermediate metal layer 20 at 450 to 400 ℃.
In one embodiment, the working gas comprises hydrogen, and optionally one or more of an inert gas and nitrogen.
In one embodiment, the gaseous carbon source may be selected from one or more of methane, methanol, ethanol, methyl formate, acetylene.
In one embodiment, the flow rate of the working gas is 100sccm to 300sccm, and the flow rate of the gaseous carbon source is 5sccm to 30 sccm.
Example 1
Preparing an electroplating solution according to a formula of 35g/L nickel sulfate, 25g/L sodium hypophosphite and 30mg/L lactic acid, placing the aluminum substrate 10 which is ultrasonically cleaned by alcohol at 100Hz for 1h into the electroplating solution at 60 ℃, taking out after 40min, and forming an intermediate metal layer 20 on the surface of the aluminum substrate 10 to obtain a double-layer structure. The aluminum substrate 10 has a diameter of 0.5 mm.
And (3) putting the double-layer structure into a vacuum tube furnace, heating to 500 ℃, opening plasma, gradually forming a graphene layer 30 on the middle metal layer 20 to obtain the graphene-aluminum composite wire, wherein the methane introduction amount is 5sccm, the hydrogen introduction amount is 100sccm, and the argon introduction amount is 200 sccm.
The graphene-aluminum composite wire forming the graphene layer 30 is slowly pulled outwards from the tail end of the vacuum tube furnace, and the time for the double-layer structure to pass through the heating area of the tube furnace is ensured to be more than 10 min.
And collecting the graphene-aluminum composite wires of the graphene layer 30 on which the graphene grows, and twisting the collected graphene-aluminum composite wires.
Example 2
Preparing a plating solution according to a formula of 30g/L copper sulfate, 20g/L sodium hypophosphite and 35mg/L lactic acid, placing the aluminum substrate 10 which is ultrasonically cleaned by alcohol at 100Hz for 1h into the plating solution at 60 ℃, taking out after 40min, and forming an intermediate metal layer 20 on the surface of the aluminum substrate 10 to obtain a double-layer structure. The aluminum substrate 10 has a diameter of 0.5 mm.
And (3) putting the double-layer structure into a vacuum tube furnace, heating to 450 ℃, opening the plasma, introducing gaseous ethanol with the introduction amount of 20sccm, introducing hydrogen with the introduction amount of 50sccm and introducing argon with the introduction amount of 100sccm, and gradually forming a graphene layer 30 on the middle metal layer 20 to obtain the graphene-aluminum composite wire.
The graphene aluminum composite wire forming the graphene layer 30 is slowly pulled outwards from the tail end of the vacuum tube furnace, and the time for the double-layer structure to pass through the heating area of the tube furnace is ensured to be more than 10 min.
And collecting the graphene-aluminum composite wires of the graphene layer 30 on which the graphene grows, and twisting the collected graphene-aluminum composite wires.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that the concentration of nickel sulfate was changed to 50 g/L.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that the graphene layer 30 is directly grown without plating the aluminum substrate 10.
The graphene aluminum composite wires of examples 1-2 and comparative examples 1-2 were cut into 400mm wires, subjected to a tensile test at a tensile rate of 0.5mm/min, and subjected to a conductivity test, with the results shown in table 1.
TABLE 1
Group of Tensile strength/MPa Conductivity/% IACS
Example 1 245.89 40.41
Example 2 234.59 40.44
Comparative example 1 225.54 55.14
Comparative example 2 204.52 50.24
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (4)

1. A preparation method of a graphene aluminum composite wire comprises the following steps:
forming an intermediate metal layer on the surface of an aluminum substrate, wherein the aluminum substrate is wrapped by the intermediate metal layer to obtain a double-layer structure, the metal in the intermediate metal layer is nickel, and the intermediate metal layer is formed by an electroplating method or a magnetron sputtering method; and
forming a graphene layer on the intermediate metal layer using a plasma chemical vapor deposition method, including:
introducing working gas and introducing gaseous carbon source in vacuum and plasma atmosphere;
and forming the graphene layer on the intermediate metal layer at 450-600 ℃.
2. The method of claim 1, wherein the working gas comprises hydrogen and optionally one or more of an inert gas and nitrogen.
3. The method for preparing the graphene aluminum composite wire according to claim 1, wherein the gaseous carbon source is selected from one or more of methane, methanol, ethanol, methyl formate and acetylene.
4. The method for preparing the graphene aluminum composite wire according to claim 1, wherein the flow rate of the working gas is 100sccm to 300sccm, and the flow rate of the gaseous carbon source is 5sccm to 30 sccm.
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CN112768139B (en) * 2020-12-29 2022-09-09 国家高速列车青岛技术创新中心 High-conductivity aluminum wire cable core and preparation method thereof

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CN103021502A (en) * 2012-12-25 2013-04-03 山东鑫汇铜材有限公司 Copper-clad aluminum conductor
CN106057288A (en) * 2016-07-22 2016-10-26 汉舟四川铜铝复合科技有限公司 Good conductive copper aluminum compound socket
CN109036697A (en) * 2018-08-16 2018-12-18 上海乔辉新材料科技有限公司 A kind of NEW TYPE OF COMPOSITE conducting wire and preparation method thereof
CN208589274U (en) * 2017-12-29 2019-03-08 汉舟四川铜铝复合科技有限公司 A kind of strong conductive copper aluminium composite bar

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Publication number Priority date Publication date Assignee Title
CN103021502A (en) * 2012-12-25 2013-04-03 山东鑫汇铜材有限公司 Copper-clad aluminum conductor
CN106057288A (en) * 2016-07-22 2016-10-26 汉舟四川铜铝复合科技有限公司 Good conductive copper aluminum compound socket
CN208589274U (en) * 2017-12-29 2019-03-08 汉舟四川铜铝复合科技有限公司 A kind of strong conductive copper aluminium composite bar
CN109036697A (en) * 2018-08-16 2018-12-18 上海乔辉新材料科技有限公司 A kind of NEW TYPE OF COMPOSITE conducting wire and preparation method thereof

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