CN117393234B - Composite conductor, preparation method thereof and conductive element - Google Patents
Composite conductor, preparation method thereof and conductive element Download PDFInfo
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- CN117393234B CN117393234B CN202311687648.6A CN202311687648A CN117393234B CN 117393234 B CN117393234 B CN 117393234B CN 202311687648 A CN202311687648 A CN 202311687648A CN 117393234 B CN117393234 B CN 117393234B
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- 239000004020 conductor Substances 0.000 title claims abstract description 145
- 239000002131 composite material Substances 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000000843 powder Substances 0.000 claims abstract description 78
- 239000002184 metal Substances 0.000 claims abstract description 72
- 229910052751 metal Inorganic materials 0.000 claims abstract description 72
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 71
- 230000005684 electric field Effects 0.000 claims abstract description 54
- 229920005989 resin Polymers 0.000 claims abstract description 40
- 239000011347 resin Substances 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 23
- 238000007731 hot pressing Methods 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 230000009471 action Effects 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 51
- 238000010438 heat treatment Methods 0.000 claims description 46
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 36
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 238000010146 3D printing Methods 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 15
- 229910044991 metal oxide Inorganic materials 0.000 claims description 14
- 150000004706 metal oxides Chemical class 0.000 claims description 14
- 239000003822 epoxy resin Substances 0.000 claims description 13
- 229920000647 polyepoxide Polymers 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- -1 alicyclic amine Chemical class 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 12
- 229910052734 helium Inorganic materials 0.000 claims description 12
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 12
- 150000001412 amines Chemical class 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 8
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 229910001316 Ag alloy Inorganic materials 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 5
- 239000005751 Copper oxide Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 150000008064 anhydrides Chemical class 0.000 claims description 5
- 229910000431 copper oxide Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 229910001923 silver oxide Inorganic materials 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 claims description 3
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 229920000180 alkyd Polymers 0.000 claims description 3
- 229920003180 amino resin Polymers 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 150000004982 aromatic amines Chemical class 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 3
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052743 krypton Inorganic materials 0.000 claims description 3
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052704 radon Inorganic materials 0.000 claims description 3
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- BCDGQXUMWHRQCB-UHFFFAOYSA-N glycine methyl ketone Natural products CC(=O)CN BCDGQXUMWHRQCB-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000002002 slurry Substances 0.000 abstract description 13
- 230000001976 improved effect Effects 0.000 abstract description 11
- 230000004927 fusion Effects 0.000 abstract description 6
- 238000003466 welding Methods 0.000 abstract description 6
- 238000007639 printing Methods 0.000 description 16
- 238000002156 mixing Methods 0.000 description 13
- 150000002431 hydrogen Chemical class 0.000 description 11
- 238000005245 sintering Methods 0.000 description 10
- 230000001939 inductive effect Effects 0.000 description 9
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- 230000000052 comparative effect Effects 0.000 description 8
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- 230000006872 improvement Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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Classifications
-
- 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
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
-
- 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
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- 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
-
- 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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Thermal Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Conductive Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses a composite conductor, a preparation method thereof and a conductive element, and relates to the technical field of conductors. The preparation method of the composite conductor comprises the following steps: providing conductive slurry, wherein the conductive slurry comprises metal powder and a reagent, and the reagent comprises resin and a polar compound; applying an electric field to the conductive paste to obtain a composite conductor precursor; coating the composite conductor precursor with a graphene layer to obtain a composite conductor preform; and performing hot pressing treatment on the composite conductor preform to obtain the composite conductor. According to the preparation method of the composite conductor, the metal powder is distributed according to the positions of the better conductive directions under the action of the electric field, and the graphene is in close contact with the metal powder, so that the conductive performance of the composite conductor is obviously improved, and the hardness and fusion welding resistance of the conductor can be further improved by the graphene.
Description
Technical Field
The application relates to the technical field of conductors, in particular to a composite conductor, a preparation method thereof and a conductive element.
Background
The graphene has excellent performances of high electric conductivity, high heat conduction, high strength, high flexibility, strong chemical inertness, excellent gas barrier property and the like, is widely applied in various fields, particularly in the technical field of conductors, and can remarkably improve the electric conductivity of metals (such as copper, copper alloy and the like).
The existing metal such as copper powder is generally in various irregular shapes, including dendritic, rod-shaped or quasi-spherical shapes containing various bulges or grooves, and the like, powder in different shapes is usually mixed at present, and the powder is forced to deform in a hot pressing mode and the like to finally form a required finished product, but the inside of a conductor finished product still has a conductive effect as irregular powder units, each powder unit has different shapes and different internal electronic sequences, so that the conductive sequences among the powder units are different, the arrangement of some powder units cannot have a good conductive effect, and a magnetic field generated by the sequence of the powder units can prevent the electronic transmission, so that the conductive performance of surrounding powder is reduced.
The existing processing mode cannot realize the ordering of all the powder according to the optimal conductive mode, although graphene with excellent conductivity is added, the overall conductive performance of the conductor is limited by the addition of the graphene and the ordering mode of the copper conductor. Therefore, how to arrange the metal powder in the optimal conductive direction to obtain the conductor finished product with high conductivity needs to be further improved.
Disclosure of Invention
In view of the above, the application provides a composite conductor, a preparation method thereof and a conductive element.
The application is realized in such a way that a preparation method of a composite conductor comprises the following steps:
providing a conductive paste, wherein the conductive paste comprises metal powder and a reagent, and the reagent comprises resin and a polar compound;
applying an electric field to the conductive paste to obtain a composite conductor precursor;
coating the composite conductor precursor with a graphene layer to obtain a composite conductor preform;
and carrying out hot pressing treatment on the composite conductor preform to obtain the composite conductor.
Optionally, the method for applying an electric field includes: the conductive paste is flowed through the electric field.
Optionally, the method of flowing the conductive paste through the electric field comprises: placing the conductive paste in 3D printing equipment, and setting an electric field at an outlet of the 3D printing equipment; the distance between the electric field and the outlet of the 3D printing device is 2 cm-8 cm.
Optionally, the method for applying an electric field includes: providing a mould, placing the conductive paste in the mould, and applying an electric field to the mould.
Optionally, the electric field strength of the electric field is 100V/cm-260V/cm; and the power supply of the electric field is direct current or alternating current.
Optionally, the material of the metal powder comprises one or more of copper, silver, copper alloy and silver alloy; the shape of the metal powder comprises one or more of dendritic, rod-like, flake-like, cube-like, spherical or nearly spherical; the average particle diameter of the metal powder is 10-100 mu m.
Optionally, the resin comprises one or more of epoxy resin, acrylic resin, amino resin, alkyd resin, polyurethane resin, cyclic silicone resin and fluorocarbon resin; and/or
The polar compound comprises one or more of methanol, ethanol, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, acetic acid, propanol, pyridine, tetramethyl ethylenediamine, acetone and triethylamine.
Optionally, in the conductive paste, the mass fraction of the metal powder is 40% -60%; and/or
The mass ratio of the resin to the polar compound is (10-30): (5-10).
Optionally, the reagent further comprises a solvent; the solvent comprises one or more of tetrahydrofuran, benzene, toluene, xylene and n-butanol; the mass ratio of the resin to the solvent is (10-30): (15-35).
Optionally, the reagent further comprises an auxiliary carbon source; the auxiliary carbon source comprises one or more of phenanthrene, anthracene, naphthalene and polymethyl methacrylate; the mass ratio of the resin to the auxiliary carbon source is (10-30): (1-3).
Optionally, the reagent further comprises a metal oxide; the metal oxide comprises one or more of copper oxide and silver oxide; the mass ratio of the resin to the metal oxide is (10-30): (0.1 to 10).
Optionally, the reagent further comprises a curing agent; the curing agent comprises one or more of an amine curing agent and an anhydride curing agent; the amine curing agent comprises one or more of polyamide curing agent, aliphatic amine curing agent, aromatic amine curing agent, alicyclic amine curing agent, polyether amine curing agent and imidazole curing agent; the anhydride curing agent comprises one or more of aromatic anhydride curing agents, aliphatic anhydride curing agents and alicyclic anhydride curing agents; the mass ratio of the resin to the curing agent is (10-30): (0.1 to 15).
Optionally, the coating the composite conductor precursor with the graphene layer includes: and (5) introducing protective gas, and performing first heat treatment to obtain carbide.
Optionally, the temperature of the first heat treatment is 500-700 ℃; the time of the first heat treatment is 20-38 min; and/or
The first heat treatment is performed in a vacuum environment having a vacuum degree of 10 -3 kPa; and/or
The protective gas comprises one or more of nitrogen, helium, argon, xenon, krypton, neon and radon.
Optionally, after obtaining the carbide, the method further includes: and introducing auxiliary gas, and performing second heat treatment to obtain the graphene layer.
Optionally, the temperature of the second heat treatment is 800-1050 ℃; the second heat treatment time is 20-50 min; and/or
The assist gas comprises hydrogen; the flow rate of the auxiliary gas is 10 sccm-500 sccm; and/or
The number of the graphene layers is 3-8.
Optionally, the temperature of the hot pressing treatment of the composite conductor preform is 800-950 ℃; the time of the hot pressing treatment of the composite conductor preform is 20-50 min; the pressure of the hot pressing treatment of the composite conductor preform is 200-1200 kN.
Accordingly, the present application also provides a composite conductor comprising:
the metal powder is orderly arranged in the conductive direction under the action of the electric field driving force; and
and the graphene is filled between the orderly arranged metal powder and the metal powder, and coats the metal powder to form a graphene layer.
Optionally, the material of the metal powder comprises one or more of copper, silver, copper alloy and silver alloy; the shape of the metal powder comprises one or more of dendritic, rod-like, flake-like, cube-like, spherical or nearly spherical; the average particle diameter of the metal powder is 10-100 mu m.
Optionally, the number of the graphene layers is 3-8.
Correspondingly, the application also provides a conductive element which comprises the composite conductor or the composite conductor prepared by the preparation method; the conductive element includes a wire or an electrical contact conductor.
According to the preparation method of the composite conductor, under the action of an electric field, the metal powder is used as a conductive unit, and the metal powder with different shapes is different in magnetic field formed during conduction due to different position ordering, so that the metal powder is moved in position due to interaction of different magnetic fields, and better conductive position distribution is formed under the action of the magnetic field; after the heating treatment, the resin can be carbonized and cracked, graphene is generated on the surface of the metal powder, and the continuous composite conductor formed by mixing the graphene and the metal powder is obtained.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flowchart of a method for preparing a composite conductor according to an embodiment of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, based on the embodiments herein, which are obtained by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application. Furthermore, it should be understood that the detailed description is presented herein for purposes of illustration and explanation only and is not intended to limit the present application.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used to generally refer to the upper and lower positions of the device in actual use or operation, and specifically the orientation of the drawing figures; while "inner" and "outer" are for the outline of the device. In addition, in the description of the present application, the term "comprising" means "including but not limited to". The terms first, second, third and the like are used merely as labels, and do not impose numerical requirements or on the order of construction.
In the present application, "and/or" describing the association relationship of the association object means that there may be three relationships, for example, a and/or B may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural.
In this application, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The technical scheme of the application is as follows:
in a first aspect, embodiments of the present application provide a composite conductor comprising:
the metal powder is orderly arranged in the conductive direction under the action of the electric field driving force; and
and the graphene is filled between the orderly arranged metal powder and the metal powder, and coats the metal powder to form a graphene layer.
It should be noted that, ordered arrangement according to the conductive direction means that when different metals have different conductive properties due to different grain orientations, under the action of an electric field or a magnetic field, the metal powder is arranged in an optimal conductive orientation, and after the conductive orientation arrangement is maintained, the conductivity of the composite conductor can be improved.
According to the composite conductor, the metal powder is distributed according to the positions of the better conductive directions, and the graphene is in close contact with the metal powder, so that the conductive performance of the composite conductor is remarkably improved, and the hardness and fusion welding resistance of the conductor can be further improved by the graphene.
In some embodiments, the material of the metal powder comprises one or more of copper, silver, copper alloy, and silver alloy.
In some embodiments, the shape of the metal powder includes one or more of dendritic, rod-like, flake-like, cubic, spherical, or near-spherical.
In some embodiments, the metal powder has an average particle size of 10 μm to 100 μm, for example, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or the like.
In some embodiments, the number of the graphene layers is 3 to 8, for example, 4 layers, 5 layers, 6 layers, 7 layers, and the like.
In some embodiments, a metal oxide is also included in the composite conductor. The metal oxide can further improve the fusion welding resistance of the composite conductor.
In some embodiments, the metal oxide comprises one or more of copper oxide, silver oxide.
In a second aspect, as shown in fig. 1, an embodiment of the present application provides a method for preparing a composite conductor, including:
s11, providing conductive paste, wherein the conductive paste comprises metal powder and a reagent, and the reagent comprises resin and a polar compound;
s12, applying an electric field to the conductive paste to obtain a composite conductor precursor;
s13, coating the graphene layer on the composite conductor precursor to obtain a composite conductor preform;
s14, performing hot pressing treatment on the composite conductor preform to obtain the composite conductor.
According to the preparation method of the composite conductor, under the action of an electric field, the metal powder is used as a conductive unit, and the metal powder with different shapes is different in magnetic field formed during conduction due to different position ordering, so that the metal powder is moved in position due to interaction of different magnetic fields, and better conductive position distribution is formed under the action of the magnetic field; after the heating treatment, the resin can be carbonized and cracked, graphene is generated on the surface of the metal powder, and the continuous composite conductor formed by mixing the graphene and the metal powder is obtained.
In the step S11:
in some embodiments, the mass fraction of the metal powder in the conductive paste is 40% -60%, for example, 42%, 45%, 48%, 50%, 52%, 55%, 58%, etc. And in the mass fraction range, the dissolution of the metal powder is facilitated.
In some embodiments, the resin comprises one or more of an epoxy resin, an acrylic resin, an amino resin, an alkyd resin, a polyurethane resin, a cyclic silicone resin, a fluorocarbon resin. The resin is used as a binder, has good compatibility with organic materials and inorganic materials, can promote the dissolution and dispersion of metal powder in polar compounds, is a high molecular organic polymer, and can provide a carbon source for the growth of graphene.
In some embodiments, the polar compound includes one or more of methanol, ethanol, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, acetic acid, propanol, pyridine, tetramethyl ethylenediamine, acetone, triethylamine. The polar compound has good conductivity due to the polarity of molecules caused by the fact that the centers of gravity of positive and negative charges in the molecules are not coincident, and can play a role in continuous conduction during the electrifying treatment, so that the movement of metal powder is promoted.
In some embodiments, the mass ratio of the resin to the polar compound is (10-30): (5-10), for example, may be 15: 8. 20: 8. 25:8, etc.
In some embodiments, a solvent is also included in the reagent. The solvent is advantageous in promoting improvement of the surface tension of the polar compound and the resin, further promoting uniform dispersion of the metal powder in the slurry.
Further, the solvent comprises one or more of tetrahydrofuran, benzene, toluene, xylene and n-butanol.
In some embodiments, the mass ratio of the resin to the solvent is (10-30): (15 to 35), for example, may be 15: 20. 15: 25. 15: 30. 20: 20. 20: 25. 20: 30. 25: 20. 25:30, etc.
In some embodiments, an auxiliary carbon source is also included in the reagent. The auxiliary carbon source can provide a carbon source for the growth of graphene and promote the growth of synthetic graphene on the surface of the metal powder.
Further, the auxiliary carbon source comprises one or more of phenanthrene, anthracene, naphthalene and polymethyl methacrylate (PMMA).
In some embodiments, the mass ratio of the resin to the auxiliary carbon source is (10-30): (1 to 3), for example, may be 12: 2. 15: 2. 18: 2. 20: 2. 22: 2. 25: 2. 28:2, etc.
In some embodiments, a metal oxide is also included in the reagent. The metal oxide can react with long-chain carbon formed after carbonization of the resin in the heating treatment process, so that the long-chain carbon is changed into short-chain carbon, and then is cracked into carbon, and the generation of graphene is promoted; and a small amount of unreacted metal oxide can be remained in the composite conductor, so that the fusion welding resistance of the composite conductor is improved.
Further, the metal oxide comprises one or more of copper oxide and silver oxide.
In some embodiments, the mass ratio of the resin to the metal oxide is (10-30): (0.1 to 10), for example, may be 12: 5. 15: 5. 18: 5. 20: 5. 22: 5. 25: 5. 28:5, etc.
In some embodiments, a curing agent is also included in the reagent. The curing agent can chemically react with the epoxy resin to form a network-shaped three-dimensional polymer.
Further, the curing agent comprises one or more of amine curing agents and anhydride curing agents. The amine curing agent comprises one or more of polyamide curing agent, aliphatic amine curing agent, aromatic amine curing agent, alicyclic amine curing agent, polyether amine curing agent and imidazole curing agent. The acid anhydride curing agent comprises one or more of aromatic acid anhydride curing agent, aliphatic acid anhydride curing agent and alicyclic acid anhydride curing agent.
In some embodiments, the mass ratio of the resin to the curing agent is (10-30): (0.1 to 15), for example, may be 12: 5. 15: 5. 18: 5. 20: 5. 22: 5. 25: 5. 28:5, etc.
It is understood that the organic matters containing carbon in the reagent can be used as carbon sources for graphene growth, such as resin, solvent and the like.
In the S12:
in some embodiments, the electric field has an electric field strength of 100V/cm to 260V/cm, for example, 120V/cm, 150V/cm, 180V/cm, 200V/cm, 220V/cm, 250V/cm, etc. And in the electric field intensity range, the metal powder is favorably induced to be orderly arranged along the conductive direction.
It will be appreciated that the power source of the electric field may be either direct current or alternating current.
In some embodiments, the method of applying an electric field comprises: the conductive paste is flowed through the electric field. It can be understood that the conductive paste is in fluid state and passes through the electric field, so that each metal powder can be ensured to be subjected to the action of the electric field force, and the movement ordering of the metal powder is further promoted.
Specifically, a 3D printing method may be adopted, the conductive paste is placed in a 3D printing apparatus, and an electric field is set at an outlet of the 3D printing apparatus.
In some embodiments, the distance between the electric field and the outlet of the 3D printing device is 2 cm-8 cm, for example, 3cm, 4cm, 5cm, 6cm, 7cm, etc. In the distance range, the flowing out of the conductive paste is not influenced, and the metal powder in the conductive paste can be effectively orderly arranged according to the conductive direction.
It can be understood that the metal powder after ordered arrangement can be solidified into a model by adopting a 3D printing mode, so that the subsequent sintering treatment is convenient.
In other embodiments, the method of applying an electric field comprises: providing a mould, placing the conductive paste in the mould, and applying an electric field to the mould. It can be understood that the electric field is directly applied to the mold, so that spillage and leakage in the flowing process of the conductive paste can be avoided, the mold is a required mold, and the follow-up operation is very convenient.
In some embodiments, the composite conductor precursor includes metal powders ordered in a conductive direction, and a reagent doped between gaps of adjacent metal powders.
In the S13:
in some embodiments, the graphene layer coating the composite conductor precursor comprises: and (5) introducing protective gas, and performing first heat treatment to obtain carbide.
Further, the temperature of the first heat treatment is 500 ℃ to 700 ℃, for example, 520 ℃, 550 ℃, 580 ℃, 600 ℃, 620 ℃, 650 ℃, 680 ℃, and the like; the time of the first heat treatment is 20min to 38min, for example, 22min, 25min, 28min, 30min, 32min, 35min and the like.
In some embodiments, the first heat treatment is performed in a vacuum environment having a vacuum level of 10 -3 kPa。
In some embodiments, the shielding gas comprises one or more of nitrogen, helium, argon, xenon, krypton, neon, radon.
In this way, under the conditions of the first heat treatment described above, the carbonization of the carbon source is facilitated, and short-chain carbides are generated and cracked into carbon.
In some embodiments, after obtaining the carbide, the method further comprises: and introducing auxiliary gas, and performing second heat treatment to obtain the graphene layer.
Further, the temperature of the second heat treatment is 800 ℃ to 1050 ℃, for example, 850 ℃, 900 ℃, 950 ℃, 1000 ℃ and the like; the second heat treatment time is 20 min-50 min, for example, 25min, 30min, 35min, 40min, 45min, etc.
In some embodiments, the assist gas comprises hydrogen. The hydrogen can promote the cracking of a carbon source and improve the uniformity and quality of graphene growth; the hydrogen has the effect of etching the boundary and internal defects of the graphene on the generated graphene, so that the size and morphology of the crystal domain of the graphene are affected.
In some embodiments, the flow rate of the assist gas is 10sccm to 500sccm, for example, 50sccm, 100sccm, 150sccm, 200sccm, 250sccm, 300sccm, 350sccm, 400sccm, 450sccm, etc.
It will be appreciated that the second heat treatment may also be performed in a vacuum environment and in an atmosphere with a protective gas.
As such, under the conditions of the second heat treatment described above, short chain carbides and carbon are advantageously converted to graphene.
The grown graphene directly fills the occupied space of the original reagent, is favorable for the continuity of the graphene, is fully contacted with the metal powder, and improves the conductivity, the hardness and the fusion welding resistance of the composite conductor.
In the step S14:
in some embodiments, the temperature of the extrusion process is 800 ℃ to 950 ℃, for example, 820 ℃, 850 ℃, 880 ℃, 900 ℃, 920 ℃, etc.; the time of the extrusion treatment is 20-50 min, for example, 25min, 30min, 35min, 40min, 45min and the like; the pressure of the extrusion treatment is 200-1200 kN, for example, 200kN, 300kN, 400kN, 500kN, 600kN, 700kN, 800kN, 900kN, 1000kN, 1100kN, etc.
Under the condition of the extrusion treatment, gaps in the composite conductor are removed, so that the graphene and the metal powder are more closely connected, and the conductivity of the composite conductor is improved.
In a third aspect, embodiments of the present application further provide a conductive element, including a composite conductor manufactured by the above manufacturing method.
In some embodiments, the conductive element comprises a wire or an electrical contact conductor.
The present application is specifically illustrated by the following examples, which are only some of the examples of the present application and are not limiting of the present application.
Example 1
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 55g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 25g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 2
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 50g of copper powder with an average particle size of 50 mu m, 10g of acrylic resin, 18g of ethanol, 15g of benzene, 2g of phenanthrene and 5g of amine curing agent, and mixing to obtain conductive paste;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 3
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 20g of acrylic resin, 15g of ethanol, 15g of tetrahydrofuran, 1g of PMMA, 5g of amine curing agent and 4g of copper oxide, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 4
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 100V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 5
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 260V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 6
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste in a die, electrifying the die, and inducing copper powder in the conductive paste to move with the electric field strength of 200V/cm, and arranging the copper powder in the conductive paste according to the conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 7
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Vacuum chamber of kPa, helium gas andnitrogen is used as protective gas, the temperature is raised to 600 ℃, and the temperature is kept for 30min, so that the resin is fully carbonized, and short-chain carbide is obtained; heating to 800 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 8
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing copper powder in the conductive paste to move, and arranging the copper powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen into a vacuum chamber of kPa as protective gases, heating to 600 ℃, and preserving heat for 30min to fully carbonize the resin to obtain short-chain carbide; heating to 1050 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Example 9
The embodiment provides a composite conductor, which is prepared by the following steps:
providing 40g of silver powder with the average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive paste;
placing the conductive paste into printing equipment, and electrifying direct current at a position of 5cm of a printing outlet of the 3D printing equipment, wherein the electric field strength is 200V/cm, inducing silver powder in the conductive paste to move, and arranging the silver powder in a conductive direction to obtain a composite conductor precursor;
placing the composite conductor precursor in vacuum degree of 10 -3 Introducing helium and nitrogen as protective gases into a vacuum chamber of kPa, heating to 600 ℃, and preserving heat for 30min to fill the resinCarbonizing to obtain short chain carbide; heating to 1000 ℃ again, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of graphene is 5; sintering and hot pressing are carried out, the temperature is 900 ℃, the heat preservation is carried out for 10min, and the pressure is 500kN, so that the composite conductor is obtained.
Comparative example 1
The comparative example provides a composite conductor, which is prepared as follows:
providing 40g of copper powder with an average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive slurry;
and heating the conductive slurry to 1000 ℃, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of the graphene is 5, so as to obtain the composite conductor.
Comparative example 2
The comparative example provides a composite conductor, which is prepared as follows:
and preparing graphene on the surface of the copper powder by adopting a vapor deposition method to obtain the composite conductor.
Comparative example 3
The comparative example provides a composite conductor, which is prepared as follows:
providing 40g of silver powder with the average particle size of 50 mu m, 30g of epoxy resin and 30g of methanol, and mixing to obtain conductive paste;
and heating the conductive slurry to 1000 ℃, introducing 200sccm of hydrogen, and preserving heat for 30min to convert short-chain carbide into graphene, wherein the number of layers of the graphene is 5, so as to obtain the composite conductor.
The thermal conductivity and the electrical conductivity of the composite conductors of examples 1 to 9 and comparative examples 1 to 3 were measured. Wherein, the method for testing the electric conductivity refers to T/CSTM00591-2022, and the method for testing the thermal conductivity refers to GB/T22588-2008. The results are shown in Table 1.
TABLE 1
As can be seen from table 1: compared with comparative examples 1-3, the electrical conductivity and the thermal conductivity of the composite conductor in examples 1-9 are remarkably improved, because the metal powder is arranged in the conductive direction after the electric field treatment, and when the composite conductor is used for conducting electricity, the magnetic fields in the metal powder cannot repel each other, so that the conductivity of the composite conductor is improved; and in the metal powder orderly arranged according to the conductive direction, graphene grows in situ, so that tight contact between the graphene and the metal powder is facilitated, the improvement of the graphene on the conductivity and fusion welding resistance of the metal powder is promoted, and the performance of the composite conductor is effectively improved.
The composite conductor, the preparation method thereof and the conductive element provided by the embodiment of the application are described in detail, and specific examples are applied to the description of the principle and the implementation mode of the application, and the description of the above examples is only used for helping to understand the method and the core idea of the application; meanwhile, those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, and the present description should not be construed as limiting the present application in view of the above.
Claims (21)
1. A method of making a composite conductor comprising:
providing a conductive paste, wherein the conductive paste comprises metal powder and a reagent, and the reagent comprises resin and a polar compound;
applying an electric field to the conductive paste to obtain a composite conductor precursor;
coating the composite conductor precursor with a graphene layer to obtain a composite conductor preform;
and carrying out hot pressing treatment on the composite conductor preform to obtain the composite conductor.
2. The method of preparing a composite conductor of claim 1, wherein the method of applying an electric field comprises: the conductive paste is flowed through the electric field.
3. The method of preparing a composite conductor of claim 2, wherein the method of flowing the conductive paste through the electric field comprises: placing the conductive paste in 3D printing equipment, and setting an electric field at an outlet of the 3D printing equipment; the distance between the electric field and the outlet of the 3D printing device is 2 cm-8 cm.
4. The method of preparing a composite conductor of claim 1, wherein the method of applying an electric field comprises: providing a mould, placing the conductive paste in the mould, and applying an electric field to the mould.
5. The method for manufacturing a composite conductor according to claim 1, wherein the electric field has an electric field strength of 100V/cm to 260V/cm; and the power supply of the electric field is direct current or alternating current.
6. The method for manufacturing a composite conductor according to claim 1, wherein the material of the metal powder comprises one or more of copper, silver, a copper alloy, and a silver alloy; the shape of the metal powder comprises one or more of dendritic, rod-like, flake-like, cube-like, spherical or nearly spherical; the average particle diameter of the metal powder is 10-100 mu m.
7. A method of producing a composite conductor according to claim 1, wherein,
the resin comprises one or more of epoxy resin, acrylic resin, amino resin, alkyd resin, polyurethane resin, cyclic organic silicon resin and fluorocarbon resin; and/or
The polar compound comprises one or more of methanol, ethanol, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, acetic acid, propanol, pyridine, tetramethyl ethylenediamine, acetone and triethylamine.
8. A method of producing a composite conductor according to claim 1, wherein,
in the conductive paste, the mass fraction of the metal powder is 40% -60%; and/or
The mass ratio of the resin to the polar compound is (10-30): (5-10).
9. The method of preparing a composite conductor according to claim 1, wherein the reagent further comprises a solvent; the solvent comprises one or more of tetrahydrofuran, benzene, toluene, xylene and n-butanol; the mass ratio of the resin to the solvent is (10-30): (15-35).
10. The method of preparing a composite conductor according to claim 1, wherein the reagent further comprises an auxiliary carbon source; the auxiliary carbon source comprises one or more of phenanthrene, anthracene, naphthalene and polymethyl methacrylate; the mass ratio of the resin to the auxiliary carbon source is (10-30): (1-3).
11. The method of preparing a composite conductor according to claim 1, wherein the reagent further comprises a metal oxide; the metal oxide comprises one or more of copper oxide and silver oxide; the mass ratio of the resin to the metal oxide is (10-30): (0.1 to 10).
12. The method of preparing a composite conductor according to claim 1, wherein the reagent further comprises a curing agent; the curing agent comprises one or more of an amine curing agent and an anhydride curing agent; the amine curing agent comprises one or more of polyamide curing agent, aliphatic amine curing agent, aromatic amine curing agent, alicyclic amine curing agent, polyether amine curing agent and imidazole curing agent; the anhydride curing agent comprises one or more of aromatic anhydride curing agents, aliphatic anhydride curing agents and alicyclic anhydride curing agents; the mass ratio of the resin to the curing agent is (10-30): (0.1 to 15).
13. The method for preparing a composite conductor according to claim 1, wherein the coating the composite conductor precursor with a graphene layer comprises: and (5) introducing protective gas, and performing first heat treatment to obtain carbide.
14. The method of manufacturing a composite conductor according to claim 13, wherein,
the temperature of the first heat treatment is 500-700 ℃; the time of the first heat treatment is 20-38 min; and/or
The first heat treatment is performed in a vacuum environment having a vacuum degree of 10 -3 kPa; and/or
The protective gas comprises one or more of nitrogen, helium, argon, xenon, krypton, neon and radon.
15. The method for preparing a composite conductor according to claim 13, wherein after obtaining the carbide, further comprising: and introducing auxiliary gas, and performing second heat treatment to obtain the graphene layer.
16. The method of manufacturing a composite conductor according to claim 15, wherein,
the temperature of the second heat treatment is 800-1050 ℃; the second heat treatment time is 20-50 min; and/or
The assist gas comprises hydrogen; the flow rate of the auxiliary gas is 10 sccm-500 sccm; and/or
The number of the graphene layers is 3-8.
17. The method for manufacturing a composite conductor according to claim 1, wherein the temperature of the heat press treatment of the composite conductor preform is 800 ℃ to 950 ℃; the time of the hot pressing treatment of the composite conductor preform is 20-50 min; the pressure of the hot pressing treatment of the composite conductor preform is 200-1200 kN.
18. A composite conductor prepared by the method for preparing a composite conductor according to any one of claims 1 to 17, the composite conductor comprising:
the metal powder is orderly arranged in the conductive direction under the action of the electric field driving force; and
and the graphene is filled between the orderly arranged metal powder and the metal powder, and coats the metal powder to form a graphene layer.
19. The composite conductor of claim 18, wherein the material of the metal powder comprises one or more of copper, silver, copper alloy, silver alloy; the shape of the metal powder comprises one or more of dendritic, rod-like, flake-like, cube-like, spherical or nearly spherical; the average particle diameter of the metal powder is 10-100 mu m.
20. The composite conductor of claim 18, wherein the number of graphene layers is 3-8.
21. A conductive element comprising a composite conductor prepared by the method of preparing a composite conductor according to any one of claims 1 to 17, or comprising a composite conductor according to any one of claims 18 to 20; the conductive element includes a wire or an electrical contact conductor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311687648.6A CN117393234B (en) | 2023-12-11 | 2023-12-11 | Composite conductor, preparation method thereof and conductive element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5399330A (en) * | 1991-02-15 | 1995-03-21 | Yazaki Corp. | Carbon thread and process for producing it |
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5399330A (en) * | 1991-02-15 | 1995-03-21 | Yazaki Corp. | Carbon thread and process for producing it |
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
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