CN112080666A - Preparation formula and preparation method of composite material with high conductivity - Google Patents
Preparation formula and preparation method of composite material with high conductivity Download PDFInfo
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- CN112080666A CN112080666A CN201910506826.8A CN201910506826A CN112080666A CN 112080666 A CN112080666 A CN 112080666A CN 201910506826 A CN201910506826 A CN 201910506826A CN 112080666 A CN112080666 A CN 112080666A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/04—Alloys based on copper with zinc as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- 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
- H01B1/026—Alloys based on copper
Abstract
The invention relates to a raw material and a method for preparing a composite material with high conductivity, wherein the formula comprises alloy atomized powder and graphene nanoplatelets, and the ratio of the alloy atomized powder to the graphene nanoplatelets is 100: 0.5; the alloy gas atomized powder comprises the following components in percentage by mass: 5.9 percent of zinc powder, 2.2 percent of magnesium powder, 1.7 percent of silver powder, 0.35 percent of iron powder, 0.1 percent of silicon powder and the balance of copper powder. During manufacturing, the raw materials are weighed according to a formula, and then the graphene nanosheets are dispersed into an absolute ethyl alcohol solution to prepare a graphene solution; and then adding the alloy gas atomized powder into the graphene solution, packaging the graphene solution in a ball milling tank, carrying out ball milling to form slurry, stirring and drying the slurry subjected to ball milling to be in a semi-dry state, and finally sintering to obtain the composite material with ultralow resistance, high strength, good ductility, friction resistance, diamagnetism, antioxidation and wide application range and high conductivity.
Description
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to a preparation formula and a preparation method of a composite material with high conductive performance.
Background
At present, the existing conductive material in the market has resistance, and the resistance value is relatively large, so that the conductivity is seriously influenced, the application range is extremely limited, and the market demand of modern high technology cannot be met.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation formula of a composite material with ultralow resistance, high strength, good ductility, friction resistance, diamagnetism and oxidation resistance, extremely wide application range and extremely strong market competitiveness and high conductivity, and a preparation method of the composite material.
In order to solve the technical problems, the invention adopts the following technical scheme:
the formula for preparing the composite material with high conductivity comprises alloy atomized powder and graphene nanoplatelets, wherein the ratio of the alloy atomized powder to the graphene nanoplatelets is 100: 0.5; wherein the content of the first and second substances,
the alloy gas atomized powder comprises the following components in percentage by mass: 5.9 percent of zinc powder, 2.2 percent of magnesium powder, 1.7 percent of silver powder, 0.35 percent of iron powder, 0.1 percent of silicon powder and the balance of copper powder.
Further, the graphene nanoplatelets are graphene nanoplatelets, and are prepared by taking natural graphite with the purity of 99.9% as a raw material and adopting an improved Hummer method to prepare graphene oxide nano powder, adding hydrazine hydrate, stirring, reducing and fully drying.
Further, the average particle diameter of the zinc powder, the magnesium powder, the silver powder, the iron powder, the silicon powder and the copper powder is 9 μm, and the zinc powder, the magnesium powder, the silver powder, the iron powder, the silicon powder and the copper powder are all formed into nearly flaky particles.
A method for manufacturing a composite material with high conductive performance sequentially comprises the following steps:
weighing raw materials, namely weighing alloy atomized powder and graphene nanosheets according to the formula of the claim 1, 2 or 3;
mechanical ball milling, namely firstly dispersing graphene nanosheets into an absolute ethyl alcohol solution, and uniformly dispersing the graphene nanosheets by adopting ultrasonic oscillation to prepare a graphene solution; adding the alloy gas atomized powder into the graphene solution, and encapsulating the graphene solution in a ball milling tank for ball milling to form slurry; finally, stirring and drying the ball-milled slurry to be in a semi-dry state;
and (4) sintering, namely filling the semi-dry slurry into a mold and sintering.
Further, adding the alloy gas atomized powder into the graphene solution, and encapsulating the graphene solution in a ball milling tank for ball milling, wherein the ball-material ratio is 6:1, and the rotating speed is 300 r.min-1The ball milling time was 12 hours.
Further, the step of putting the semi-dry slurry into a mold and sintering specifically comprises the following steps:
firstly, feeding the slurry into a mold, feeding the slurry into a furnace, namely, feeding the slurry into the mold in a semi-dry state, and placing the slurry on the inner wall of a furnace body of sintering furnace equipment;
then, pre-pressing treatment, namely placing the die between an upper electrode and a lower electrode of the furnace body, and pressurizing through an oil pressure system;
then, vacuum treatment, namely, vacuumizing the cavity of the furnace body until the resistance unit of the composite vacuum gauge is 5.3E0pa and the displacement value is unchanged, so that liquid or alcohol of composite powder on the inner wall of the furnace can be removed;
then sintering, namely sintering the semi-dry slurry in the die by adopting a two-stage heating mode, namely preheating at 600 ℃, and then preserving heat under the environment of 40MPa to finish sintering;
and finally, cooling and demolding, namely taking out the sintered mold, and putting the mold into a hydraulic demolding device for demolding at room temperature below 23 ℃ to obtain the composite material with high conductive performance.
Further, the mold is a graphite mold, and a graphite paper layer is arranged on the inner surface of the graphite mold.
Further, the sintering furnace equipment is SPS discharge plasma sintering furnace equipment.
Furthermore, after the composite material with high conductivity is prepared, MPT grinding and polishing head equipment can be adopted to carry out polishing and grinding treatment on the surface of the composite material.
Further, before the pre-pressing treatment, the furnace body is firstly pumped until the resistance unit of the composite vacuum gauge shows 1.0E2 pa.
The invention has the beneficial effects that:
according to the technical scheme, the composite material with ultralow resistance, high strength, good ductility, friction resistance, diamagnetism and antioxidation and high conductivity can be produced and processed, can be applied to products such as strong current, weak current, diamagnetism and the like, and has a wide application range and strong market competitiveness.
Drawings
FIG. 1 is a schematic flow chart of a method for making a composite material with high electrical conductivity according to the present invention;
FIG. 2 is a schematic flow chart of sintering in the method for manufacturing a composite material with high conductivity according to the present invention;
FIG. 3 is a graph showing the results of tensile testing of a composite material made by the method of the present invention;
FIG. 4 is a graph showing the melting point test results of a composite material manufactured by the method for manufacturing a composite material with high conductive performance according to the present invention;
FIG. 5 is a metallographic structure of a composite material manufactured by the method for manufacturing a composite material with high electrical conductivity according to the present invention;
FIG. 6 is a further metallographic structure of a composite material produced by the method of the invention for producing a composite material with high electrical conductivity;
FIG. 7 is a further metallographic structure of a composite material produced by the method of the invention for producing a composite material with high electrical conductivity;
FIG. 8 is an SEM photograph of tensile fracture of a composite material manufactured by the method for manufacturing a composite material with high conductive performance;
FIG. 9 is an SEM photograph of a tensile fracture of a composite material manufactured by the method for manufacturing a composite material with high conductivity according to the present invention;
FIG. 10 is an SEM photograph of a tensile fracture of a composite material manufactured by the method for manufacturing a composite material with high electrical conductivity according to the present invention;
FIG. 11 is a graph showing the results of magnetic property tests of a composite material manufactured by the method for manufacturing a composite material with high conductive properties according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation formula of the composite material with high conductivity comprises alloy atomized powder and graphene nanoplatelets, wherein the ratio of the alloy atomized powder to the graphene nanoplatelets is 100: 0.5. Wherein the content of the first and second substances,
the alloy gas atomized powder comprises the following components in percentage by mass: 5.9% of zinc powder, 2.2% of magnesium powder, 1.7% of silver powder, 0.35% of iron powder, 0.1% of silicon powder and the balance of copper powder; the average grain diameter of the zinc powder, the magnesium powder, the silver powder, the iron powder, the silicon powder and the copper powder is 9 mu m, and the zinc powder, the magnesium powder, the silver powder, the iron powder, the silicon powder and the copper powder are all multi-flaky particles.
The graphene nanoplatelets are graphene nanoplatelets, and are obtained by taking natural graphite with the purity of 99.9% as a raw material, preparing graphene oxide nano powder by adopting an improved Hummer method, adding hydrazine hydrate, stirring and reducing (for example, mechanically stirring and reducing at 98 ℃) and fully drying.
As shown in fig. 1, the method for manufacturing a composite material with high conductive performance according to the present invention sequentially comprises the following steps:
s100, weighing raw materials, namely weighing the alloy atomized powder and the graphene nanosheets according to the formula.
S200, mechanical ball milling, namely firstly dispersing graphene nanosheets into an absolute ethyl alcohol solution, and uniformly dispersing the graphene nanosheets by adopting ultrasonic oscillation to prepare a graphene solution; followed by gas atomization of the alloyAdding the powder into the graphene solution, packaging the graphene solution in a ball milling tank, and carrying out ball milling to form slurry; finally, stirring and drying the ball-milled slurry to be in a semi-dry state; wherein, the alloy gas atomized powder is added into the graphene solution and packaged in a ball milling tank for ball milling, the ball-material ratio is 6:1, and the rotating speed is 300 r.min-1The ball milling time was 12 hours.
And S300, sintering, namely filling the semi-dry slurry into a mold and sintering. As shown in fig. 2, the method specifically includes the following steps:
s301, putting the slurry into a mold, putting the slurry into a furnace, namely putting the slurry in a semi-dry state into the mold and placing the slurry on the inner wall of a furnace body of sintering furnace equipment; the mold is a graphite mold, and a graphite paper layer is arranged on the inner surface of the graphite mold; the sintering furnace equipment is SPS discharge plasma sintering furnace equipment.
S302, performing prepressing treatment, namely placing a mould between an upper electrode and a lower electrode of a furnace body, and pressurizing through an oil pressure system;
and S303, performing vacuum treatment, namely vacuumizing the cavity of the furnace body until the resistance unit of the composite vacuum gauge is 5.3E0pa, and removing liquid or alcohol of composite powder on the inner wall of the furnace without changing the displacement value.
And S304, sintering, namely sintering the semi-dry slurry in the mold by adopting a two-stage heating mode, namely preheating at 600 ℃, and then preserving heat under the environment of 40MPa to finish sintering.
The current and voltage change values of the sintering process at each stage are as shown in the table I, and the sintering principle is as follows: the pulse heavy current is directly applied to a conductive mould (graphite mould) and a material (slurry in a semi-dry state), partial current of the material and gaps activates the surfaces of crystal grains, partial discharge is generated among pores, plasma is generated, and the surfaces of powder particles are activated and heated; meanwhile, the mold is heated by partial current of the mold, so that the mold starts to transfer heat to the material, the temperature of the material rises, the material starts to shrink, and a certain density is generated.
Table one:
| voltage of | 2.5V | 2.6V | 2.6V | 2.9V |
| Electric current | 1612A | 1683A | 1810A | 1926A |
And S305, cooling, demolding, namely taking out the sintered mold, putting the mold into a hydraulic demolding device for demolding at room temperature below 23 ℃, so as to prepare the composite material with high conductivity, wherein the surface of the composite material can be subjected to preliminary graphite removal in the process.
And S306, polishing and grinding, namely polishing and grinding the surface of the composite material by adopting MPT grinding and polishing head equipment.
In addition, before the pre-pressing treatment, the furnace body is firstly pumped until the resistance unit of the composite vacuum gauge is 1.0E2 pa.
The ultra-low resistance (the resistance value is 2.4 multiplied by 10) can be produced and processed by adopting the manufacturing formula and the manufacturing method of the invention through detection of related detection mechanisms-11Ω · m), high strength and ductility (see fig. 3-10), friction resistance (coefficient of friction 0.462), diamagnetism (see fig. 11), oxidation resistance, and high conductivity, and can be used in a high-voltage (for example: power generation, transmission, and energy storage for large currents), weak current (for example: superconducting computer, superconducting microwave device, superconducting antenna) and diamagnetismThe product (such as thermonuclear fusion reactor, magnetic suspension train) and the like, has wide application range and strong market competitiveness.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation formula of the composite material with high conductivity is characterized by comprising alloy atomized powder and graphene nanoplatelets, wherein the ratio of the alloy atomized powder to the graphene nanoplatelets is 100: 0.5; wherein the content of the first and second substances,
the alloy gas atomized powder comprises the following components in percentage by mass: 5.9 percent of zinc powder, 2.2 percent of magnesium powder, 1.7 percent of silver powder, 0.35 percent of iron powder, 0.1 percent of silicon powder and the balance of copper powder.
2. The formula of claim 1, wherein the graphene nanoplatelets are graphene nanoplatelets, and are obtained by preparing graphene oxide nanopowder from natural graphite with a purity of 99.9% by an improved Hummer method, adding hydrazine hydrate, stirring for reduction, and fully drying.
3. The formulation of claim 1, wherein the zinc powder, the magnesium powder, the silver powder, the iron powder, the silicon powder and the copper powder have an average particle size of 9 μm and are all multi-lamellar particles.
4. The preparation method of the composite material with high conductive performance is characterized by sequentially comprising the following steps of:
weighing raw materials, namely weighing alloy atomized powder and graphene nanosheets according to the formula of the claim 1, 2 or 3;
mechanical ball milling, namely firstly dispersing graphene nanosheets into an absolute ethyl alcohol solution, and uniformly dispersing the graphene nanosheets by adopting ultrasonic oscillation to prepare a graphene solution; adding the alloy gas atomized powder into the graphene solution, and encapsulating the graphene solution in a ball milling tank for ball milling to form slurry; finally, stirring and drying the ball-milled slurry to be in a semi-dry state;
and (4) sintering, namely filling the semi-dry slurry into a mold and sintering.
5. The method of claim 4, wherein the alloy gas atomized powder is added into the graphene solution and encapsulated in a ball milling pot for ball milling at a ball-to-material ratio of 6:1 and a rotation speed of 300 r-min-1The ball milling time was 12 hours.
6. The method as claimed in claim 4, wherein the step of filling the semi-dry slurry into the mold and sintering comprises the following steps:
firstly, feeding the slurry into a mold, feeding the slurry into a furnace, namely, feeding the slurry into the mold in a semi-dry state, and placing the slurry on the inner wall of a furnace body of sintering furnace equipment;
then, pre-pressing treatment, namely placing the die between an upper electrode and a lower electrode of the furnace body, and pressurizing through an oil pressure system;
then, vacuum treatment, namely, vacuumizing the cavity of the furnace body until the resistance unit of the composite vacuum gauge is 5.3E0pa, and the displacement value is unchanged, so that the liquid or alcohol of the composite powder on the inner wall of the furnace can be removed;
then sintering, namely sintering the semi-dry slurry in the die by adopting a two-stage heating mode, namely preheating at 600 ℃, and then preserving heat under the environment of 40MPa to finish sintering;
and finally, cooling and demolding, namely taking out the sintered mold, and putting the mold into a hydraulic demolding device for demolding at room temperature below 23 ℃ to obtain the composite material with high conductive performance.
7. The method of claim 6, wherein the mold is a graphite mold having a graphite paper layer disposed on an inner surface thereof.
8. The method according to claim 6, wherein the sintering furnace equipment is SPS discharge plasma sintering furnace equipment.
9. The method as claimed in claim 6, wherein after the composite material with high conductivity is obtained, the surface of the composite material is polished and smoothed by MPT polishing head equipment.
10. The method of claim 6, wherein before the pre-pressing treatment, the furnace body is evacuated until the resistance cell of the composite vacuum gauge is 1.0E2 pa.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571855A (en) * | 2001-10-18 | 2005-01-26 | 加拿大电子粉末公司 | Powder for laminated ceramic capacitor internal electrode |
| CN101680056A (en) * | 2007-03-28 | 2010-03-24 | 古河电气工业株式会社 | Copper alloy material, and method for production thereof |
| US20110240180A1 (en) * | 2010-04-05 | 2011-10-06 | Dowa Metaltech Co., Ltd. | Copper alloy sheet, manufacturing method of copper alloy sheet, and electric/electronic component |
| CN105063403A (en) * | 2015-06-25 | 2015-11-18 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of copper matrix graphene alloy |
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- 2019-06-12 CN CN201910506826.8A patent/CN112080666A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571855A (en) * | 2001-10-18 | 2005-01-26 | 加拿大电子粉末公司 | Powder for laminated ceramic capacitor internal electrode |
| CN101680056A (en) * | 2007-03-28 | 2010-03-24 | 古河电气工业株式会社 | Copper alloy material, and method for production thereof |
| US20110240180A1 (en) * | 2010-04-05 | 2011-10-06 | Dowa Metaltech Co., Ltd. | Copper alloy sheet, manufacturing method of copper alloy sheet, and electric/electronic component |
| CN105063403A (en) * | 2015-06-25 | 2015-11-18 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of copper matrix graphene alloy |
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Application publication date: 20201215 |