CN105695783B - A kind of graphene/Cu-base composites and preparation method thereof - Google Patents
A kind of graphene/Cu-base composites and preparation method thereof Download PDFInfo
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- CN105695783B CN105695783B CN201610054525.2A CN201610054525A CN105695783B CN 105695783 B CN105695783 B CN 105695783B CN 201610054525 A CN201610054525 A CN 201610054525A CN 105695783 B CN105695783 B CN 105695783B
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- graphene
- copper
- alkene
- cladding
- rod
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- 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
Abstract
The present invention provides a kind of graphene/Cu-base composites and preparation method thereof, carries out leaching copper to graphene base body by hot isostatic pressing technique and prepares graphene/copper composite material.Specific embodiment is：Graphene powder is mixed with a small amount of binding agent, is suppressed on a hydraulic press after being mixed evenly, controls suitable pressure size, pressed compact is made；By obtained pressed compact in N2Sintered in protective atmosphere sintering furnace, graphene precast body is made；Graphene precast body there is into N2Impregnated in the copper melt of protective atmosphere, then cooling obtains Cu-cladding Al Rod alkene ingot bar；The boat for containing Cu-cladding Al Rod alkene ingot bar is placed in hot isostatic press, carries out high temperature insostatic pressing (HIP) impregnation, copper liquid body is filled graphene briquet inner pore, cools down and just obtain graphene/Cu-base composites.Its advantage is：Method provided by the invention has simple process, and cost is low, the advantages that being adapted to mass produce.Prepared graphene/Cu-base composites consistency is high, not only good mechanical performance but also has good heat conduction, conduction and self-lubricating property, new application prospect is hewed out for the material.
Description
Technical field
The present invention relates to industrial technical field, and in particular to a kind of graphene/Cu-base composites and preparation method thereof.
Background technology
Metal-impregnated carbon graphite material considerably improves mechanical strength and wearability, has dropped the porosity, enhanced and answer
The specific load of used time, heat conduction and electric conductivity etc. are improved, in terms of the machinery carbon that some technical parameters require higher
To extensive use.Graphene is the single layer structure of graphite, relative to graphite, graphene have more excellent heat conduction, heat conduction and
Mechanical property.And the batch production of graphene industrially at present, is had been realized in by physics and chemical method, graphene
Cost is prepared to be greatly lowered.
Copper and copper alloy are widely used to navigate due to preferable electrical and thermal conductivity, corrosion resistance and the advantages that be easy to shaping
The fields such as empty space flight, mechanical industry, derived energy chemical, electric and electronic and national defense industry.Copper as traditional conduction, Heat Conduction Material,
It is that graphene gives full play to one of optimum carrier material of efficiency.Graphene base body leaching copper is prepared by hot isostatic pressing technique
Graphene/copper composite material, realize " combination among the strong ones ", composite can be made to obtain high intensity, highly conductive, highly thermally conductive, low-heat
The excellent combination property such as expansion, lightweight, it more difficult to can valuable be graphene pliability it is good, make composite be readily able to process
And processing, in summary, graphene/copper composite material is expected to turn into high-performance copper based composites of new generation.
The content of the invention
It is an object of the invention to provide a kind of preparation side of suitable large-scale industrial production graphene/Cu-base composites
Method, copper-based material performance is improved, widen its application.
Specific embodiment step is：
a：Graphene powder and 1-5% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, are mixed evenly
Suppressed on a hydraulic press afterwards, control pressure 200-300MPa, pressed compact is made；
b：By obtained pressed compact in N2800-1000 DEG C of sintering in protective atmosphere sintering furnace, is made graphene precast body；
c：Graphene is prefabricated in N2Immerse in 1200-1400 DEG C of copper melt and impregnated under protective atmosphere, it is then cold
But Cu-cladding Al Rod alkene ingot bar is obtained；
d：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out heat etc.
Static pressure impregnation.The first baker under 80-180Pa is to 350-500 DEG C；Logical Ar gas 0.1-0.2MPa, are warming up to copper and fully melt；
Disconnected heating power supply, it is 100-800Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1200-1380 DEG C, 80-90MPa
After insulation, pressurize 1-2 hours, furnace cooling is powered off；
e：Power-off cools to less than 100 DEG C with the furnace and come out of the stove, and the copper pulled down with Vehicle Processing around leaching copper graphene, soaks material after copper
Material density was more originally significantly improved, and its apparent porosity declines.
Embodiment
Embodiment 1
Step of preparation process：
(1)：Graphene powder and 2% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, are mixed evenly
Suppressed on a hydraulic press afterwards, control pressure 200MPa, pressed compact is made；
(2)：By obtained pressed compact in N2800 DEG C of sintering in protective atmosphere sintering furnace, are made graphene precast body；
(3)：By graphene precast body in N2Immerse in 1400 DEG C of copper melt and impregnated under protective atmosphere, then cooling
Obtain Cu-cladding Al Rod alkene ingot bar；
(4)：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out heat
Isostatic pressed impregnation.The first baker under 100Pa is to 350 DEG C；Logical Ar gas 0.1MPa, are warming up to copper and fully melt；Disconnected heating electricity
Source, it is 300Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1200 DEG C, 80MPa after insulation, pressurize 1 hour, power-off
Furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
Embodiment 2
Step of preparation process：
(1)：Graphene powder and 3% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, are mixed evenly
Suppressed on a hydraulic press afterwards, control pressure 250MPa, pressed compact is made；
(2)：By obtained pressed compact in N2900 DEG C of sintering in protective atmosphere sintering furnace, are made graphene precast body；
(3)：By graphene precast body in N2Immerse in 1300 DEG C of copper melt and impregnated under protective atmosphere, then cooling
Obtain Cu-cladding Al Rod alkene ingot bar；
(4)：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out heat
Isostatic pressed impregnation.The first baker under 150Pa is to 400 DEG C；Logical Ar gas 0.15MPa, are warming up to copper and fully melt；Disconnected heating electricity
Source, it is 200Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1350 DEG C, 85MPa after insulation, pressurize 1.5 hours, is broken
Electric furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
Embodiment 3
Step of preparation process：
(1)：Graphene powder and 5% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, are mixed evenly
Suppressed on a hydraulic press afterwards, control pressure 300MPa, pressed compact is made；
(2)：By obtained pressed compact in N21000 DEG C of sintering in protective atmosphere sintering furnace, are made graphene precast body；
(3)：By graphene precast body in N2Immerse in 1300 DEG C of copper melt and impregnated under protective atmosphere, then cooling
Obtain Cu-cladding Al Rod alkene ingot bar；
(4)：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out heat
Isostatic pressed impregnation.The first baker under 180Pa is to 450 DEG C；Logical Ar gas 0.2MPa, are warming up to copper and fully melt；Disconnected heating electricity
Source, it is 500Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1380 DEG C, 90MPa after insulation, pressurize 2 hours, power-off
Furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
Embodiment 4
Step of preparation process：
(6)：Graphene powder and 6% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, are mixed evenly
Suppressed on a hydraulic press afterwards, control pressure 250MPa, pressed compact is made；
(7)：By obtained pressed compact in N21000 DEG C of sintering in protective atmosphere sintering furnace, are made graphene precast body；
(8)：By graphene precast body in N2Immerse in 1200 DEG C of copper melt and impregnated under protective atmosphere, then cooling
Obtain Cu-cladding Al Rod alkene ingot bar；
(9)：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out heat
Isostatic pressed impregnation.The first baker under 180Pa is to 500 DEG C；Logical Ar gas 0.2MPa, are warming up to copper and fully melt；Disconnected heating electricity
Source, it is 500Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1200 DEG C, 90MPa after insulation, pressurize 1.5 hours, is broken
Electric furnace cooling；
(10) power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
Embodiment 5
Step of preparation process：
(11)：Graphene powder and 8% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, mixed equal
Suppressed on a hydraulic press after even, control pressure 300MPa, pressed compact is made；
(12)：By obtained pressed compact in N2900 DEG C of sintering in protective atmosphere sintering furnace, are made graphene precast body；
(13)：By graphene precast body in N2Immerse in 1200 DEG C of copper melt and impregnated under protective atmosphere, it is then cold
But Cu-cladding Al Rod alkene ingot bar is obtained；
(14)：The boat for containing Cu-cladding Al Rod alkene ingot bar and Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carried out
High temperature insostatic pressing (HIP) impregnation.The first baker under 80Pa is to 400 DEG C；Logical Ar gas 0.1MPa, are warming up to copper and fully melt；Disconnected heating electricity
Source, it is 800Pa to be evacuated to vacuum；Ar and electrified regulation are filled, under 1250 DEG C, 80MPa after insulation, pressurize 1 hour, power-off
Furnace cooling；
(15) power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
Finally it should be noted that：Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
Among the obvious changes or variations that Shen goes out is still in protection scope of the present invention.
Claims (1)
1. a kind of preparation method of suitable large-scale industrial production graphene/Cu-base composites, specific embodiment step
For：
Step 1：Graphene powder and 1-5% polyvinyl alcohol (PVA) binding agent are stirred according to mass percent, mixed equal
Suppressed on a hydraulic press after even, control pressure 200-300MPa, pressed compact is made；
Step 2：By obtained pressed compact in N2800-1000 DEG C of sintering in protective atmosphere sintering furnace, is made graphene precast body；
Step 3：By graphene precast body in N2Immerse in 1200-1400 DEG C of copper melt and impregnated under protective atmosphere, then
Cooling obtains Cu-cladding Al Rod alkene ingot bar；
Step 4：The boat for containing Cu-cladding Al Rod alkene ingot bar is placed in hot isostatic press, carries out high temperature insostatic pressing (HIP) impregnation, first
Baker is to 350-500 DEG C under 80-180Pa；Logical Ar gas 0.1-0.2MPa, are warming up to copper and fully melt；Disconnected heating power supply, take out true
Sky to vacuum is 100-800Pa；Ar and electrified regulation are filled, insulation, pressurize 1-2 hours under 1200-1380 DEG C, 80-90MPa
Afterwards, furnace cooling is powered off；
Step 5：Power-off cools to less than 100 DEG C with the furnace and come out of the stove, the copper pulled down with Vehicle Processing around leaching copper graphene, after soaking copper
Density of material was more originally significantly improved, and its apparent porosity declines.
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| CN201610054525.2A CN105695783B (en) | 2016-01-21 | 2016-01-21 | A kind of graphene/Cu-base composites and preparation method thereof |
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| CN201610054525.2A CN105695783B (en) | 2016-01-21 | 2016-01-21 | A kind of graphene/Cu-base composites and preparation method thereof |
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| CN105695783A CN105695783A (en) | 2016-06-22 |
| CN105695783B true CN105695783B (en) | 2018-01-16 |
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| CN107245590B (en) * | 2017-06-14 | 2019-04-23 | 上海电缆研究所有限公司 | Copper-graphite alkene composite material and preparation method |
| CN107705874A (en) * | 2017-11-08 | 2018-02-16 | 无锡市长城电线电缆有限公司 | A kind of compounding method of compound copper conductor |
| CN108002844B (en) * | 2017-11-22 | 2020-11-03 | 中国科学院兰州化学物理研究所 | Wide-temperature-range self-lubricating sialon-based composite material |
| CN110079784A (en) * | 2018-01-26 | 2019-08-02 | 中车工业研究院有限公司 | The preparation method and copper-base graphite alkene composite material of copper-base graphite alkene composite material |
| CN108220950A (en) * | 2018-03-07 | 2018-06-29 | 西迪技术股份有限公司 | A kind of face coat and preparation method for hydraulic motor |
| CN111074243A (en) * | 2020-01-02 | 2020-04-28 | 中国科学院深圳先进技术研究院 | Method for plating silver on surface of carbon material |
| CN111705231A (en) * | 2020-07-03 | 2020-09-25 | 毛金昌 | Nickel-based copper-clad graphite self-lubricating composite material and sintering method thereof |
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| CN102146552B (en) * | 2010-02-09 | 2012-09-05 | 航天材料及工艺研究所 | Copper/graphite compound material and preparation method thereof |
| CN102730671B (en) * | 2012-06-14 | 2014-02-05 | 天津大学 | Copper-graphene composite material and method for preparation of graphene film on copper-based metal surface |
| CN105063405A (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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