CN105695783A - Graphene/copper-based composite and preparation method thereof - Google Patents
Graphene/copper-based composite and preparation method thereof Download PDFInfo
- Publication number
- CN105695783A CN105695783A CN201610054525.2A CN201610054525A CN105695783A CN 105695783 A CN105695783 A CN 105695783A CN 201610054525 A CN201610054525 A CN 201610054525A CN 105695783 A CN105695783 A CN 105695783A
- Authority
- CN
- China
- Prior art keywords
- graphene
- copper
- preparation
- protective atmosphere
- hot isostatic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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 invention provides a graphene/copper-based composite and a preparation method thereof. Copper immersion plating is conducted on graphene matrices through the hot isostatic pressure technique, and the graphene/copper composite is prepared. The preparation method specifically comprises the steps that graphene powder and a small amount of binding agents are mixed and then pressed on a hydraulic machine after being mixed uniformly, the pressure is controlled to be proper, and a compact is obtained; the obtained compact is sintered in a sintering furnace under the N2 protective atmosphere, and a graphene prefabricated part is obtained; the graphene prefabricated part is soaked in molten copper under the N2 protective atmosphere, and a copper-coated graphene ingot is obtained after cooling; and a boat containing the copper-coated graphene ingot is placed in a hot isostatic press, hot isostatic pressure soaking is conducted, holes in the graphene compact are made to be filled with the molten copper, and the graphene/copper-based composite is obtained after cooling. The preparation method has the advantages of being simple and convenient in technique, low in cost, suitable for large-scale production and the like. The prepared graphene/copper-based composite is high in compactness, excellent in mechanical property and good in heat conduction performance, electric conduction performance and self-lubricating performance, and new application prospects are developed for the composite.
Description
Technical field
The present invention relates to industrial technical field, be specifically related 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, dropped the porosity, specific load when enhancing application, improve heat conduction and electric conductivity etc., requires to be used widely in higher machinery carbon at some technical parameters。Graphene is the single layer structure of graphite, and relative to graphite, Graphene has more excellent heat conduction, heat conduction and mechanical property。And at present, the industrial batch production being had been realized in Graphene by physics and chemical method, the preparation cost of Graphene obtains and is greatly lowered。
Copper and copper alloy due to good electrical and thermal conductivity, corrosion resistance and are prone to the advantages such as molding, are widely used to the fields such as Aero-Space, mechanical industry, derived energy chemical, electric and electronic and national defense industry。Copper, as traditional conduction, Heat Conduction Material, is one of Graphene optimum carrier material giving full play to efficiency。By hot isostatic pressing technique, graphene base body is soaked copper and prepare graphene/copper composite material, realize " combination among the strong ones ", composite can be made to obtain the combination property that high intensity, high connductivity, highly thermally conductive, low-thermal-expansion, lightweight etc. are excellent, the pliability of more estimable is Graphene is good, composite is made to be readily able to processing and process, in sum, graphene/copper composite material is expected to become a new generation's high-performance copper based composites。
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of applicable large-scale industrial production Graphene/Cu-base composites, improves copper-based material serviceability, widens its range of application。
Specific embodiment step is:
A: according to mass percent, Graphene powder is mixed with the stirring of 1-5% polyvinyl alcohol (PVA) binding agent, suppress on a hydraulic press after being mixed evenly, control pressure 200-300MPa, prepare pressed compact；
B: by prepared pressed compact at N2800-1000 DEG C of sintering in protective atmosphere sintering furnace, prepares Graphene precast body；
C: by prefabricated for Graphene at N2Immersing under protective atmosphere in the copper melt of 1200-1400 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
D: the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 80-180Pa baker to 350-500 DEG C；Logical Ar gas 0.1-0.2MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 100-800Pa；Fill Ar electrified regulation, 1200-1380 DEG C, insulation under 80-90MPa, after pressurize 1-2 hour, power-off furnace cooling；
E: power-off cools to less than 100 DEG C with the furnace and comes out of the stove, pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Detailed description of the invention
Embodiment 1
Step of preparation process:
(1): according to mass percent, Graphene powder and 2% polyvinyl alcohol (PVA) binding agent are stirred mixing, suppress on a hydraulic press after being mixed evenly, control pressure 200MPa, prepare pressed compact；
(2): by prepared pressed compact at N2800 DEG C of sintering in protective atmosphere sintering furnace, prepare Graphene precast body；
(3): by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1400 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
(4): the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 100Pa baker to 350 DEG C；Logical Ar gas 0.1MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 300Pa；Fill Ar electrified regulation, 1200 DEG C, insulation under 80MPa, after pressurize 1 hour, power-off furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and comes out of the stove, and pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Embodiment 2
Step of preparation process:
(1): according to mass percent, Graphene powder and 3% polyvinyl alcohol (PVA) binding agent are stirred mixing, suppress on a hydraulic press after being mixed evenly, control pressure 250MPa, prepare pressed compact；
(2): by prepared pressed compact at N2900 DEG C of sintering in protective atmosphere sintering furnace, prepare Graphene precast body；
(3): by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1300 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
(4): the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 150Pa baker to 400 DEG C；Logical Ar gas 0.15MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 200Pa；Fill Ar electrified regulation, 1350 DEG C, insulation under 85MPa, after pressurize 1.5 hours, power-off furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and comes out of the stove, and pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Embodiment 3
Step of preparation process:
(1): according to mass percent, Graphene powder and 5% polyvinyl alcohol (PVA) binding agent are stirred mixing, suppress on a hydraulic press after being mixed evenly, control pressure 300MPa, prepare pressed compact；
(2): by prepared pressed compact at N21000 DEG C of sintering in protective atmosphere sintering furnace, prepare Graphene precast body；
(3): by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1300 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
(4): the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 180Pa baker to 450 DEG C；Logical Ar gas 0.2MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 500Pa；Fill Ar electrified regulation, 1380 DEG C, insulation under 90MPa, after pressurize 2 hours, power-off furnace cooling；
(5) power-off cools to less than 100 DEG C with the furnace and comes out of the stove, and pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Embodiment 4
Step of preparation process:
(6): according to mass percent, Graphene powder and 6% polyvinyl alcohol (PVA) binding agent are stirred mixing, suppress on a hydraulic press after being mixed evenly, control pressure 250MPa, prepare pressed compact；
(7): by prepared pressed compact at N21000 DEG C of sintering in protective atmosphere sintering furnace, prepare Graphene precast body；
(8): by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1200 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
(9): the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 180Pa baker to 500 DEG C；Logical Ar gas 0.2MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 500Pa；Fill Ar electrified regulation, 1200 DEG C, insulation under 90MPa, after pressurize 1.5 hours, power-off furnace cooling；
(10) power-off cools to less than 100 DEG C with the furnace and comes out of the stove, and pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Embodiment 5
Step of preparation process:
(11): according to mass percent, Graphene powder and 8% polyvinyl alcohol (PVA) binding agent are stirred mixing, suppress on a hydraulic press after being mixed evenly, control pressure 300MPa, prepare pressed compact；
(12): by prepared pressed compact at N2900 DEG C of sintering in protective atmosphere sintering furnace, prepare Graphene precast body；
(13): by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1200 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
(14): the boat and Cu-cladding Al Rod alkene ingot bar that contain Cu-cladding Al Rod alkene ingot bar are placed in hot isostatic press, carry out high temperature insostatic pressing (HIP) impregnation process。First under 80Pa baker to 400 DEG C；Logical Ar gas 0.1MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 800Pa；Fill Ar electrified regulation, 1250 DEG C, insulation under 80MPa, after pressurize 1 hour, power-off furnace cooling；
(15) power-off cools to less than 100 DEG C with the furnace and comes out of the stove, and pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Last it is noted that obvious, above-described embodiment is only for clearly demonstrating example of the present invention, and is not the restriction to embodiment。For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description。Here without also cannot all of embodiment be given exhaustive。And the apparent change thus amplified out or variation are still among protection scope of the present invention。
Claims (1)
1. a preparation method for applicable large-scale industrial production Graphene/Cu-base composites, specific embodiment step is:
Step one: according to mass percent, Graphene powder is mixed with the stirring of 1-5% polyvinyl alcohol (PVA) binding agent, suppress on a hydraulic press after being mixed evenly, control pressure 200-300MPa, prepare pressed compact；
Step 2: by prepared pressed compact at N2800-1000 DEG C of sintering in protective atmosphere sintering furnace, prepares Graphene precast body；
Step 3: by Graphene precast body at N2Immersing under protective atmosphere in the copper melt of 1200-1400 DEG C and impregnate, cooling subsequently obtains Cu-cladding Al Rod alkene ingot bar；
Step 4: the boat containing Cu-cladding Al Rod alkene ingot bar is placed in hot isostatic press, carries out high temperature insostatic pressing (HIP) impregnation process。First under 80-180Pa baker to 350-500 DEG C；Logical Ar gas 0.1-0.2MPa, is warming up to copper and fully melts；Disconnected heating power supply, being evacuated to vacuum is 100-800Pa；Fill Ar electrified regulation, 1200-1380 DEG C, insulation under 80-90MPa, after pressurize 1-2 hour, power-off furnace cooling；
Step 5: power-off cools to less than 100 DEG C with the furnace and comes out of the stove, pulls down the copper around leaching copper Graphene with Vehicle Processing, and after leaching copper, density of material was more originally significantly improved, and its apparent porosity declines。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054525.2A CN105695783B (en) | 2016-01-21 | 2016-01-21 | A kind of graphene/Cu-base composites and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054525.2A CN105695783B (en) | 2016-01-21 | 2016-01-21 | A kind of graphene/Cu-base composites and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105695783A true CN105695783A (en) | 2016-06-22 |
| CN105695783B CN105695783B (en) | 2018-01-16 |
Family
ID=56228550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610054525.2A Expired - Fee Related CN105695783B (en) | 2016-01-21 | 2016-01-21 | A kind of graphene/Cu-base composites and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105695783B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245590A (en) * | 2017-06-14 | 2017-10-13 | 上海电缆研究所有限公司 | Copper graphene 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 |
| CN108002844A (en) * | 2017-11-22 | 2018-05-08 | 中国科学院兰州化学物理研究所 | Grand based composites are matched in a kind of width temperature range self-lubricating |
| 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 |
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102146552A (en) * | 2010-02-09 | 2011-08-10 | 航天材料及工艺研究所 | Copper/graphite compound material and preparation method thereof |
| CN102730671A (en) * | 2012-06-14 | 2012-10-17 | 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 |
-
2016
- 2016-01-21 CN CN201610054525.2A patent/CN105695783B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102146552A (en) * | 2010-02-09 | 2011-08-10 | 航天材料及工艺研究所 | Copper/graphite compound material and preparation method thereof |
| CN102730671A (en) * | 2012-06-14 | 2012-10-17 | 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245590A (en) * | 2017-06-14 | 2017-10-13 | 上海电缆研究所有限公司 | Copper graphene composite material and preparation method |
| 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 |
| CN108002844A (en) * | 2017-11-22 | 2018-05-08 | 中国科学院兰州化学物理研究所 | Grand based composites are matched in a kind of width temperature range self-lubricating |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105695783B (en) | 2018-01-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105695783A (en) | Graphene/copper-based composite and preparation method thereof | |
| CN102628149B (en) | Preparation method of graphite whisker reinforced copper base composite material | |
| CN110157932B (en) | Preparation method of graphene modified copper-based electrical contact material based on in-situ synthesis | |
| CN108610081B (en) | Preparation method of C/C-Cu composite material | |
| CN106735207B (en) | A kind of preparation method of high-compactness Cu/CuCr gradient composites | |
| CN102586703B (en) | Method for preparing graphite whisker reinforced aluminum matrix composite material | |
| CN105503227B (en) | A kind of preparation method of stereo fabric enhancing silicon carbide diamond composite | |
| CN104874803A (en) | Method for preparing graphene/copper composite material by in-situ catalysis of solid carbon source on surfaces of copper powders | |
| CN101525730B (en) | Low-pressure auxiliary infiltration preparation method for high volume fraction C/Cu composite material | |
| CN103171207B (en) | Heat sink material and preparation method thereof | |
| CN114309596B (en) | Preparation method of high-heat-conductivity surface-metallized diamond/copper composite substrate | |
| CN103724032B (en) | A kind of two-dimensional fiber cloth strengthens silicon nitride-silicon carbide ceramic composite and preparation method thereof | |
| CN105648257B (en) | A kind of serialization high temperature insostatic pressing (HIP) dipping method for preparing large-size carbon carbon/carbon-copper composite material | |
| JP2000203973A (en) | Carbon-base metal composite material and its production | |
| CN104014792A (en) | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials | |
| CN103232257B (en) | Fast connection method of carbon/carbon composite material | |
| CN110284019B (en) | Method for directionally doping graphite in metal | |
| CN106884159B (en) | The method that carbon-coating coats the preparation method and its assistant brazing C/C composite material and metal of foam carbon/carbon-copper composite material | |
| CN104651658B (en) | Preparation method of novel copper-based composite material having high thermal conductivity | |
| CN104087776B (en) | Carbon dope strengthens the preparation method of W-Cu composite | |
| JP2006045596A (en) | Composite body with high thermal conductivity and low thermal expansion, and its manufacturing method | |
| CN106011510A (en) | Making method of copper-tungsten contact material | |
| CN106756190B (en) | Prepare the serialization hot isostatic pressing dipping method of high impregnation increment composite carbon-copper material | |
| CN107675108B (en) | A kind of preparation method of carbon-carbon/carbon-copper composite material | |
| CN101845567B (en) | Method for strengthening diamond powder degreasing blank subjected to injection molding by infiltrating Cu |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180116 Termination date: 20220121 |