CN107988513B - The method that graphene enhances Cu-base composites and its injection molding - Google Patents
The method that graphene enhances Cu-base composites and its injection molding Download PDFInfo
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- CN107988513B CN107988513B CN201711251633.XA CN201711251633A CN107988513B CN 107988513 B CN107988513 B CN 107988513B CN 201711251633 A CN201711251633 A CN 201711251633A CN 107988513 B CN107988513 B CN 107988513B
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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
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1042—Alloys containing non-metals starting from a melt by atomising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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Abstract
The present invention relates to the methods of a kind of graphene enhancing Cu-base composites and its injection molding, belong to transmission of electricity copper conductor production technical field.Industrial pure copper and Kufil, which are added in vacuum electromagnetic induction furnace, for it melts, and obtains copper liquid；It is injected into inert gas jet atomization device, copper liquid is atomized into droplet by high-pressure inert gas, graphene platelet is sprayed into spray chamber simultaneously, graphene platelet covers in the copper liquid drop of sinking, form copper/graphene mixture of liquid or half melt, through cooling ingot casting, and roll forming obtains graphene enhancing Cu-base composites.Preparation method simple possible in the present invention, step is easily operated, and the product of preparation has the advantages that Material texture is uniform, and compact structure, intensity is high, and wearability, electrical and thermal conductivity performance are good.
Description
Technical field
The present invention relates to the methods of a kind of graphene enhancing Cu-base composites and its injection molding, belong to transmission of electricity copper conductor
Production technical field.
Background technique
In recent years with the appearance of graphene, graphene and metal it is compound be in graphene nanocomposite material research very
One of the hot spot that important a part, the especially research of graphene-carbon/carbon-copper composite material are current investigation of materials field.Graphene
Addition can improve the performance of copper product electric-conductivity heat-conductivity high, moreover it is possible to improve the intensity, wearability, mechanical shock resistance of material
Energy, resistance fusion welding.Graphene is the film of single layer or several layers of carbon atom thickness, itself is easy to generate reunion, to influence stone
The useful effect of black alkene performance.
The main preparation method of copper-graphite alkene composite material is mainly powder metallurgy, but this needs higher processing temperature
Degree, pressure, particle is difficult to be evenly distributed, and material is easy to produce voidage.Also there is this to make in other ways at present.In such as
A kind of wire and cable preparation method with copper-graphite alkene complex phase conductor wire core of state patent CN 2014101943972, by graphite
Alkene disperses in copper-bath, using the plate of electrolysis method production copper-graphite alkene complex phase, leads by the production of rolling, drawing technique
Body core.These methods are all relatively difficult to resolve certainly graphene bad dispersibility in Copper substrate, are easy the technical problems such as reunion.
Summary of the invention
Present invention aim to address grapheme materials be uniformly dispersed in Copper substrate it is poor, be easy to reunite, difficult continuous production
Problem provides the method for a kind of graphene enhancing Cu-base composites and its injection molding.
Technical solution of the present invention, graphene enhance Cu-base composites, and formula rate is as follows by mass percentage: stone
Black alkene 0.05%~5%, silver 0.05%~0.2%, impurity element summation≤0.05%, remaining is copper；
The impurity element is specific as follows: iron≤0.005%, bismuth≤0.002%, zinc≤0.003%, mercury≤0.01%, and lead≤
0.01%, cadmium≤0.01%, chromium≤0.01%, phosphorus≤0.003%, sulphur≤0.005%, oxygen≤0.003%.
The method of the graphene enhancing Cu-base composites injection molding, step are as follows: by industrial pure copper and Kufil
It is added in vacuum electromagnetic induction furnace and melts, obtain copper liquid；It is injected into inert gas jet atomization device, passes through high pressure inert gas
Copper liquid is atomized into droplet by body, while graphene platelet is sprayed into spray chamber, and graphene platelet covers the copper liquid in sinking
In drop, copper/graphene mixture of liquid or half melt is formed, through cooling ingot casting, and roll forming obtains graphene enhancing copper
Based composites.
The method of the graphene enhancing Cu-base composites injection molding, the specific steps are as follows:
(1) industrial pure copper and Kufil are added in vacuum electromagnetic induction furnace and are melted, copper liquid temperature control 1410~
1450 DEG C, the copper alloy liquid melted is injected into inert gas jet atomization device, temperature is adjusted to 1380~1420 DEG C；
(2) spray gun for opening jet atomization device, is passed through the inert gas of 1~1.5MPa of pressure, copper alloy liquid is passed through
Spray gun atomization, controls the flow-rate ratio of copper alloy liquid flow and inert gas in spray gun, and the copper alloy liquid flow by nozzle is 200
~ 250 Grams Per Seconds, inert gas flow are 1400 ~ 1600 cubic millimeters/second, make copper alloy liquid-drop diameter at 10-100 μm；
(3) after drop atomization adjustment is suitable, graphene adding set is opened, Cu-base composites are enhanced according to graphene
Graphene content ratio requirement, according to the injection graphene platelet of copper alloy liquid flow continuous and quantitative, graphene platelet passes through
The inert gas of 100~150KPa of pressure is sent graphene platelet in spray deposition room forth by nozzle；The thin injection of graphene
Amount is atomized flow speeds match with copper alloy liquid, and the mass percent that control graphene enhances the copper-based graphene for meeting material exists
Between 0.05%~5%；
(4) graphene platelet floated covers on the copper alloy drop of sinking, deposits to the cone of settling chamber bottom
In funnel, copper/graphene mixture of liquid or half melt is formed, copper/graphene mixture is injected by conical funnel and cast
Ingot molding machine；
(5) open ingot casting shaping device, regulate cooling system, make continuous casting temperature control 780~870 DEG C it
Between；
(6) graphene copper alloy casting ingot is introduced into rolling equipment, continuous rolling is at required profile；
(7) graphene copper alloy profile is received by receiving around equipment around packing.
The purity of industrial pure copper is 99.90% or more in step (1).
Silver content is greater than 3% or more in Kufil in step (1)；It is accounted for by calculating the silver element in control Kufil
Final graphene enhancing Cu-base composites mass ratio is 0.05%~0.2%.
Inert gas is the nitrogen of 99.99% or more purity in step (2) and (3).
The nozzle of graphene adding set is arranged in spray deposition room middle and lower part in the step (3), makes the graphite sent forth
The copper alloy drop that alkene is atomized during floating with step (2) covers.
The carbon atom thickness of the graphene platelet is no more than 8 layers.
Beneficial effects of the present invention: preparation method simple possible in the present invention, step is easily operated, and the product of preparation has
The advantages that Material texture is uniform, compact structure, and intensity is high, and wearability, electrical and thermal conductivity performance are good.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below in conjunction with attached drawing, the invention will be further described.
Embodiment 1
Material selection: selecting the no-oxygen copper plate of 1200kg Cu 99.95, the mass percent of each element in copper ingot are as follows: iron:
0.0012%, bismuth: 0.0008%, zinc: 0.0011%, mercury: 0.0000%, lead: 0.001%, cadmium: 0.0002%, chromium: 0.0003%, phosphorus:
0.0021%, sulphur: 0.003%, oxygen: 0.0012%, impurity element summation: 01090%, copper content 99.9891%；
The Kufil cast-in vacuum electromagnetic induction furnace of no-oxygen copper plate and 14kg 5% are melted, and opens electromagnetism and stirs
Device is mixed, the melt of injecting jet atomising device contains collection room after copper liquid filtering when copper liquid temperature reaches 1450 DEG C, when melt is contained
After when collection room copper liquid is adjusted to 1420 DEG C, the spray gun of jet atomization device is opened, pressure 1.5MPa argon gas is passed through, melt is contained and is collected
The copper liquid of room is atomized with the speed of 250g/s by spray gun, and copper liquid-drop diameter is at 10-100 μm；Graphene addition is opened after 5min
Device is continuously sent forth from nozzle into spray deposition room with the speed of 11.25g/s by pressure 145KPa argon gas.Deposit copper/stone
Black alkene mixture injects ingot casting shaping device by the conical funnel of settling chamber bottom, pours into section 600mm2Trapezoidal casting
Ingot, and it is rolled into the graphene enhancing Cu-base composites pole stock of diameter 8.0mm, and carry out take-up by receiving winding apparatus.
After graphene obtained enhancing Cu-base composites pole stock is placed for 24 hours, detection graphene enhances copper-based composite wood
Expect 446.4 ~ 458.8W/mk of thermal coefficient of pole stock；Conductivity 102.24% ~ 104.69% IACS, 469 ~ 487MPa of intensity,
Elongation at break 5.78% ~ 6.36%.
Embodiment 2
Material selection: selecting the no-oxygen copper plate of 1200kg Cu99.97, the mass percent of each element in copper ingot are as follows: iron:
0.0011%, bismuth: 0.0007%, zinc: 0.0012%, mercury: 0.0000%, lead: 0.0004%, cadmium: 0.0002%, chromium: 0.0003%, phosphorus:
0.0017%, sulphur: 0.003%, oxygen: 0.0011%, impurity element summation: 0097%, copper content 99.9903%；
The Kufil cast-in vacuum electromagnetic induction furnace of no-oxygen copper plate and 2kg 5% are melted, and open electromagnetic agitation
Device, when copper liquid temperature reaches 1420 DEG C, the melt of injecting jet atomising device contains collection room after copper liquid filtering, contains and collects when melt
After when room copper liquid is adjusted to 1380 DEG C, the spray gun of jet atomization device is opened, pressure 1.0MPa nitrogen is passed through, melt is contained into collection room
Copper liquid with the speed of 200g/s by spray gun be atomized, copper liquid-drop diameter is at 10-100 μm；Graphene addition dress is opened after 5min
It sets, is continuously sent forth from nozzle into spray deposition room with the speed of 0.16g/s by pressure 145KPa argon gas.Deposit copper/graphite
Alkene mixture injects ingot casting shaping device by the conical funnel of settling chamber bottom, pours into section 600mm2Trapezoidal casting
Ingot, and it is rolled into the graphene enhancing Cu-base composites pole stock of diameter 8.0mm, and carry out take-up by receiving winding apparatus.
After graphene obtained enhancing Cu-base composites pole stock is placed for 24 hours, detection graphene enhances copper-based composite wood
Expect 396.24 ~ 425.7W/mk of thermal coefficient of pole stock；Conductivity 108.73% ~ 114.37% IACS, 420 ~ 437MPa of intensity,
Elongation at break 4.88% ~ 5.64%.Diameter is drawn into the graphene of 8.0mm is enhanced copper-based compound pole stock by wire drawing machine
2.85mm copper single line, through detecting conductivity 102.12 ~ 105.33% IACS of copper single line, 452 ~ 463MPa of intensity, extension at break
Rate 2.58% ~ 3.47%.
Embodiment 3
Graphene enhances Cu-base composites, and formula rate is as follows by mass percentage: graphene 5%, and silver 0.2% is miscellaneous
Prime element summation≤0.05%, remaining is copper；
The method of the graphene enhancing Cu-base composites injection molding, the specific steps are as follows:
(1) industrial pure copper and Kufil being added in vacuum electromagnetic induction furnace and is melted, copper liquid temperature is controlled at 1450 DEG C,
The copper alloy liquid melted is injected into inert gas jet atomization device, temperature is adjusted to 1400 DEG C；
(2) spray gun for opening jet atomization device, is passed through the inert gas of pressure 1.2MPa, copper alloy liquid is passed through spray gun
Atomization controls the flow-rate ratio of copper alloy liquid flow and inert gas in spray gun, by the copper alloy liquid flow of nozzle be 230 grams/
Second, inert gas flow is 1500 cubic millimeters/second, makes copper alloy liquid-drop diameter at 10~100 μm；
(3) after drop atomization adjustment is suitable, graphene adding set is opened, Cu-base composites are enhanced according to graphene
Graphene content ratio requirement, according to the injection graphene platelet of copper alloy liquid flow continuous and quantitative, graphene platelet passes through
The inert gas of pressure 130KPa is sent graphene platelet in spray deposition room forth by nozzle；The thin injection rate of graphene with
Copper alloy liquid is atomized flow speeds match, control graphene enhance the mass percent of the copper-based graphene for meeting material 5% it
Between；
(4) graphene platelet floated covers on the copper alloy drop of sinking, deposits to the cone of settling chamber bottom
In funnel, copper/graphene mixture of liquid or half melt is formed, copper/graphene mixture is injected by conical funnel and cast
Ingot molding machine；
(5) open ingot casting shaping device, regulate cooling system, make continuous casting temperature control 780~870 DEG C it
Between；
(6) graphene copper alloy casting ingot is introduced into rolling equipment, continuous rolling is at required profile；
(7) graphene copper alloy profile is received by receiving around equipment around packing.
The purity of industrial pure copper is 99.90% or more in step (1).
Silver content is greater than 3% or more in Kufil in step (1)；It is accounted for by calculating the silver element in control Kufil
Final graphene enhancing Cu-base composites mass ratio is 0.2%.
Inert gas is the nitrogen of 99.99% or more purity in step (2) and (3).
Claims (6)
1. the method that graphene enhances Cu-base composites injection molding, it is characterized in that step are as follows: by industrial pure copper and Kufil
Gold, which is added in vacuum electromagnetic induction furnace, to be melted, and copper liquid is obtained；Copper liquid is injected into inert gas jet atomization device, it is lazy by high pressure
Copper liquid is atomized into droplet by property gas, while graphene platelet is sprayed into spray chamber, and graphene platelet is covered in sinking
In copper liquid drop, copper/graphene mixture of liquid or half melt is formed, cooling ingot casting, roll forming obtain graphene enhancing copper
Based composites；
Specific step is as follows:
(1) industrial pure copper and Kufil are added in vacuum electromagnetic induction furnace and are melted, copper liquid temperature is controlled 1410~1450
DEG C, the copper alloy liquid melted is injected into inert gas jet atomization device, temperature is adjusted to 1380~1420 DEG C；
(2) spray gun for opening jet atomization device, is passed through the inert gas of 1~1.5MPa of pressure, copper alloy liquid is passed through spray gun
Atomization controls the flow-rate ratio of copper alloy liquid flow and inert gas in spray gun, and the copper alloy liquid flow by nozzle is 200 ~ 250
Grams Per Second, inert gas flow are 1400 ~ 1600 cubic millimeters/second, make copper alloy liquid-drop diameter at 10-100 μm；
(3) after drop atomization adjustment is suitable, graphene adding set is opened, enhances the stone of Cu-base composites according to graphene
Black alkene content ratio requirement, according to the injection graphene film of copper alloy liquid flow continuous and quantitative, graphene platelet passes through pressure 100
The inert gas of~150KPa is sent graphene platelet in spray deposition room forth by nozzle；Graphene platelet injection rate with
Copper alloy liquid is atomized flow speeds match, and the mass percent of the graphene of control graphene enhancing Cu-base composites exists
Between 0.05%~5%；
(4) graphene platelet floated covers on the copper alloy drop of sinking, deposits to the conical funnel of settling chamber bottom
In, form copper/graphene mixture of liquid or half melt, copper/graphene mixture by conical funnel injection ingot casting at
Type device；
(5) ingot casting shaping device is opened, cooling system is regulated, controls the temperature of continuous casting between 780~870 DEG C；
(6) graphene copper alloy casting ingot is introduced into rolling equipment, continuous rolling is at required profile；
(7) graphene copper alloy profile is received by receiving around equipment around packing；
Graphene enhances Cu-base composites, and formula rate is as follows by mass percentage: graphene 0.05%~5%, silver 0.05%
~0.2%, impurity element summation≤0.05%, remaining is copper；
The impurity element is specific as follows: iron≤0.005%, bismuth≤0.002%, zinc≤0.003%, mercury≤0.01%, and lead≤
0.01%, cadmium≤0.01%, chromium≤0.01%, phosphorus≤0.003%, sulphur≤0.005%, oxygen≤0.003%.
2. the method for graphene enhancing Cu-base composites injection molding as described in claim 1, it is characterized in that: in step (1)
The purity of industrial pure copper is 99.90% or more.
3. the method for graphene enhancing Cu-base composites injection molding as described in claim 1, it is characterized in that: in step (1)
Silver content is greater than 3% or more in Kufil；It is copper-based that final graphene enhancing is accounted for by the silver element in calculating control Kufil
Composite material mass ratio is 0.05%~0.2%.
4. the method for graphene as described in claim 1 enhancing Cu-base composites injection molding, it is characterized in that: step (2) and
(3) inert gas is the nitrogen or argon gas of 99.99% or more purity in.
5. the method for graphene enhancing Cu-base composites injection molding as described in claim 1, it is characterized in that: the step
(3) the nozzle setting of graphene adding set is in spray deposition room middle and lower part in, during so that the graphene sent forth is floated with
The copper alloy drop of step (2) atomization covers.
6. the method for graphene enhancing Cu-base composites injection molding as described in claim 1, it is characterized in that: the graphene
The carbon atom thickness of thin slice is no more than 8 layers.
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| CN109628789B (en) * | 2019-01-31 | 2020-12-29 | 中国科学院过程工程研究所 | Graphene composite aluminum alloy, wire rod prepared from graphene composite aluminum alloy, preparation method and application |
| CN110280175A (en) * | 2019-06-14 | 2019-09-27 | 慧隆(厦门)石墨烯科技有限公司 | A kind of modification copper process units |
| CN110600161B (en) * | 2019-09-23 | 2020-11-03 | 西北有色金属研究院 | Preparation method of high-strength high-conductivity graphene-reinforced copper-silver composite wire |
| CN111809078B (en) * | 2020-07-21 | 2021-06-04 | 深圳市中金岭南科技有限公司 | Composite copper-silver alloy wire and preparation method thereof |
| CN115786763B (en) * | 2022-11-15 | 2024-09-06 | 华为数字能源技术有限公司 | Copper-carbon composite material, preparation method and application thereof, and conductive product |
| CN116356192A (en) * | 2023-04-10 | 2023-06-30 | 松山湖材料实验室 | Graphene composite metal material and preparation method and preparation device thereof |
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| CN105965025A (en) * | 2016-07-13 | 2016-09-28 | 江苏省特种设备安全监督检验研究院 | Method and device for producing high-strength and high-conductivity graphene copper-based powder material |
| CN107012356A (en) * | 2017-03-22 | 2017-08-04 | 郭和谦 | A kind of high-intensity high-conductivity copper based alloy blank of graphene-containing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105965025A (en) * | 2016-07-13 | 2016-09-28 | 江苏省特种设备安全监督检验研究院 | Method and device for producing high-strength and high-conductivity graphene copper-based powder material |
| CN107012356A (en) * | 2017-03-22 | 2017-08-04 | 郭和谦 | A kind of high-intensity high-conductivity copper based alloy blank of graphene-containing and preparation method thereof |
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