CN107201535A - A kind of method for preparing graphene/copper composite material using aerobic sintering - Google Patents
A kind of method for preparing graphene/copper composite material using aerobic sintering Download PDFInfo
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- CN107201535A CN107201535A CN201710247094.6A CN201710247094A CN107201535A CN 107201535 A CN107201535 A CN 107201535A CN 201710247094 A CN201710247094 A CN 201710247094A CN 107201535 A CN107201535 A CN 107201535A
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- graphene
- copper
- copper composite
- composite material
- oxygen
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 82
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 73
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 69
- 239000010949 copper Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000005245 sintering Methods 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001301 oxygen Substances 0.000 claims abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000011889 copper foil Substances 0.000 claims abstract description 14
- 238000004070 electrodeposition Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 11
- -1 graphite alkene Chemical class 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 150000002815 nickel Chemical class 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 150000001879 copper Chemical class 0.000 claims abstract description 4
- 150000001336 alkenes Chemical class 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- 238000009713 electroplating Methods 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical compound [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- XIKYYQJBTPYKSG-UHFFFAOYSA-N nickel Chemical compound [Ni].[Ni] XIKYYQJBTPYKSG-UHFFFAOYSA-N 0.000 description 2
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- HKIQZBZCKQBMJT-UHFFFAOYSA-J nickel(2+) disulfate Chemical compound [Ni++].[Ni++].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HKIQZBZCKQBMJT-UHFFFAOYSA-J 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
-
- B22F1/0003—
-
- 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
-
- 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
-
- 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
A kind of method for preparing graphene/copper composite material using aerobic sintering, graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is negative electrode, the mixed solution of soluble copper salt, soluble nickel salt and graphene oxide is electrolyte, logical direct current carries out electro-deposition, and it is graphene/copper composite powder to keep certain current density to deposit products therefrom for a period of time, on negative electrode；Washes of absolute alcohol product is used, residual impurity is removed, places into vacuum drying chamber and dried, grinds, is pressed into graphene/copper composite block；In atmosphere sintering furnace, under oxygen and carrier gas protection, partial pressure of oxygen is controlled, sintering graphite alkene/copper composite block obtains graphene/copper composite material.The present invention improves the binding ability of graphene and Copper substrate, improves the interfacial combined function of graphene and Copper substrate, and technique is simple, and operation is easy, with low cost, no especial equipment requirements.
Description
Technical field
The invention belongs to metal-base composites technical field, it is related to Metallic Functional Materials preparation.
Background technology
Graphene is because with high intensity and excellent electrical and thermal conductivity performance（Intensity is 130 GPa, carrier mobility
For 15000 cm2/ Vs, thermal conductivity factor is 5300 W/mK）And it is considered as the optimal strong of high-strength highly-conductive Cu-base composites
Change phase, but big and graphene and copper the interfacial combined function difference of difficulty that graphene uniform is dispersed in Copper substrate is that graphene is strong
Change two hang-ups prepared by Cu-base composites.
In a kind of utilization electrochemical deposition prepares the method for graphene/copper composite powder, using electrolytic copper foil as anode, copper foil
For negative electrode, the mixed solution of mantoquita, nickel salt and graphene oxide is carries out electro-deposition in electrolyte, negative electrode deposition gained is graphite
Alkene is dispersed in graphene/copper composite powder in Copper substrate, solves the difficulty that graphene uniform is dispersed in Copper substrate big
The problem of.
The Kim such as Kim Y, Lee J, Yeom MS, Shin JW, Kim H, Cui Y, Kysar JW, Hone J,
Jung Y, Joen S, Han SM. Strengthening effect of single-atomic-layer graphene
in metal-graphene nanolayered composites, Nature Communications, DOI:
10.1038/ncomms3114,2013. deposits the individual layer stone of alternating growth using chemical vapour deposition technique on Copper substrate surface
Black alkene film, so as to obtain the copper-base graphite alkene composite of multilayer, its tensile strength can reach 1.5 GPa.Although they
The copper-base graphite alkene composite with practical value can not be prepared, but they think to enter material during chemical vapor deposition
In oxygen generation copper and graphene can share the interfacial structure of oxygen in sintering, and then improve the interfacial bonding property of graphene and copper
Can, it is indicated that a kind of to prepare the method that High-performance graphene strengthens Cu-base composites.In fact, the Kim K such as Kim T, Cha
S I, Gemming T, Eckert J, Hong S H. The role of interfacial oxygen atoms in
the enhanced mechanical properties of carbon-nanotue-reinforced metal matrix
Nanocomposites, Small, 4 (11), pp1936-1940,2008. and Park etc.[3]Park M, Kim B H, Kim
S, Han D S, Kim G. Improved binding between copper and carbon nanotubes in a
composite using oxygen-containing functional groups, Carbon, 49, pp811-818,
2011.
Also the interfacial combined function of CNT and metallic element is improved using oxygen.Therefore the boundary that copper shares oxygen with graphene is formed
Face structure, which may is that, improves a good method of graphene and copper interfacial combined function.
As can be seen here, oxygen content during control graphene/copper composite material sintering, carries out aerobic sintering, can form copper
The interfacial structure of oxygen is shared with graphene, there is positive reality to anticipate the structure and performance for improving graphene/copper composite material
Adopted and good application prospect.
The content of the invention
It is an object of the invention to made for existing technology of preparing and technologic deficiency there is provided one kind using aerobic sintering
The method of standby graphene/copper composite material.
The present invention is achieved by the following technical solutions.
One kind of the present invention prepares graphene/copper composite material using aerobic sintering method, as follows.
Graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is negative electrode, soluble copper
The mixed solution of salt, soluble nickel salt and graphene oxide is electrolyte, leads to direct current and carries out electro-deposition, keeps certain electric current
It is graphene/copper composite powder that density deposits products therefrom for a period of time, on negative electrode.
Washes of absolute alcohol product is used, residual impurity is removed, places into vacuum drying chamber and dried, grinds, is pressed into
Graphene/copper composite block.
In atmosphere sintering furnace, under the protection of oxygen and carrier gas, control partial pressure of oxygen, sintering graphite alkene/copper composite block,
Obtain graphene/copper composite material.
Described soluble copper salt is one kind in copper chloride, copper sulphate or copper nitrate.
Described soluble nickel salt is one kind in nickel chloride, nickel sulfate or nickel nitrate.
The addition of described graphene oxide is 0.01%-10%.
Described soluble copper salt and the mass ratio of soluble nickel salt are 5:1-100:1.
Described concentration of electrolyte is 0.01 g/ml-1.0 g/ml.
Described current density is 5 A/m2-5000 A/m2。
Described electroplating time is 2 h-48 h.
Described partial pressure of oxygen is 0.01-1.0 kPa.
Described sintering temperature is 700-1200 DEG C.
Described soaking time is 20-300 min.
It is an advantage of the invention that.
（1）The present invention has intended to solve the problem of interfacial combined function of graphene and copper is poor, is improved by adding appropriate oxygen
The binding ability of graphene and Copper substrate.
（2）By controlling the partial pressure of oxygen when addition and sintering of graphene in graphene/copper composite powder, stone is not being destroyed
On the basis of the structure of black alkene and the performance of reduction composite, the interfacial combined function of graphene and Copper substrate is improved.
（3）Technique is simple, and operation is easy, with low cost：Absolute ethyl alcohol, carrier gas etc. is common industrial raw material, tabletting and
Sintering process is without especial equipment requirements.
Brief description of the drawings
Fig. 1 is the x-ray photoelectron power spectrum spectrogram of graphene/copper composite powder prepared by embodiment 1.
Fig. 2 is the stereoscan photograph of graphene/copper composite material fracture prepared by embodiment 1.
Embodiment
The present invention will be described further by following examples, but protection scope of the present invention not limited to this.
Embodiment 1.
Graphene/copper composite material is prepared, should be carried out according to the following steps：Graphene/copper is prepared using electrodeposition process to be combined
Powder, using electrolytic copper foil as anode, copper foil is negative electrode, soluble copper salt copper sulphate（CuSO4）And soluble nickel salt nickel sulfate
（NiSO4）, by mantoquita：Nickel salt=10:1 mass ratio, is electrolyte, graphene oxide with the mixed solution of graphene oxide
Addition percent by volume be 0.6%, concentration of electrolyte be 0.12 g/ml, lead to direct current carry out electro-deposition, keep 50 A/
m2The h of current density 24, deposition products therefrom is graphene/copper composite powder on negative electrode.Washes of absolute alcohol product is used, is removed
Residual impurity is removed, places into vacuum drying chamber and is dried, grinds, is pressed into graphene/copper composite block.In atmosphere sintering furnace
In, under oxygen and argon gas protection, it is 0.06 kPa to control partial pressure of oxygen, and 800 DEG C of insulation 120 min sintering graphites alkene/copper are combined
Block, obtains graphene/copper composite material.
Embodiment 2.
Graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is negative electrode, soluble copper
Salt copper chloride（CuCl2）And soluble nickel salt nickel chloride（NiCl2）, by mantoquita：Nickel salt=20:1 mass ratio, with graphene oxide
Mixed solution is electrolyte, and the percent by volume of the addition of graphene oxide is 1.0%, and concentration of electrolyte is 0.20 g/
Ml, leads to direct current and carries out electro-deposition, keep 100 A/m2The h of current density 48, deposition products therefrom is graphite on negative electrode
Alkene/copper composite powder.Washes of absolute alcohol product is used, residual impurity is removed, places into vacuum drying chamber and dried, is ground,
It is pressed into graphene/copper composite block.In atmosphere sintering furnace, under oxygen and nitrogen protection, it is 0.10 kPa to control partial pressure of oxygen,
750 DEG C of insulation 200 min sintering graphites alkene/copper composite blocks, obtain graphene/copper composite material.
Embodiment 3.
Graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is negative electrode, soluble copper
Salt copper nitrate（CuNO3）And soluble nickel salt nickel nitrate（NiNO3）, by mantoquita：Nickel salt=15:1 mass ratio, with graphene oxide
Mixed solution is electrolyte, and the percent by volume of the addition of graphene oxide is 1.5%, and concentration of electrolyte is 0.15 g/
Ml, leads to direct current and carries out electro-deposition, keep 80 A/m2The h of current density 12, on negative electrode deposition products therefrom be graphene/
Copper composite powder.Washes of absolute alcohol product is used, residual impurity is removed, places into vacuum drying chamber and dried, grinds, is pressed into
Graphene/copper composite block.In atmosphere sintering furnace, under oxygen and nitrogen protection, it is 0.15 kPa, 850 to control partial pressure of oxygen
DEG C insulation 100 min sintering graphites alkene/copper composite block, obtain graphene/copper composite material.
Claims (9)
1. a kind of method for preparing graphene/copper composite material using aerobic sintering, it is characterised in that including preparing in detail below
Step：
Graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is negative electrode, soluble copper salt, can
The mixed solution of insoluble nickel salt and graphene oxide is electrolyte, leads to direct current and carries out electro-deposition, keeps certain current density
For a period of time, it is graphene/copper composite powder products therefrom to be deposited on negative electrode；
Washes of absolute alcohol product is used, residual impurity is removed, places into vacuum drying chamber and dried, grinds, is pressed into graphite
Alkene/copper composite block；
In atmosphere sintering furnace, under oxygen and carrier gas protection, partial pressure of oxygen is controlled, sintering graphite alkene/copper composite block obtains stone
Black alkene/carbon/carbon-copper composite material.
2. it is according to claim 1 prepare graphene/copper composite material method, it is characterised in that in step a) can
Dissolubility mantoquita is one kind in copper chloride, copper sulphate or copper nitrate.
3. it is according to claim 1 prepare graphene/copper composite material method, it is characterised in that in step a) can
Insoluble nickel salt is one kind in nickel chloride, nickel sulfate or nickel nitrate.
4. the method according to claim 1 for preparing graphene/copper composite material, it is characterised in that the oxygen in step a)
The addition of graphite alkene is 0.01%-10%.
5. it is according to claim 1 prepare graphene/copper composite material method, it is characterised in that in step a) can
Dissolubility mantoquita and the mass ratio of soluble nickel salt are 5:1-100:1.
6. the method according to claim 1 for preparing graphene/copper composite material, it is characterised in that the electricity in step a)
It is 0.01 g/ml-1.0 g/ml to solve liquid concentration；Current density is 5 A/m2-5000 A/m2；Electroplating time is 2 h-48 h.
7. the method according to claim 1 for preparing graphene/copper composite material, it is characterised in that the load in step c)
Gas is argon gas or nitrogen.
8. the method according to claim 1 for preparing graphene/copper composite material, it is characterised in that the oxygen in step c)
Partial pressure is 0.01-1.0 kPa.
9. the method according to claim 1 for preparing graphene/copper composite material, it is characterised in that the burning in step c)
Junction temperature is 700-1200 DEG C, and soaking time is 20-300 min.
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| CN107201535B CN107201535B (en) | 2018-12-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158123A (en) * | 2019-05-10 | 2019-08-23 | 东北大学 | A kind of surface metalation graphene and preparation method thereof |
| CN110327925A (en) * | 2019-07-29 | 2019-10-15 | 西安建筑科技大学 | Coal Quito pore catalyst and its preparation method and application of carbon monoxide in a kind of removing sintering flue gas |
| CN112063998A (en) * | 2020-08-28 | 2020-12-11 | 南昌大学 | Preparation method of ultrathin copper/graphene composite foil |
| CN114713821A (en) * | 2022-01-12 | 2022-07-08 | 西安理工大学 | Preparation method of Cu-W graphene-containing composite material |
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| CN102174702A (en) * | 2011-01-11 | 2011-09-07 | 湖南大学 | Preparation method for metallic nano-particle and graphene composite |
| CN102896834A (en) * | 2012-10-11 | 2013-01-30 | 湖南大学 | Graphene-copper nanoparticle composite, and preparation and application thereof |
| CN105603231A (en) * | 2015-12-07 | 2016-05-25 | 宁波墨西科技有限公司 | Graphene-modified copper alloy nano-material and preparation method thereof |
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2017
- 2017-04-17 CN CN201710247094.6A patent/CN107201535B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174702A (en) * | 2011-01-11 | 2011-09-07 | 湖南大学 | Preparation method for metallic nano-particle and graphene composite |
| CN102896834A (en) * | 2012-10-11 | 2013-01-30 | 湖南大学 | Graphene-copper nanoparticle composite, and preparation and application thereof |
| CN105603231A (en) * | 2015-12-07 | 2016-05-25 | 宁波墨西科技有限公司 | Graphene-modified copper alloy nano-material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158123A (en) * | 2019-05-10 | 2019-08-23 | 东北大学 | A kind of surface metalation graphene and preparation method thereof |
| CN110327925A (en) * | 2019-07-29 | 2019-10-15 | 西安建筑科技大学 | Coal Quito pore catalyst and its preparation method and application of carbon monoxide in a kind of removing sintering flue gas |
| CN112063998A (en) * | 2020-08-28 | 2020-12-11 | 南昌大学 | Preparation method of ultrathin copper/graphene composite foil |
| CN114713821A (en) * | 2022-01-12 | 2022-07-08 | 西安理工大学 | Preparation method of Cu-W graphene-containing composite material |
| CN114713821B (en) * | 2022-01-12 | 2024-03-12 | 西安理工大学 | Preparation method of Cu-W graphene-containing composite material |
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