CN107201535B - A method of graphene/copper composite material is prepared using aerobic sintering - Google Patents
A method of graphene/copper composite material is prepared using aerobic sintering Download PDFInfo
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- CN107201535B CN107201535B CN201710247094.6A CN201710247094A CN107201535B CN 107201535 B CN107201535 B CN 107201535B CN 201710247094 A CN201710247094 A CN 201710247094A CN 107201535 B CN107201535 B CN 107201535B
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 74
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 70
- 239000010949 copper Substances 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 28
- 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
- -1 graphite alkene Chemical class 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 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
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 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
- 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 group 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
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000243 solution Substances 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
- 150000001879 copper Chemical class 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- VEMHQNXVHVAHDN-UHFFFAOYSA-J [Cu+2].[Cu+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O Chemical compound [Cu+2].[Cu+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VEMHQNXVHVAHDN-UHFFFAOYSA-J 0.000 description 1
- HAZNKDJFOOUKJY-UHFFFAOYSA-N [Ni++].[Ni++].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound [Ni++].[Ni++].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HAZNKDJFOOUKJY-UHFFFAOYSA-N 0.000 description 1
- SGDPVQRGBHPKIH-UHFFFAOYSA-L [Ni].Cl[Ni]Cl Chemical compound [Ni].Cl[Ni]Cl SGDPVQRGBHPKIH-UHFFFAOYSA-L 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- XCBKGJWOCHSAMS-UHFFFAOYSA-L copper;dichlorocopper Chemical compound [Cu].Cl[Cu]Cl XCBKGJWOCHSAMS-UHFFFAOYSA-L 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- APTUIUORLSQNEF-UHFFFAOYSA-N dicopper tetranitrate Chemical compound [Cu++].[Cu++].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O APTUIUORLSQNEF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000010410 layer Substances 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
- 239000002994 raw material Substances 0.000 description 1
- 239000002356 single layer Substances 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 method of graphene/copper composite material is prepared using aerobic sintering, graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is cathode, the mixed solution of soluble copper salt, soluble nickel salt and graphene oxide is electrolyte, logical direct current carries out electro-deposition, and keeping certain current density to deposit products therefrom for a period of time, on cathode is graphene/copper composite powder；With washes of absolute alcohol product, residual impurity is removed, places into vacuum oven and is dried, ground, be 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 performance of graphene and Copper substrate, improves the interfacial combined function of graphene and Copper substrate, simple process, and operation is easy, low in cost, no especial equipment requirements.
Description
Technical field
The invention belongs to metal-base composites technical fields, are related to Metallic Functional Materials preparation.
Background technique
Graphene is because with high intensity and excellent electrical and thermal conductivity performance, (intensity is 130 GPa, carrier mobility
For 15000 cm2/ Vs, thermal coefficient are 5300 W/mK) and it is considered as the best strong of high-strength highly-conductive Cu-base composites
Change phase, but it is that graphene is strong that graphene uniform, which is dispersed in the big difficulty in Copper substrate and graphene and the interfacial combined function difference of copper,
Change two hang-ups in Cu-base composites preparation.
It is prepared in graphene/copper composite powder method a kind of using electrochemical deposition, using electrolytic copper foil as anode, copper foil
For cathode, the mixed solution of mantoquita, nickel salt and graphene oxide is that electro-deposition is carried out in electrolyte, and cathode deposition gained is graphite
Alkene is dispersed in graphene/copper composite powder in Copper substrate, and it is big to solve the difficulty that graphene uniform is dispersed in Copper substrate
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 single layer stone of alternating growth on Copper substrate surface using chemical vapour deposition technique
Black alkene film, to obtain the copper-base graphite alkene composite material of multilayer, tensile strength can achieve 1.5 GPa.Although they
The copper-base graphite alkene composite material with practical value cannot be prepared, but they think to enter material when chemical vapor deposition
In oxygen the interfacial structure that copper and graphene share oxygen can be generated in sintering, and then improve the interfacial bonding property of graphene and copper
It can, it is indicated that a kind of method for preparing High-performance graphene and strengthening 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 improve the interfacial combined function of carbon nanotube and metallic element using oxygen.Therefore it forms copper and graphene shares oxygen
Interfacial structure may is that improve graphene and copper interfacial combined function a good method.
It can be seen that oxygen content when control graphene/copper composite material sintering, carries out aerobic sintering, can form copper
The interfacial structure that oxygen is shared with graphene there is positive reality to anticipate the structure and performance that improve graphene/copper composite material
Adopted and good application prospect.
Summary of the invention
It is an object of the invention to be directed to existing technology of preparing and technologic deficiency, a kind of aerobic sintering of utilization is provided and is made
The method of standby graphene/copper composite material.
The present invention is achieved by the following technical solutions.
It is of the present invention a kind of using aerobic sintering method preparation graphene/copper composite material, as follows.
Graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is cathode, 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, which deposits products therefrom for a period of time, on cathode,.
With washes of absolute alcohol product, residual impurity is removed, places into vacuum oven and is dried, ground, be 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.
The soluble copper salt is copper chloride, one of copper sulphate or copper nitrate.
The soluble nickel salt is nickel chloride, one of nickel sulfate or nickel nitrate.
The additive amount of the graphene oxide is 0.01%-10%.
The mass ratio of the soluble copper salt and soluble nickel salt is 5:1-100:1.
The concentration of electrolyte is 0.01 g/ml-1.0 g/ml.
The current density is 5 A/m2-5000 A/m2。
The electroplating time is 2 h-48 h.
The partial pressure of oxygen is 0.01-1.0 kPa.
The sintering temperature is 700-1200 DEG C.
The soaking time is 20-300 min.
It is an advantage of the invention that.
(1) present invention has intended to solve the problem of the interfacial combined function difference of graphene and copper, is improved by adding appropriate oxygen
The binding performance of graphene and Copper substrate.
(2) by additive amount and the sintering of graphene in control graphene/copper composite powder partial pressure of oxygen when, is not destroying stone
On the basis of the structure of black alkene and the performance of reduction composite material, the interfacial combined function of graphene and Copper substrate is improved.
(3) simple process, operation is easy, low in cost: dehydrated alcohol, carrier gas etc. are common industrial raw material, tabletting and
Sintering process is without especial equipment requirements.
Detailed description of the invention
Fig. 1 is graphene/copper composite powder x-ray photoelectron spectroscopy spectrogram prepared by embodiment 1.
Fig. 2 is the stereoscan photograph of graphene/copper composite material fracture prepared by embodiment 1.
Specific embodiment
The present invention will be described further by following embodiment, and but the scope of the present invention is not limited thereto.
Embodiment 1.
Graphene/copper composite material is prepared, should sequentially include the following steps: that prepare graphene/copper using electrodeposition process compound
Powder, using electrolytic copper foil as anode, copper foil is cathode, 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
Additive amount 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/
m224 h of current density, deposition products therefrom is graphene/copper composite powder on cathode.With washes of absolute alcohol product, remove
Residual impurity is removed, places into vacuum oven and is dried, grinds, is pressed into graphene/copper composite block.In atmosphere sintering furnace
In, under oxygen and argon gas protection, control partial pressure of oxygen is 0.06 kPa, and 800 DEG C of heat preservation 120 min sintering graphite alkene/copper are compound
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 cathode, 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 additive amount of graphene oxide is 1.0%, and concentration of electrolyte is 0.20 g/
Ml leads to direct current and carries out electro-deposition, keeps 100 A/m248 h of current density, deposition products therefrom is graphite on cathode
Alkene/copper composite powder.With washes of absolute alcohol product, residual impurity is removed, places into vacuum oven and is dried, ground,
It is pressed into graphene/copper composite block.In atmosphere sintering furnace, under oxygen and nitrogen protection, control partial pressure of oxygen is 0.10 kPa,
750 DEG C of heat preservation 200 min sintering graphite 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 cathode, 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 additive amount of graphene oxide is 1.5%, and concentration of electrolyte is 0.15 g/
Ml leads to direct current and carries out electro-deposition, keeps 80 A/m212 h of current density, on cathode deposition products therefrom be graphene/
Copper composite powder.With washes of absolute alcohol product, residual impurity is removed, places into vacuum oven and is dried, ground, be pressed into
Graphene/copper composite block.In atmosphere sintering furnace, under oxygen and nitrogen protection, control partial pressure of oxygen be 0.15 kPa, 850
DEG C heat preservation 100 min sintering graphite alkene/copper composite block, obtain graphene/copper composite material.
Claims (9)
1. a kind of method using aerobic sintering preparation graphene/copper composite material, it is characterised in that including preparing in detail below
Step:
A) graphene/copper composite powder is prepared using electrodeposition process, using electrolytic copper foil as anode, copper foil is cathode, 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, which deposits products therefrom for a period of time, on cathode,；
B) washes of absolute alcohol product is used, residual impurity is removed, places into vacuum oven and dried, grinds, is pressed into stone
Black alkene/copper composite block；
C) in atmosphere sintering furnace, under oxygen and carrier gas protection, partial pressure of oxygen is controlled, sintering graphite alkene/copper composite block obtains
To graphene/copper composite material.
2. it is according to claim 1 preparation graphene/copper composite material method, it is characterised in that in step a) can
Dissolubility mantoquita is copper chloride, one of copper sulphate or copper nitrate.
3. it is according to claim 1 preparation graphene/copper composite material method, it is characterised in that in step a) can
Insoluble nickel salt is nickel chloride, one of nickel sulfate or nickel nitrate.
4. the method for preparation graphene/copper composite material according to claim 1, it is characterised in that the oxygen in step a)
The additive amount of graphite alkene is 0.01vol.%-10vol.%.
5. it is according to claim 1 preparation 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 for preparation graphene/copper composite material according to claim 1, it is characterised in that the electricity in step a)
Solution liquid concentration is 0.01 g/ml-1.0 g/ml；Current density is 5 A/m2-5000 A/m2；Electroplating time is 2 h-48 h.
7. the method for preparation graphene/copper composite material according to claim 1, it is characterised in that the load in step c)
Gas is argon gas or nitrogen.
8. the method for preparation graphene/copper composite material according to claim 1, it is characterised in that the oxygen in step c)
Partial pressure is 0.01-1.0 kPa.
9. the method for preparation graphene/copper composite material according to claim 1, 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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| CN110158123B (en) * | 2019-05-10 | 2021-03-30 | 东北大学 | Surface metallization 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 |
| CN112063998B (en) * | 2020-08-28 | 2022-10-11 | 南昌大学 | Preparation method of ultrathin copper/graphene composite foil |
| 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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| 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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