CN109147985A - The composite material and preparation method and application of graphene and wicker copper nanoparticle - Google Patents
The composite material and preparation method and application of graphene and wicker copper nanoparticle Download PDFInfo
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- CN109147985A CN109147985A CN201811005727.3A CN201811005727A CN109147985A CN 109147985 A CN109147985 A CN 109147985A CN 201811005727 A CN201811005727 A CN 201811005727A CN 109147985 A CN109147985 A CN 109147985A
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- graphene
- copper
- wicker
- composite material
- wicker copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 84
- 239000010949 copper Substances 0.000 title claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 63
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 81
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000012300 argon atmosphere Substances 0.000 claims description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 11
- 239000004020 conductor Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 229920002521 macromolecule Polymers 0.000 claims description 9
- 150000001336 alkenes Chemical class 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003463 adsorbent Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 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
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- JTTXECQCCPZGII-UHFFFAOYSA-M sodium;ethane-1,2-diol;hydroxide Chemical compound [OH-].[Na+].OCCO JTTXECQCCPZGII-UHFFFAOYSA-M 0.000 claims description 2
- 241000446313 Lamella Species 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 32
- 239000002245 particle Substances 0.000 abstract description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001431 copper ion Inorganic materials 0.000 abstract description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 12
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides the composite materials and preparation method and application of a kind of graphene and wicker copper nanoparticle, the mass percent of graphene is 1-20% in composite material, the mass percent of wicker copper nanoparticle is 80-99%, and wherein wicker copper nanoparticle is adsorbed on graphene sheet layer.The colloidal solution that graphene oxide is prepared using Hummers method is utilized respectively mantoquita and silvery for wicker copper nanoparticle slurry, composite material is prepared by the colloidal solution and wicker copper nanoparticle slurry of graphene oxide.The present invention passes through the high-ratio surface suction-operated of graphene, silver ion and copper ion can be effectively adsorbed, to prevent silver ion and copper ion migration；In addition the oxygen characteristic that blocks water of graphene can effectively prevent the oxidation of silver and copper；Wicker copper particle can effectively reduce contact resistance by the bridge joint between graphene, so that the obtained material of the present invention will have preferably electric conductivity compared to the particle of single wicker copper.
Description
Technical field
The present invention relates to field of material preparation, and in particular to the composite material of a kind of graphene and wicker copper nanoparticle and
Preparation method and application.
Background technique
Conductive material has many purposes, such as circuit board, electric wire and spot welding material etc..Wherein graphene is a kind of
A kind of substance with very good electric conductivity.Graphene is the sp by Hexagonal array2Carbon atom composition has monoatomic thickness
Two-dimensional slice, it is the composition primitive of graphite.In addition, silver and copper are also extraordinary conductive material.Graphene is as two dimension
Conductive material, it is lower in the electron transport rate of interlayer, affect its electric conductivity, and the nanoparticle of silver and copper just can be with
As bridge conductive between graphene layer.
Silver is expensive as conductive material, and copper is cheap as conductive material, and its conductivity and silver are close.But
It is copper as conductive material, especially easy to oxidize at the nanoscale, electric conductivity declines to a great extent, therefore people utilize silver
Copper nano-particle is coated as conductive material, while reducing material cost and antioxygenic property.
Interface resistance in order to solve the problems, such as graphite alkenyl conductive material is larger, needs to develop anti-oxidant, good conductivity
And low-cost graphene-based composite material.The invention patent for this problem, has developed new structural compound.
Summary of the invention
The invention proposes the composite materials and preparation method and application of a kind of graphene and wicker copper nanoparticle, solve
The above problem.
Realize the composite material the technical scheme is that a kind of graphene and wicker copper nanoparticle, composite material
The mass percent of middle graphene is 1-20%, and the mass percent of wicker copper nanoparticle is 80-99%, wherein wicker copper nanometer
Particle absorption is on graphene sheet layer.
The size of the wicker copper nanoparticle is 10-500nm.
Silver-colored mass percent is 10-30% in the wicker copper nanoparticle, and the mass percent of copper is 70-90%.
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(1) using natural flaky graphite as raw material, the colloidal solution of graphene oxide is prepared using Hummers method；
The natural flaky graphite of 1 unit mass is added to the concentrated sulfuric acid of 20-50 unit mass and the mixed solution of sodium metaperiodate
In, it is stirred 3-5 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 0.5 hour to 10 hours, institute
It obtains mixture and becomes thick；Then the water of 50-100 unit mass is added into the mixture, and increases temperature to 90-95
DEG C, maintain this temperature 15-60 minutes；The hydrogen peroxide of 1-5 unit mass is added later, and stirring adds after 0.5 to 5 hours
The water of 50-100 unit mass, is filtered while hot, cleans 3 times and mistake with deionized water again after being washed 3-5 times with dilute hydrochloric acid (3-10%)
Filter；Gained filter cake is put into and is ultrasonically treated 1-3 hours in the water of 400-1000 unit mass to get the colloid for arriving graphene oxide
Solution；
(2) mantoquita is dissolved in ethylene glycol, the ethylene glycol solution of macromolecule dispersant and sodium hydroxide is added, stirs evenly
Afterwards, copper Nano sol is obtained in 130-180 DEG C of reaction 2-24 h under nitrogen or argon atmosphere；Nitre is added into copper Nano sol
Sour silver, reacts 1-72 h under 60-150 DEG C of nitrogen or argon atmosphere；Obtain wicker copper nano particle slurry；Sedimentation, centrifugation are washed
It washs；
(3) in the wicker copper nano particle slurry dispersion ethylene glycol obtained step (2), the oxygen that step (1) obtains is added later
The colloidal solution of graphite alkene is uniformly mixed, and is reacted 0.5-36 h under nitrogen or argon atmosphere between 70-190 DEG C, is obtained stone
The composite material of black alkene and wicker copper nanoparticle.
In the step (2) on the basis of 1 part of mantoquita, ethylene glycol, macromolecule dispersant, sodium hydroxide ethylene glycol solution
Additional amount with silver nitrate is respectively 25-50 parts, 1-3 parts, 25-50 parts and 0.1-0.3 parts, and wherein the ethylene glycol of sodium hydroxide is molten
The mass fraction of sodium hydroxide is 1%-10% in liquid.
Mantoquita is one of copper sulphate, copper chloride, copper nitrate and copper acetate or a variety of in the step (2).
It disperses 1 part of wicker copper nano particle slurry in 30-50 parts of ethylene glycol in the step (3), wicker copper nanometer
The mass ratio of particle and graphene oxide is (80-99): (1-20).
The composite material conductive material of the graphene and wicker copper nanoparticle and the application in adsorbent material.
The beneficial effects of the present invention are:
(1) by the high-ratio surface suction-operated of graphene, silver ion and copper ion can effectively be adsorbed, thus prevent silver from
Son migration, copper ion migration；Additionally, due to the oxygen characteristic that blocks water of graphene, the oxidation of silver and copper can be effectively prevented.
(2) wicker copper particle can effectively reduce contact resistance, so that this hair by the bridge joint between graphene
Bright obtained material will have preferably electric conductivity compared to the particle of single wicker copper.
(3) compared to the composite material of graphene and silver, cost is more cheap.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the stereoscan photograph of wicker copper nanoparticle prepared by embodiment 1.
Fig. 2 is the composite material stereoscan photograph of graphene and wicker copper nanoparticle prepared by embodiment 1.
Fig. 3 is the composite material stereoscan photograph of embodiment 2 gained graphene and wicker copper nanoparticle.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(a) the natural flaky graphite of 1g is added to (the matter that periodic acid is received in the concentrated sulfuric acid of 50g and the mixed solution of sodium metaperiodate
Measuring score is 4%), to stir 5 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 5 hours, gained
Mixture becomes thick；Then the water of 100g is added into the mixture, and increases temperature to 95 DEG C, maintains this temperature 60
Minute；The hydrogen peroxide of 5g is added later, and stirring adds the water of 100g, filters while hot, wash 3 with 10% dilute hydrochloric acid after 2 hours
It is secondary to be cleaned 3 times with deionized water again, gained filter cake is put into the water of 600g and is ultrasonically treated 1 hour to get graphene oxide is arrived
Colloidal solution.
(b) 100g copper chloride is dissolved in the ethylene glycol of 2500g, 200g polyvinylpyrrolidone is added, 2500g is added
The ethylene glycol solution of sodium hydroxide wherein sodium hydroxide mass fraction be 5%, after mixing evenly, nitrogen protection it is lower 150 DEG C reaction
10 hours, copper Nano sol is obtained, the silver nitrate of 10g is added, reacts 10 hours, obtains under 100 DEG C of nitrogen or argon atmosphere
Wicker copper nanoparticle；By settle, be centrifuged and etc. wash away extra macromolecule dispersant, wicker copper nano particle will be obtained
Slurry is dispersed in the ethylene glycol of 1000g.Gained wicker copper particulate scan electromicroscopic photograph is as shown in Figure 1.
(c) step a is mixed with sample obtained by step b, reacts 10 hours under 150 DEG C of nitrogen atmospheres to get graphite is arrived
The composite material of alkene and wicker copper nanoparticle.The composite material stereoscan photograph of gained graphene and wicker copper nanoparticle
As shown in Figure 2.
Embodiment 2
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(a) the natural flaky graphite of 1g is added to (the matter that periodic acid is received in the concentrated sulfuric acid of 50g and the mixed solution of sodium metaperiodate
Measuring score is 4%), to stir 5 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 5 hours, gained
Mixture becomes thick；Then the water of 100g is added into the mixture, and increases temperature to 95 DEG C, maintains this temperature 60
Minute；The hydrogen peroxide of 5g is added later, and stirring adds the water of 100g, filters while hot, wash 3 with 10% dilute hydrochloric acid after 2 hours
It is secondary to be cleaned 3 times with deionized water again, gained filter cake is put into the water of 600g and is ultrasonically treated 1 hour to get graphene oxide is arrived
Colloidal solution.
(b) 150g copper chloride is dissolved in the ethylene glycol of 2500g, 200g polyvinylpyrrolidone is added, 2500g is added
The ethylene glycol solution of sodium hydroxide wherein sodium hydroxide mass fraction be 5%, after mixing evenly, nitrogen protection it is lower 150 DEG C reaction
10 hours, copper Nano sol is obtained, the silver nitrate of 30g is added, reacts 10 hours, obtains under 100 DEG C of nitrogen or argon atmosphere
Wicker copper nanoparticle；By settle, be centrifuged and etc. wash away extra macromolecule dispersant, wicker copper nano particle will be obtained
Slurry is dispersed in the ethylene glycol of 1000g.
(c) step a is mixed with sample obtained by step b, reacts 10 hours under 150 DEG C of nitrogen atmospheres to get graphite is arrived
The composite material of alkene and wicker copper nanoparticle.The composite material stereoscan photograph of gained graphene and wicker copper nanoparticle
As shown in Figure 3.
Embodiment 3
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(a) the natural flaky graphite of 1g is added to (the matter that periodic acid is received in the concentrated sulfuric acid of 50g and the mixed solution of sodium metaperiodate
Measuring score is 4%), to stir 3 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 5 hours, gained
Mixture becomes thick；Then the water of 50g is added into the mixture, and increases temperature to 90 DEG C, this temperature 15 is maintained to divide
Clock；The hydrogen peroxide of 1g is added later, and stirring adds the water of 50g, filters while hot, wash 3 times again with 3% dilute hydrochloric acid after 2 hours
It is cleaned 3 times with deionized water, gained filter cake is put into and is ultrasonically treated 1 hour in the water of 400g to get the glue for arriving graphene oxide
Liquid solution.
(b) 100g copper chloride is dissolved in the ethylene glycol of 2500g, 100g polyvinylpyrrolidone is added, 2500g is added
The ethylene glycol solution of sodium hydroxide wherein sodium hydroxide mass fraction be 1%, after mixing evenly, nitrogen protection it is lower 180 DEG C reaction
2 hours, copper Nano sol is obtained, the silver nitrate of 10g is added, is reacted 72 hours under 60 DEG C of nitrogen or argon atmosphere, obtains silver
Copper-clad nanoparticle；By settle, be centrifuged and etc. wash away extra macromolecule dispersant, wicker copper nanoparticle slurry will be obtained
Material is dispersed in the ethylene glycol of 3000g.
(c) step a is mixed with sample obtained by step b, reacts 36 hours under 70 DEG C of nitrogen atmospheres to get graphene is arrived
With the composite material of wicker copper nanoparticle.
Embodiment 4
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(a) the natural flaky graphite of 1g is added to (the matter that periodic acid is received in the concentrated sulfuric acid of 50g and the mixed solution of sodium metaperiodate
Measuring score is 4%), to stir 4 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 5 hours, gained
Mixture becomes thick；Then the water of 60g is added into the mixture, and increases temperature to 93 DEG C, this temperature 30 is maintained to divide
Clock；The hydrogen peroxide of 3g is added later, and stirring adds the water of 60g, filters while hot, wash 4 times again with 6% dilute hydrochloric acid after 2 hours
It is cleaned 3 times with deionized water, gained filter cake is put into and is ultrasonically treated 2 hours in the water of 600g to get the glue for arriving graphene oxide
Liquid solution.
(b) 100g copper chloride is dissolved in the ethylene glycol of 3000g, 200g polyvinylpyrrolidone is added, 3000g is added
The ethylene glycol solution of sodium hydroxide wherein sodium hydroxide mass fraction be 6%, after mixing evenly, nitrogen protection it is lower 150 DEG C reaction
10 hours, copper Nano sol is obtained, the silver nitrate of 20g is added, reacts 30 hours, obtains under 100 DEG C of nitrogen or argon atmosphere
Wicker copper nanoparticle；By settle, be centrifuged and etc. wash away extra macromolecule dispersant, wicker copper nano particle will be obtained
Slurry is dispersed in the ethylene glycol of 3000-5000g.
(c) step a is mixed with sample obtained by step b, reacts 20 hours under 100 DEG C of nitrogen atmospheres to get graphite is arrived
The composite material of alkene and wicker copper nanoparticle.
Embodiment 5
A kind of preparation method of graphene and the composite material of wicker copper nanoparticle, steps are as follows:
(a) the natural flaky graphite of 1g is added to (the matter that periodic acid is received in the concentrated sulfuric acid of 50g and the mixed solution of sodium metaperiodate
Measuring score is 4%), to stir 5 hours under 0 DEG C of ice bath；Then temperature is increased again to 35 DEG C, and keeps this temperature 5 hours, gained
Mixture becomes thick；Then the water of 100g is added into the mixture, and increases temperature to 95 DEG C, maintains this temperature 60
Minute；The hydrogen peroxide of 5g is added later, and stirring adds the water of 100g, filters while hot, wash 5 with 10% dilute hydrochloric acid after 2 hours
It is secondary to be cleaned 3 times with deionized water again, gained filter cake is put into the water of 1000g and is ultrasonically treated 3 hours to get graphene oxide is arrived
Colloidal solution.
(b) 100g copper chloride is dissolved in the ethylene glycol of 5000g, 300g polyvinylpyrrolidone is added, 5000g is added
The mass fraction of the ethylene glycol solution of sodium hydroxide wherein sodium hydroxide is 10%, and after mixing evenly, lower 180 DEG C of nitrogen protection is anti-
It answers 2 hours, obtains copper Nano sol, the silver nitrate of 30g is added, react 1 hour, obtain under 150 DEG C of nitrogen or argon atmosphere
Wicker copper nanoparticle；By settle, be centrifuged and etc. wash away extra macromolecule dispersant, wicker copper nano particle will be obtained
Slurry is dispersed in the ethylene glycol of 5000g.
(c) step a is mixed with sample obtained by step b, reacts 0.5 hour under 190 DEG C of nitrogen atmospheres to get graphite is arrived
The composite material of alkene and wicker copper nanoparticle.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the composite material of a kind of graphene and wicker copper nanoparticle, it is characterised in that: the quality of graphene in composite material
Percentage is 1-20%, and the mass percent of wicker copper nanoparticle is 80-99%, and wherein wicker copper nanoparticle is adsorbed on graphite
On alkene lamella.
2. the composite material of graphene according to claim 1 and wicker copper nanoparticle, it is characterised in that: the silver packet
The size of copper nano-particle is 10-500nm.
3. the composite material of graphene according to claim 1 and wicker copper nanoparticle, it is characterised in that: the silver packet
Silver-colored mass percent is 10-30% in copper nano-particle, and the mass percent of copper is 70-90%.
4. a kind of preparation method of the composite material of graphene and wicker copper nanoparticle, it is characterised in that steps are as follows:
(1) using natural flaky graphite as raw material, the colloidal solution of graphene oxide is prepared using Hummers method；
(2) mantoquita is dissolved in ethylene glycol, the ethylene glycol solution of macromolecule dispersant and sodium hydroxide is added, stirs evenly
Afterwards, copper Nano sol is obtained in 130-180 DEG C of reaction 2-24 h under nitrogen or argon atmosphere；Nitre is added into copper Nano sol
Sour silver, 1-72 h is reacted under 60-150 DEG C of nitrogen or argon atmosphere, obtains wicker copper nano particle slurry；Sedimentation, centrifugation are washed
It washs；
(3) it disperses the wicker copper nano particle slurry that step (2) obtains in ethylene glycol, addition step (1) obtains later
The colloidal solution of graphene oxide is uniformly mixed, and 0.5-36 h is reacted under 70-190 DEG C of nitrogen or argon atmosphere, obtains graphite
The composite material of alkene and wicker copper nanoparticle.
5. the preparation method of the composite material of graphene according to claim 4 and wicker copper nanoparticle, feature exist
In: in the step (2) on the basis of 1 part of mantoquita, ethylene glycol, macromolecule dispersant, sodium hydroxide ethylene glycol solution and nitre
The additional amount of sour silver is respectively 25-50 parts, 1-3 parts, 25-50 parts and 0.1-0.3 parts, wherein in the ethylene glycol solution of sodium hydroxide
The mass fraction of sodium hydroxide is 1%-10%.
6. the preparation method of the composite material of graphene according to claim 4 and wicker copper nanoparticle, feature exist
In: mantoquita is one of copper sulphate, copper chloride, copper nitrate and copper acetate or a variety of in the step (2).
7. the preparation method of the composite material of graphene according to claim 4 and wicker copper nanoparticle, feature exist
In: disperse 1 part of wicker copper nano particle slurry in 30-50 parts of ethylene glycol in the step (3), wicker copper nano particle with
The mass ratio of graphene oxide is (80-99): (1-20).
8. the composite material of graphene described in claim 1 and wicker copper nanoparticle is in conductive material and adsorbent material
Using.
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| CN201811005727.3A CN109147985B (en) | 2018-08-30 | 2018-08-30 | Composite material of graphene and silver-coated copper nanoparticles, preparation method and application |
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| CN201811005727.3A CN109147985B (en) | 2018-08-30 | 2018-08-30 | Composite material of graphene and silver-coated copper nanoparticles, preparation method and application |
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| CN109147985B CN109147985B (en) | 2020-09-29 |
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| CN111560193A (en) * | 2020-06-10 | 2020-08-21 | 三棵树涂料股份有限公司 | Antibacterial and antiviral interior wall latex paint and preparation method thereof |
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| US20110186789A1 (en) * | 2008-05-22 | 2011-08-04 | The University Of North Carolina At Chapel Hill | Synthesis of graphene sheets and nanoparticle composites comprising same |
| CN103639421A (en) * | 2013-12-04 | 2014-03-19 | 北京印刷学院 | Preparation method for high-conductivity graphene and silver nanoparticle composite materials |
| CN104999076A (en) * | 2015-06-01 | 2015-10-28 | 浙江亚通焊材有限公司 | One-pot prepared silver covered copper nanometer powder with controllable shell thickness and preparation method of silver covered copper nanometer powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110186789A1 (en) * | 2008-05-22 | 2011-08-04 | The University Of North Carolina At Chapel Hill | Synthesis of graphene sheets and nanoparticle composites comprising same |
| CN103639421A (en) * | 2013-12-04 | 2014-03-19 | 北京印刷学院 | Preparation method for high-conductivity graphene and silver nanoparticle composite materials |
| CN104999076A (en) * | 2015-06-01 | 2015-10-28 | 浙江亚通焊材有限公司 | One-pot prepared silver covered copper nanometer powder with controllable shell thickness and preparation method of silver covered copper nanometer powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560193A (en) * | 2020-06-10 | 2020-08-21 | 三棵树涂料股份有限公司 | Antibacterial and antiviral interior wall latex paint and preparation method thereof |
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