CN105944721A - Hydrothermal preparation method of flaky nano copper oxide/graphene composite materials - Google Patents
Hydrothermal preparation method of flaky nano copper oxide/graphene composite materials Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 68
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 39
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 229960004643 cupric oxide Drugs 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 33
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 239000000243 solution Substances 0.000 abstract description 21
- 239000011259 mixed solution Substances 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 abstract 2
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 150000004706 metal oxides Chemical class 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229960002163 hydrogen peroxide Drugs 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- -1 lithium (sodium) ion Chemical class 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/23—
-
- B01J35/30—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a hydrothermal preparation method of flaky nano copper oxide/graphene composite materials. Copper acetate monohydrate with different mass is dissolved in deionized water, graphene oxide solutions are added to the solutions, the solutions are stirred magnetically, then sodium hydroxide is dissolved in deionized water, the mixtures are dropwise added to copper acetate monohydrate and graphene oxide mixed solutions stirred previously, the mixtures are stirred magnetically for 1 h and then subjected to hydrothermal treatment for 10 h, after the reaction ends and products are cooled to the normal temperature, the products are washed repeatedly with deionized water and then placed in a vacuum drying oven to be dried at the temperature of 60 DEG C, and flaky nano copper oxide/graphene composite material powder containing copper oxide and graphene in different mass ratios is obtained after drying. Flaky nano copper oxide/graphene composite material samples prepared with the hydrothermal method have the characteristics of good crystallinity, high uniformity, flaky microstructures and the like, and the composite materials can increase reaction rates of light-catalyzed reactions.
Description
Technical field
The present invention relates to a kind of preparation method realizing nano cupric oxide/graphene composite material, belong to field of composite material preparation.
Background technology
Copper oxide is as a kind of metal oxide semiconductor, and its energy gap is 1.7 electron-volts, can absorb visible ray, can apply
In photoelectric device, photoelectrocatalysis, energy storage and conversion, various kinds of sensors, the application of the aspects such as environment, there is low toxicity, surely
Fixed, efficiently, low cost and other advantages.Graphene is as a kind of two-dimension nano materials, and it has good dispersion, and electron mobility is high,
Nontoxic, the advantages such as specific surface area is big, Graphene is to be obtained by the graphene oxide that also reason hummers method prepares,
The advantage of the method is that course of reaction is relatively mild, compared with having higher yield from the point of view of the methods such as chemical vapour deposition technique, and preparation
Cost is relatively low.The surface of graphene oxide and marginal distribution have substantial amounts of hydroxyl and carboxyl, and therefore it shows good
Hydrophilic so that it is can be dispersed in water, and above-mentioned hydroxyl and carboxyl can be combined with metal cation, because of
This can use graphene oxide to go dispersed metal cation, makes metal cation be uniformly distributed at graphenic surface, then by spy
Fixed method processes and obtains metallic compound/graphene composite material.
The composite that the metal-oxide that Graphene loads with it is formed can show cooperative effect under certain condition.Urge at light
Changing in reaction, the catalysis activity of single metal-oxide is relatively low, is primarily due to these metal-oxides in course of reaction
In there occurs a certain degree of reunion, cause active reaction sites to reduce, the efficiency of photo-generated carrier declines, thus causes light to be urged
Change catalytic rate in reaction to reduce；Owing to Graphene has bigger specific surface area, when metal-oxide loads as light absorbent
When surface and the edge of Graphene, it is possible to effectively promote separation and the migration of photo-generated carrier, decrease photo-generated carrier
Recombination rate again, the composite construction therefore constructing copper oxide/Graphene is conducive to improving its light-catalysed reaction rate.When being applied to storage
During energy device, the negative material of such as lithium ion battery or sodium-ion battery, copper oxide/graphene composite material can utilize it
Interfacial effect, adds storage density and the cyclical stability of lithium (sodium) ion；Further, have higher due to Graphene
Carrier mobility, this is conducive to the migration of electric charge, adds the charge-discharge velocity of battery.Meanwhile, the nanostructured of copper oxide
Pattern has important impact for its application in the field such as photocatalysis, energy storage device, compares other nanostructured, lamellar
The two-dimensional nano hetero-junctions that constitutes of copper oxide and Graphene owing to there is bigger interracial contact, this makes them in photocatalysis
Journey can effectively facilitate the raising of the separation of carrier, transmission and active reaction sites；Also make them at energy storage
Part application can improve energy storage density and promote the efficiency of electric charge transmission.Therefore, flake nano copper oxide/graphene composite material
There is relatively broad application prospect.
The method preparing metal oxide composite at present is divided into solid phase method and liquid phase method, in this two classes method, mainly includes height
Temperature solid phase method, sol-gel process, chemical precipitation method, the method such as hydro-thermal method.High temperature solid-state method refers at high temperature between solid interface
Through contact, reaction, nucleation, crystal growth reacts and generates a kind of method of product, has low cost, and yield is big, preparation
The features such as technique is simple；Its shortcoming includes that energy consumption is big, and sample is easily reunited, and easily mixes impurity etc. in course of reaction.Colloidal sol-
The process of gel method is ester type compound or metal alkoxide to be dissolved in organic solvent, forms uniform solution, is subsequently adding other
Component, reaction at a certain temperature forms gel, and last drying processes and makes sample, and its advantage is that reactions steps is simple, all
Even property is good, and the temperature needed for reaction is relatively low；Its shortcoming be reaction expensive starting materials and part poisonous, the time of reaction is longer.Change
Learn the sedimentation method to refer to utilize precipitant by sample pellet under solution state, the most again sample drying or calcination process are obtained
Corresponding sample, its advantage is that the instrument used in reaction is simple, is suitable for preparing sample on a large scale, and shortcoming is difficult to sample quality
To control, uniformity is relatively low.Hydro-thermal method refers to that sample removes to create the ring of a High Temperature High Pressure in airtight container by heating
Border, makes crystal occur to dissolve this process of recrystallization in course of reaction, prepares sample by hydro-thermal method and have good dispersion,
The crystallinity high of crystal, the features such as it is middle low temperature that the method has reaction temperature, and equipment is simple, easy to operate.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the present invention provides a kind of flake nano copper oxide/graphene composite material of realizing
Hydrothermal preparing process, utilizes hydro-thermal method to prepare good crystallinity, nano cupric oxide/Graphene that uniformity is high and microscopic appearance is lamellar
Composite, this composite can promote the reaction rate of light-catalyzed reaction.
The technical solution used in the present invention step is as follows:
The first step: with deionized water dissolving one water copper acetate, obtain solution A；
Second step: use hummers method that graphite is prepared as graphene oxide solution；
3rd step: graphene oxide solution be dropwise added dropwise in solution A, magnetic agitation obtains solution B in 8 hours；
4th step: sodium hydroxide is dissolved in deionized water, is added dropwise to solution B, the most again magnetic agitation 1 hour
Obtain solution C；
5th step: solution C be transferred in the polytetrafluoroethyllining lining of rustless steel autoclave, reacts 10 at 100 degrees Celsius
Hour obtain mixed reaction product D, after rustless steel autoclave naturally cools to room temperature, first remove the supernatant,
Subsequently mixed reaction product D is transferred in beaker；
6th step: use deionized water to clean product D, the supernatant waste liquid after using pH meter detection to clean, when supernatant waste liquid
PH value when reaching 7, obtain aqueous solid product E after staticly settling removing supernatant；
7th step: put in vacuum drying oven by aqueous solid product E, 60 degrees Celsius are dried 24 hours, obtain the sheet being dried
Shape nano cupric oxide/graphene composite material.
The mass ratio of the described graphene oxide in graphene oxide solution and a water copper acetate is 3%～6%.
A described water copper acetate is 1: 20 with the mol ratio of sodium hydroxide.
It is with graphite as raw material that described hummers method prepares the basic process of graphene oxide, uses concentrated sulphuric acid and potassium permanganate
As oxidant, it is added sequentially in graphite, after stirring 6 hours, by deionized water and hydrogenperoxide steam generator the most successively
It is added thereto, uses hydrochloric acid and deionized water that sample is carried out pickling and washing the most respectively, utilize ultrasonic Treatment afterwards
Sample, is scattered in graphene oxide in aqueous solution, forms graphene oxide solution.
The invention has the beneficial effects as follows:
1. use Graphene to be combined with nano cupric oxide, cupric oxide nano structure can be avoided to reunite in course of reaction, have
It is beneficial to improve copper oxide/Graphene composite nanostructure carrier separation during light-catalyzed reaction, transmission,
Reduce the recombination rate again after the separation of carrier；Be conducive to this composite construction as lithium (sodium) ion battery negative pole
There is during material higher electrical conductance, energy storage density and cyclical stability.
2. the flake nano copper oxide/graphene composite material sample using hydro-thermal method to prepare has good crystallinity, and sample is homogeneous
Degree high, and technique is simple, favorable repeatability.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the flake nano copper oxide/graphene composite material of embodiment 1 gained.
Fig. 2 is the stereoscan photograph of the flake nano copper oxide/graphene composite material of embodiment 1 gained.
Fig. 3 is the XRD figure spectrum of the flake nano copper oxide/graphene composite material of embodiment 2 gained.
Fig. 4 is the stereoscan photograph of the flake nano copper oxide/graphene composite material of embodiment 2 gained.
Fig. 5 is the XRD figure spectrum of the flake nano copper oxide/graphene composite material of embodiment 3 gained.
Fig. 6 is the stereoscan photograph of the flake nano copper oxide/graphene composite material of embodiment 3 gained.
Detailed description of the invention
The method using hummers method to prepare graphene oxide is: the graphite of 0.8 gram is slowly put into 50 milliliters of mass fractions 98%
Concentrated sulphuric acid in, use glass rod to be stirred continuously, afterwards 4 grams of potassium permanganate divided 10 addition, every time need to stir with glass rod after addition
Mixing 30 seconds, sample uses magnetic stirrer 6 hours afterwards, after the stirring until 6 hours completes, by 100 milliliters of deionizations
Water is slowly dropped into just in the sample of magnetic agitation, is slowly dripped by the hydrogenperoxide steam generator that 4 milliliters of mass fractions are 30% the most again
Enter just in the sample of magnetic agitation, then sample is used ultrasonic Treatment 30 minutes；The dilute salt using mass fraction to be 9%
Acid solution wash sample, afterwards to sample centrifugal treating, this process is repeated 3 times；Make to be washed with deionized sample, the most right
Sample centrifugal treating, this process is repeated 3 times；Afterwards sample is used ultrasonic Treatment 15 minutes, after it cools down, take unit
The sample of quality is dried, the mass fraction of the graphene oxide can being calculated in graphene oxide solution.
Embodiment 1:
833 milligram of one water copper acetate is dissolved in 25 ml deionized water, magnetic agitation 10 minutes, molten at copper acetate afterwards
Liquid adds the solution containing 50 milligrams of graphene oxides, continues magnetic agitation 10 hours；3.331 grams of sodium hydroxide are dissolved in
15 ml deionized water, stir 10 minutes, are added into afterwards in the mixed solution of copper acetate and graphene oxide, and magnetic force stirs
Mix 1 hour, then mixed solution is transferred to the polytetrafluoroethyllining lining of 100 milliliters of rustless steel autoclaves, use air blast
Under 100 degrees Celsius, it is incubated 10 hours in drying baker, makes it naturally cool to room temperature afterwards, take out sample, use deionized water
Solid repeatedly, during until the pH of the waste liquid after Xi Di is neutral, is sent into the vacuum drying oven condition in vacuum by water washing sample
Under with 60 degrees Celsius be dried 12 hours, obtained copper oxide/graphene composite material afterwards.Fig. 1 is that this copper oxide/Graphene is multiple
The XRD figure spectrum of condensation material, the three strongest ones peak (2 θ angles are 36.4 °, 42.3 °, 61.4 °) of this collection of illustrative plates and the standard of copper oxide
The three strongest ones peak of card (JCPDS NO.67-850) coincide, and the thing of sample synthesized by embodiment 1 is copper oxide mutually.Fig. 2 is this
The scanning electron microscope (SEM) photograph of copper oxide/graphene composite material, electron microscopic picture shows that the microscopic appearance of this material is lamellar, the thickness of lamellar
Concentrate in the range of 30～40nm.
Embodiment 2:
1249 milligram of one water copper acetate is dissolved in 25 ml deionized water, magnetic agitation 10 minutes, molten at copper acetate afterwards
Liquid adds the solution containing 50 milligrams of graphene oxides, continues magnetic agitation 10 hours；4.997 grams of sodium hydroxide are dissolved in
15 ml deionized water, stir 10 minutes, are added into afterwards in the mixed solution of copper acetate and graphene oxide, and magnetic force stirs
Mix 1 hour, then mixed solution is transferred to the polytetrafluoroethyllining lining of 100 milliliters of rustless steel autoclaves, use air blast
Under 100 degrees Celsius, it is incubated 10 hours in drying baker, makes it naturally cool to room temperature afterwards, take out sample, use deionized water
Solid repeatedly, during until the pH of the waste liquid after Xi Di is neutral, is sent into the vacuum drying oven condition in vacuum by water washing sample
Under with 60 degrees Celsius be dried 12 hours, obtained copper oxide/graphene composite material afterwards.Fig. 3 is that this copper oxide/Graphene is multiple
The XRD figure spectrum of condensation material, the three strongest ones peak (2 θ angles are 36.4 °, 42.3 °, 61.4 °) of this collection of illustrative plates and the standard of copper oxide
The three strongest ones peak of card (JCPDS NO.67-850) coincide, and the thing of sample synthesized by embodiment 2 is copper oxide mutually.Fig. 4 is this
The scanning electron microscope (SEM) photograph of copper oxide/graphene composite material, electron microscopic picture shows that the microscopic appearance of this material is lamellar, the thickness of lamellar
Concentrate in the range of 25～35nm.
Embodiment 3:
1666 milligram of one water copper acetate is dissolved in 25 ml deionized water, magnetic agitation 10 minutes, molten at copper acetate afterwards
Liquid adds the solution containing 50 milligrams of graphene oxides, continues magnetic agitation 10 hours；6.662 grams of sodium hydroxide are dissolved in
15 ml deionized water, stir 10 minutes, are added into afterwards in the mixed solution of copper acetate and graphene oxide, and magnetic force stirs
Mix 1 hour, then mixed solution is transferred to the polytetrafluoroethyllining lining of 100 milliliters of rustless steel autoclaves, use air blast
Under 100 degrees Celsius, it is incubated 10 hours in drying baker, makes it naturally cool to room temperature afterwards, take out sample, use deionized water
Solid repeatedly, during until the pH of the waste liquid after Xi Di is neutral, is sent into the vacuum drying oven condition in vacuum by water washing sample
Under with 60 degrees Celsius be dried 12 hours, obtained copper oxide/graphene composite material afterwards.Fig. 5 is that this copper oxide/Graphene is multiple
The XRD figure spectrum of condensation material, the three strongest ones peak (2 θ angles are 36.4 °, 42.3 °, 61.4 °) of this collection of illustrative plates and the standard of copper oxide
The three strongest ones peak of card (JCPDS NO.67-850) coincide, and the thing of sample synthesized by embodiment 3 is copper oxide mutually.Fig. 6 is this
The scanning electron microscope (SEM) photograph of copper oxide/graphene composite material, electron microscopic picture shows that the microscopic appearance of this material is lamellar, the thickness of lamellar
Concentrate in the range of 25～30nm.
Claims (3)
1. the hydrothermal preparing process of flake nano copper oxide/graphene composite material, it is characterised in that:
The first step: with deionized water dissolving one water copper acetate, obtain solution A；
Second step: use hummers method that graphite is prepared as graphene oxide solution；
3rd step: graphene oxide solution be dropwise added dropwise in solution A, magnetic agitation obtains solution B in 8 hours；
4th step: sodium hydroxide is dissolved in deionized water, is added dropwise to solution B, the most again magnetic agitation 1 hour
Obtain solution C；
5th step: solution C be transferred in the polytetrafluoroethyllining lining of rustless steel autoclave, reacts 10 at 100 degrees Celsius
Hour obtain mixed reaction product D, after rustless steel autoclave naturally cools to room temperature, first remove the supernatant,
Subsequently mixed reaction product D is transferred in beaker；
6th step: use deionized water to clean product D, the supernatant waste liquid after using pH meter detection to clean, when supernatant waste liquid
PH value when reaching 7, obtain aqueous solid product E after staticly settling removing supernatant；
7th step: put in vacuum drying oven by aqueous solid product E, 60 degrees Celsius are dried 24 hours, obtain the sheet being dried
Shape nano cupric oxide/graphene composite material.
The hydrothermal preparing process of a kind of flake nano copper oxide/graphene composite material the most according to claim 1, its feature exists
In: the mass ratio of the described graphene oxide in graphene oxide solution and a water copper acetate is 3%～6%.
The hydrothermal preparing process of a kind of flake nano copper oxide/graphene composite material the most according to claim 1, its feature exists
In: a described water copper acetate is 1: 20 with the mol ratio of sodium hydroxide.
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| CN106517161A (en) * | 2016-11-16 | 2017-03-22 | 常州大学 | Preparation method for compounding copper oxide nitrogen-doped graphene aerogel based on hydrothermal method |
| CN106732589A (en) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | A kind of preparation method of cupric oxide/cuprous oxide/graphene nanocomposite material |
| CN106920592A (en) * | 2017-04-10 | 2017-07-04 | 徐州乐泰机电科技有限公司 | A kind of power cable |
| CN106935826A (en) * | 2017-03-23 | 2017-07-07 | 江西理工大学 | The lithium ion battery preparation method of nano cupric oxide graphene composite material |
| CN107089683A (en) * | 2017-04-25 | 2017-08-25 | 中国计量大学 | A kind of preparation method of molybdenum disulfide/copper sulfide/cuprous nano composite |
| CN108199078A (en) * | 2018-01-03 | 2018-06-22 | 深圳锂硫科技有限公司 | A kind of lithium ion battery |
| CN108346782A (en) * | 2017-12-28 | 2018-07-31 | 杭州电子科技大学 | Porous copper oxide microballoon/multi-layer graphene composite material and preparation method |
| CN110813293A (en) * | 2019-10-31 | 2020-02-21 | 曲阜师范大学 | Preparation method and application of Cu NPs-rGO electrocatalyst |
| CN111422896A (en) * | 2019-01-10 | 2020-07-17 | 中国计量大学 | Preparation method of bitter gourd-shaped CuO nanoparticle SERS substrate |
| CN113040172A (en) * | 2021-03-10 | 2021-06-29 | 西北农林科技大学 | Reduced graphene oxide-metal/metal oxide functional composite material, preparation method and application thereof |
| CN113675393A (en) * | 2021-08-20 | 2021-11-19 | 西安热工研究院有限公司 | Morphology-controllable high-performance lithium ion battery negative electrode material and preparation method thereof |
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| CN106517161B (en) * | 2016-11-16 | 2018-10-19 | 常州大学 | A kind of preparation of hydro-thermal method synthesis copper oxide nitrogen-doped graphene aeroge |
| CN106517161A (en) * | 2016-11-16 | 2017-03-22 | 常州大学 | Preparation method for compounding copper oxide nitrogen-doped graphene aerogel based on hydrothermal method |
| CN106732589A (en) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | A kind of preparation method of cupric oxide/cuprous oxide/graphene nanocomposite material |
| CN106935826A (en) * | 2017-03-23 | 2017-07-07 | 江西理工大学 | The lithium ion battery preparation method of nano cupric oxide graphene composite material |
| CN106935826B (en) * | 2017-03-23 | 2020-06-12 | 江西理工大学 | Preparation method of nano copper oxide graphene composite material for lithium ion battery |
| CN106920592A (en) * | 2017-04-10 | 2017-07-04 | 徐州乐泰机电科技有限公司 | A kind of power cable |
| CN107089683B (en) * | 2017-04-25 | 2019-02-15 | 中国计量大学 | A kind of preparation method of molybdenum disulfide/copper sulfide/cuprous nano composite material |
| CN107089683A (en) * | 2017-04-25 | 2017-08-25 | 中国计量大学 | A kind of preparation method of molybdenum disulfide/copper sulfide/cuprous nano composite |
| CN108346782A (en) * | 2017-12-28 | 2018-07-31 | 杭州电子科技大学 | Porous copper oxide microballoon/multi-layer graphene composite material and preparation method |
| CN108346782B (en) * | 2017-12-28 | 2020-08-04 | 杭州电子科技大学 | Porous copper oxide microsphere/multilayer graphene composite material and preparation method thereof |
| CN108199078A (en) * | 2018-01-03 | 2018-06-22 | 深圳锂硫科技有限公司 | A kind of lithium ion battery |
| CN111422896A (en) * | 2019-01-10 | 2020-07-17 | 中国计量大学 | Preparation method of bitter gourd-shaped CuO nanoparticle SERS substrate |
| CN111422896B (en) * | 2019-01-10 | 2022-07-15 | 中国计量大学 | Preparation method of bitter gourd-shaped CuO nanoparticle SERS substrate |
| CN110813293A (en) * | 2019-10-31 | 2020-02-21 | 曲阜师范大学 | Preparation method and application of Cu NPs-rGO electrocatalyst |
| CN113040172A (en) * | 2021-03-10 | 2021-06-29 | 西北农林科技大学 | Reduced graphene oxide-metal/metal oxide functional composite material, preparation method and application thereof |
| CN113675393A (en) * | 2021-08-20 | 2021-11-19 | 西安热工研究院有限公司 | Morphology-controllable high-performance lithium ion battery negative electrode material and preparation method thereof |
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