CN114717624A - Vertically oriented graphene and preparation method and application thereof - Google Patents
Vertically oriented graphene and preparation method and application thereof Download PDFInfo
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- CN114717624A CN114717624A CN202210367901.9A CN202210367901A CN114717624A CN 114717624 A CN114717624 A CN 114717624A CN 202210367901 A CN202210367901 A CN 202210367901A CN 114717624 A CN114717624 A CN 114717624A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 72
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 229940071125 manganese acetate Drugs 0.000 claims description 8
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 5
- 238000004070 electrodeposition Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- KQFUCKFHODLIAZ-UHFFFAOYSA-N manganese Chemical compound [Mn].[Mn] KQFUCKFHODLIAZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of nano material preparation, and discloses a vertically oriented graphene, and a preparation method and application thereof. Vertically oriented graphene grows on the foamed nickel through an electrodeposition technology, and then the vertically oriented graphene growing on the foamed nickel is used as a substrate, and manganese dioxide is deposited on the substrate to obtain the composite material. The method and the required equipment have the advantages of simple requirements, easily-controlled conditions, safety and low cost, the prepared graphene has a large specific surface area, and the composite material obtained by compounding the graphene and manganese dioxide has good electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to vertically oriented graphene and a preparation method and application thereof.
Background
Vertical graphene is of great interest due to its unique structural properties, including its non-agglomerated morphological features and extremely large specific surface area. The vertical graphene is also called a carbon nanowall, and is a graphene material which is formed by vertically standing a graphene sheet structure consisting of multiple layers of graphene on a substrate and has a through channel and rich edges. As a typical oriented material, the vertical graphene has the following obvious advantages in morphology compared with the traditional horizontal graphene: the vertical orientation growth avoids the interlayer stacking of a horizontal structure, and the utilization rate of the specific surface area is improved; the exposed edge provides a chemical modification site and has extremely high conductivity and electrochemical activity; the vertical network structure forms a transmission channel, which is beneficial to the diffusion of ions in the channel and the transmission of electrons between graphene sheets. At present, the preparation of the vertical graphene is carried out by a thermal chemical vapor deposition method and a plasma enhanced chemical vapor deposition method. Due to the chemical vapor deposition method, the required equipment is complex, the conditions are harsh, high-temperature vacuum is involved, the cost is high, only pure graphene materials can be obtained, and the application range of the materials is narrow. The electrodeposition technology is simple, rapid and cheap, and various composite materials can be prepared by selecting proper composite components, so that the application range is wide.
Manganese dioxide has the advantages of low price, abundant reserves, environmental friendliness, high specific capacitance, wide voltage window and the like, but the poor conductivity and reversibility limit the practical application of manganese dioxide electrode materials, so that manganese dioxide and graphene with good conductivity are compounded, and the prepared graphene/manganese dioxide composite material can exert the characteristics of high conductivity, large specific surface area and the like of the graphene on one hand; on the other hand, the composite material has good electrochemical performance due to the synergistic effect of the vertical graphene and the manganese dioxide.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide a preparation method of vertically oriented graphene; the method is a simple electrodeposition technology, the vertically oriented graphene directly grows on the foamed nickel, and the obtained graphene has a large specific surface area.
The invention further aims to provide the vertically-oriented graphene prepared by the preparation method.
Still another object of the present invention is to provide an application of the above vertically aligned graphene; the application is that vertically oriented graphene growing on foamed nickel is used as a substrate, and then manganese dioxide is directly deposited on the substrate by an electrodeposition method to prepare the composite material with good electrochemical performance.
The purpose of the invention is realized by the following technical scheme:
a preparation method of vertically-oriented graphene comprises the following operation steps:
(1) pretreating the foamed nickel sheet: cutting the foamed nickel into slices of 1cm multiplied by 2cm, carrying out ultrasonic cleaning by using hydrochloric acid, deionized water and ethanol in sequence, and then drying;
(2) preparing a mixed solution of graphene oxide dispersion liquid and a sodium chloropalladate solution, taking the mixed solution as an electrolyte, taking the dried foam nickel sheet obtained in the step (1) as a working electrode, depositing by using a cyclic voltammetry under magnetic stirring, taking out the foam nickel sheet, cleaning and drying the foam nickel sheet, and obtaining the vertically oriented graphene on the foam nickel sheet.
The concentration of the graphene oxide dispersion liquid in the step (2) is 0.1-1g/L, and the concentration of the sodium chloropalladate solution is 1mmol/L-10 mmol/L; and mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution according to the volume ratio of 1:1 to form a mixed liquid.
The number of the deposited circles in the step (2) is 5-30 circles.
And (3) cleaning with deionized water in the step (2).
The vertically oriented graphene prepared by the preparation method is provided.
The application of the vertically oriented graphene in preparing the vertically oriented graphene/manganese dioxide composite material comprises the following steps: preparing a mixed solution of manganese acetate and sodium sulfate, taking the mixed solution as an electrolyte, taking the vertically oriented graphene on the foamed nickel sheet as a working electrode, electrolyzing at a constant potential of 0.6V, taking out the working electrode, cleaning, and drying to obtain the vertically oriented graphene/manganese dioxide composite material.
The mixed solution is prepared by mixing a manganese acetate solution with the concentration of 0.01-0.1mol/L and a sodium sulfate solution with the concentration of 0.01-0.1mol/L in a volume ratio of 1: 1.
The time of the electrolysis is 50-500 s.
The cleaning is performed by using deionized water.
Compared with the prior art, the invention has the following advantages and effects:
(1) the vertically oriented graphene obtained by the invention has a large specific surface area, and a vertical network structure forms a transmission channel, so that ions can be diffused in the channel and electrons can be transferred between graphene sheets.
(2) The preparation method of the invention avoids the use of the adhesive and the conductive agent, has simple requirement on the required equipment, simple and convenient operation, safety and low cost, and is beneficial to large-scale production.
(3) The vertically-oriented graphene/manganese dioxide composite material obtained by the invention has excellent electrochemical performance.
Drawings
Fig. 1 is an SEM image of one of the vertically aligned graphene prepared in example 1.
Fig. 2 and 3 are electrochemical test results of the vertically aligned graphene/manganese dioxide composite material prepared in example 1.
Detailed Description
The following further describes the present invention with reference to specific examples and drawings, but the present invention should not be construed as being limited thereto.
Example 1
(1) Firstly, cutting the foamed nickel into slices of 1cm multiplied by 2cm, ultrasonically cleaning the slices by hydrochloric acid, deionized water and ethanol in sequence, and then drying the slices in an oven. Respectively preparing 0.3g/L graphene oxide dispersion liquid and 4mmol/L sodium chloropalladate solution, mixing the two solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the dried foamed nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry method under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on a foamed nickel sheet.
(2) Respectively preparing 0.05mol/L manganese acetate solution and 0.05mol/L sodium sulfate solution, mixing the solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the vertically oriented graphene growing on the foamed nickel as a working electrode, electrolyzing for 200S at a constant potential of 0.6V, taking out the electrode, washing with a large amount of deionized water, and drying to obtain the vertically oriented graphene/manganese dioxide composite material.
Characterizing the vertically oriented graphene obtained on the nickel foam sheet in the step (1), and referring to fig. 1 as an SEM image thereof, it can be seen that the prepared graphene vertically and uniformly grows on the nickel foam sheet, and a large number of pores/voids exist between the nano sheets. FIG. 2 and FIG. 3 are the electrochemical performance diagrams of the vertically oriented graphene/manganese dioxide composite material obtained in step (2), at 1mA/cm2The discharge time reaches 1190s under the current density, and the area specific capacitance reaches 1.19F/cm2。
Example 2
(1) Firstly, cutting the foamed nickel into slices of 1cm multiplied by 2cm, ultrasonically cleaning the slices by hydrochloric acid, deionized water and ethanol in sequence, and then drying the slices in an oven. Respectively preparing 0.3g/L graphene oxide dispersion liquid and 4mmol/L sodium chloropalladate solution, mixing the two solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the dried foamed nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry method under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on a foamed nickel sheet.
(2) Respectively preparing 0.06mol/L manganese acetate solution and 0.06mol/L sodium sulfate solution, mixing the solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the vertically oriented graphene growing on the foamed nickel as a working electrode, electrolyzing for 200 seconds at a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, drying to obtain a vertically oriented graphene/manganese dioxide composite material, and obtaining the composite material at 1mA/cm2The discharge time under the current density reaches 781s, and the area specific capacitance is 0.781F/cm2。
Example 3
(1) Firstly, cutting the foamed nickel into slices of 1cm multiplied by 2cm, ultrasonically cleaning the slices by hydrochloric acid, deionized water and ethanol in sequence, and then drying the slices in an oven. Respectively preparing 0.3g/L graphene oxide dispersion liquid and 4mmol/L sodium chloropalladate solution, mixing the two solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the dried foamed nickel as a working electrode, depositing for 5 circles by using a cyclic voltammetry method under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on a foamed nickel sheet.
(2) Respectively preparing 0.06mol/L manganese acetate solution and 0.06mol/L sodium sulfate solution, mixing the solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the vertically oriented graphene growing on the foamed nickel as a working electrode, electrolyzing for 200 seconds at a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, and drying to obtain the manganese-manganese mixed solutionTo a vertically oriented graphene/manganese dioxide composite at 1mA/cm2The discharge time under the current density reaches 568s, and the area specific capacitance is 0.568F/cm2。
Example 4
(1) Firstly, cutting the foamed nickel into slices of 1cm multiplied by 2cm, ultrasonically cleaning the slices by hydrochloric acid, deionized water and ethanol in sequence, and then putting the slices into an oven to dry. Respectively preparing 0.3g/L graphene oxide dispersion liquid and 4mmol/L sodium chloropalladate solution, mixing the two solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the dried foamed nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry method under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on a foamed nickel sheet.
(2) Respectively preparing 0.06mol/L manganese acetate solution and 0.06mol/L sodium sulfate solution, mixing the solutions in a volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking the vertically oriented graphene growing on the foamed nickel as a working electrode, electrolyzing for 100S at a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, drying to obtain a vertically oriented graphene/manganese dioxide composite material, and obtaining the composite material at a concentration of 1mA/cm2The discharge time under the current density reaches 287.6s, and the area specific capacitance is 0.2876F/cm2。
The above embodiments are suitable embodiments of the present invention, and the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent replacements within the protection scope of the present invention.
Claims (9)
1. A preparation method of vertically-oriented graphene is characterized by comprising the following operation steps:
(1) pretreating the foamed nickel sheet: cutting the foamed nickel into slices of 1cm multiplied by 2cm, carrying out ultrasonic cleaning by using hydrochloric acid, deionized water and ethanol in sequence, and then drying;
(2) preparing a mixed solution of graphene oxide dispersion liquid and a sodium chloropalladate solution, taking the mixed solution as an electrolyte, taking the dried foam nickel sheet obtained in the step (1) as a working electrode, depositing by using a cyclic voltammetry under magnetic stirring, taking out the foam nickel sheet, cleaning and drying the foam nickel sheet, and obtaining the vertically oriented graphene on the foam nickel sheet.
2. The method for preparing vertically aligned graphene according to claim 1, wherein: the concentration of the graphene oxide dispersion liquid in the step (2) is 0.1-1g/L, and the concentration of the sodium chloropalladate solution is 1mmol/L-10 mmol/L; and mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution according to the volume ratio of 1:1 to form a mixed liquid.
3. The method for preparing vertically aligned graphene according to claim 1, wherein: the number of the deposited circles in the step (2) is 5-30 circles.
4. The method of claim 1, wherein the method comprises the steps of: and (3) cleaning with deionized water in the step (2).
5. A vertically aligned graphene produced by the production method according to any one of claims 1 to 4.
6. Use of the vertically oriented graphene according to claim 5 in the preparation of a vertically oriented graphene/manganese dioxide composite material, wherein: the application comprises the following steps: preparing a mixed solution of manganese acetate and sodium sulfate, taking the mixed solution as an electrolyte, taking the vertically oriented graphene on the foamed nickel sheet as a working electrode, electrolyzing at a constant potential of 0.6V, taking out the working electrode, cleaning, and drying to obtain the vertically oriented graphene/manganese dioxide composite material.
7. Use according to claim 6, characterized in that: the mixed solution is prepared by mixing a manganese acetate solution with the concentration of 0.01-0.1mol/L and a sodium sulfate solution with the concentration of 0.01-0.1mol/L in a volume ratio of 1: 1.
8. Use according to claim 6, characterized in that: the time of the electrolysis is 50-500 s.
9. Use according to claim 6, characterized in that: the cleaning is performed by using deionized water.
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