CN114717624B - 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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- CN114717624B CN114717624B CN202210367901.9A CN202210367901A CN114717624B CN 114717624 B CN114717624 B CN 114717624B CN 202210367901 A CN202210367901 A CN 202210367901A CN 114717624 B CN114717624 B CN 114717624B
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- 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 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000006260 foam Substances 0.000 claims abstract description 33
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 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 14
- 239000006185 dispersion Substances 0.000 claims description 14
- 229910052708 sodium Inorganic materials 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- 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 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 40
- 239000002131 composite material Substances 0.000 abstract description 19
- 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
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 10
- 229940071125 manganese acetate Drugs 0.000 description 10
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 description 10
- 235000011152 sodium sulphate Nutrition 0.000 description 10
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method 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
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification 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
Classifications
-
- 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 vertically oriented graphene, and a preparation method and application thereof. And growing vertically oriented graphene on the foam nickel by an electrodeposition technology, and then depositing manganese dioxide on a substrate by taking the vertically oriented graphene grown on the foam nickel as the substrate to prepare the composite material. The method and the required equipment are simple in requirements, easy to control conditions, safe and low in cost, and 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 characteristics, including its non-agglomerated morphology and extremely large specific surface area. Vertical graphene, also known as carbon nanowall, is a graphene material with through channels and rich edges formed by a graphene sheet structure consisting of multiple layers of graphene standing vertically on a substrate. As a typical alignment material, vertical graphene has the following obvious advantages in morphology compared to conventional horizontal graphene: the vertical orientation growth avoids interlayer stacking of a horizontal structure, and improves the utilization rate of the specific surface area; the exposed edges provide chemically modified sites, while also being extremely highly conductive and electrochemically active; the vertical network structure forms a transmission channel, which is beneficial to the diffusion of ions in the channel and the transfer of electrons between graphene sheets. The vertical graphene is currently prepared by thermal chemical vapor deposition and plasma enhanced chemical vapor deposition. Because of 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, quick and low in cost, 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 cost, 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 graphene conductivity, large specific surface area and the like on one hand; on the other hand, the synergistic effect of the vertical graphene and manganese dioxide can enable the composite material to have good electrochemical performance.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the primary purpose of the invention is to provide a preparation method of vertically oriented graphene; the method is a simple electrodeposition technology, vertically oriented graphene is directly grown on foam nickel, and the obtained graphene has a larger specific surface area.
The invention also aims to provide the vertically oriented graphene prepared by the preparation method.
It is a further object of the present invention to provide an application of the above vertically oriented graphene; the application is that vertically oriented graphene grows on foam nickel as a substrate, and manganese dioxide is directly deposited on the substrate by an electrodeposition method, so that a composite material with good electrochemical performance is prepared.
The aim of the invention is achieved by the following technical scheme:
the preparation method of the vertically oriented graphene comprises the following operation steps:
(1) The foam nickel sheet is pretreated: cutting foam nickel into slices with the length of 1cm multiplied by 2cm, sequentially carrying out ultrasonic cleaning by hydrochloric acid, deionized water and ethanol, 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 in the step (1) as a working electrode, performing deposition by using a cyclic voltammetry under magnetic stirring, and then taking out the foam nickel sheet for cleaning and drying to obtain 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 1-10 mmol/L; and mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution according to a volume ratio of 1:1 to form a mixed liquid.
The number of turns deposited in the step (2) is 5-30.
The cleaning in the step (2) is carried out by deionized water.
The vertical orientation 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 vertically oriented graphene on a foam nickel sheet as a working electrode, carrying out 0.6V constant potential electrolysis, taking out the working electrode for 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 according to the volume ratio of 1:1.
The electrolysis time is 50-500s.
The cleaning is carried out by deionized water.
Compared with the prior art, the invention has the following advantages and effects:
(1) The vertical oriented graphene obtained by the method has a large specific surface area, and the 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 binder and the conductive agent, has simple equipment requirements, simple and convenient operation, safety and low cost, and is beneficial to mass production.
(3) The vertical orientation graphene/manganese dioxide composite material has excellent electrochemical performance.
Drawings
Fig. 1 is an SEM image of a vertically oriented graphene prepared in example 1.
Fig. 2 and 3 are electrochemical test results of the vertically oriented graphene/manganese dioxide composite material prepared in example 1.
Detailed Description
The present invention will be further described with reference to specific examples and drawings, but should not be construed as limiting the invention.
Example 1
(1) Firstly cutting foam nickel into slices with the length of 1cm multiplied by 2cm, sequentially ultrasonically cleaning the slices with hydrochloric acid, deionized water and ethanol, and then putting the slices into an oven for drying. Preparing graphene oxide dispersion liquid with the volume ratio of 0.3g/L and sodium chloropalladate solution with the volume ratio of 4mmol/L respectively, mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution with the volume ratio of 1:1 to form mixed liquid, taking the mixed liquid as electrolyte, taking the dried foam nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on the foam nickel sheet.
(2) Preparing a manganese acetate solution with the concentration of 0.05mol/L and a sodium sulfate solution with the concentration of 0.05mol/L respectively, mixing the manganese acetate solution and the sodium sulfate solution with the volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking vertically oriented graphene growing on foam nickel as a working electrode, electrolyzing for 200S under a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, and drying to obtain the vertically oriented graphene/manganese dioxide composite material.
Characterization of the vertically oriented graphene obtained on the foam nickel sheet in step (1) above, fig. 1 is an SEM image thereof, and it can be seen that the prepared graphene vertically and uniformly grows on the foam nickel, and a large number of pores/voids exist between the nano sheets. FIGS. 2 and 3 are electrochemical performance graphs of the vertically oriented graphene/manganese dioxide composite of step (2), at 1mA/cm 2 The discharge time under the current density reaches 1190s, and the area specific capacitance reaches 1.19F/cm 2 。
Example 2
(1) Firstly cutting foam nickel into slices with the length of 1cm multiplied by 2cm, sequentially ultrasonically cleaning the slices with hydrochloric acid, deionized water and ethanol, and then putting the slices into an oven for drying. Preparing graphene oxide dispersion liquid with the volume ratio of 0.3g/L and sodium chloropalladate solution with the volume ratio of 4mmol/L respectively, mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution with the volume ratio of 1:1 to form mixed liquid, taking the mixed liquid as electrolyte, taking the dried foam nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on the foam nickel sheet.
(2) Respectively preparing a manganese acetate solution with the concentration of 0.06mol/L and a sodium sulfate solution with the concentration of 0.06mol/L, mixing the manganese acetate solution and the sodium sulfate solution with the volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking vertically oriented graphene growing on foam nickel as a working electrode, electrolyzing for 200S under a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, drying to obtain the vertically oriented graphene/manganese dioxide composite material, and carrying out treatment on the vertically oriented graphene/manganese dioxide composite material at the concentration of 1mA/cm 2 The discharge time of the capacitor under the current density reaches 781s, and the area specific capacitance is 0.781F/cm 2 。
Example 3
(1) Firstly cutting foam nickel into slices with the length of 1cm multiplied by 2cm, sequentially ultrasonically cleaning the slices with hydrochloric acid, deionized water and ethanol, and then putting the slices into an oven for drying. Preparing graphene oxide dispersion liquid with the volume ratio of 0.3g/L and sodium chloropalladate solution with the volume ratio of 4mmol/L respectively, mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution with the volume ratio of 1:1 to form mixed liquid, taking the mixed liquid as electrolyte, taking the dried foam nickel as a working electrode, depositing for 5 circles by using a cyclic voltammetry under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on the foam nickel sheet.
(2) Respectively preparing a manganese acetate solution with the concentration of 0.06mol/L and a sodium sulfate solution with the concentration of 0.06mol/L, mixing the manganese acetate solution and the sodium sulfate solution with the volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking vertically oriented graphene growing on foam nickel as a working electrode, electrolyzing for 200S under a constant potential of 0.6V, taking out the electrode, cleaning with a large amount of deionized water, drying to obtain the vertically oriented graphene/manganese dioxide composite material, and carrying out electrolysis on the vertically oriented graphene/manganese dioxide composite material at the concentration of 1mA/cm 2 The discharge time under the current density reaches 568s, and the area specific capacitance is 0.568F/cm 2 。
Example 4
(1) Firstly cutting foam nickel into slices with the length of 1cm multiplied by 2cm, sequentially ultrasonically cleaning the slices with hydrochloric acid, deionized water and ethanol, and then putting the slices into an oven for drying. Preparing graphene oxide dispersion liquid with the volume ratio of 0.3g/L and sodium chloropalladate solution with the volume ratio of 4mmol/L respectively, mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution with the volume ratio of 1:1 to form mixed liquid, taking the mixed liquid as electrolyte, taking the dried foam nickel as a working electrode, depositing for 10 circles by using a cyclic voltammetry under magnetic stirring, taking out the working electrode, washing with a large amount of deionized water, drying, and obtaining the vertically oriented graphene on the foam nickel sheet.
(2) Respectively preparing a manganese acetate solution with the concentration of 0.06mol/L and a sodium sulfate solution with the concentration of 0.06mol/L, mixing the manganese acetate solution and the sodium sulfate solution according to the volume ratio of 1:1 to form a mixed solution, taking the mixed solution as an electrolyte, taking vertically oriented graphene growing on foam nickel as a working electrode, electrolyzing at a constant potential of 0.6V for 100S, taking out the electrode, cleaning with a large amount of deionized water, drying to obtain a vertically oriented graphene/manganese dioxide composite material, and carrying out constant potential electrolysis on the vertically oriented graphene/manganese dioxide composite material at the concentration of 1mA/cm 2 The discharge time under the current density reaches 287.6s, and the area specific capacitance is 0.2876F/cm 2 。
The foregoing examples are illustrative of the present invention and are not intended to be limiting, and other changes, modifications, substitutions, combinations and simplifications that do not depart from the spirit and principles of the invention are intended to be equivalent arrangements which are within the scope of the invention.
Claims (3)
1. The preparation method of the vertically oriented graphene is characterized by comprising the following operation steps of:
(1) The foam nickel sheet is pretreated: cutting foam nickel into 1cm multiplied by 2cm slices, sequentially carrying out ultrasonic cleaning by hydrochloric acid, deionized water and ethanol, 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 in the step (1) as a working electrode, performing deposition by using a cyclic voltammetry under magnetic stirring, and then taking out the foam nickel sheet for cleaning and drying to obtain the vertically oriented graphene on the foam nickel sheet.
2. The method for preparing the vertically oriented graphene according to claim 1, wherein the method comprises the following steps: 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 1-10 mmol/L; and mixing the graphene oxide dispersion liquid and the sodium chloropalladate solution according to a volume ratio of 1:1 to form a mixed liquid.
3. The method for preparing the vertically oriented graphene according to claim 1, wherein the method comprises the following steps: the number of turns deposited in the step (2) is 5-30.
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| CN102568853A (en) * | 2012-03-01 | 2012-07-11 | 浙江大学 | Super-capacitor electrode based on vertical oriented graphene and manufacturing method thereof |
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