CN115424874B - MXene-based flexible supercapacitor electrode material and preparation method thereof - Google Patents
MXene-based flexible supercapacitor electrode material and preparation method thereof Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- VCDRAONLIPOEFL-UHFFFAOYSA-N 4-n-[4-(4-anilinoanilino)phenyl]benzene-1,4-diamine Chemical compound C1=CC(N)=CC=C1NC(C=C1)=CC=C1NC(C=C1)=CC=C1NC1=CC=CC=C1 VCDRAONLIPOEFL-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000725 suspension Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000002356 single layer Substances 0.000 claims abstract description 35
- 238000005406 washing Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 22
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 14
- ATGUVEKSASEFFO-UHFFFAOYSA-N p-aminodiphenylamine Chemical compound C1=CC(N)=CC=C1NC1=CC=CC=C1 ATGUVEKSASEFFO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 10
- SBZDIRMBQJDCLB-UHFFFAOYSA-N 5-azidopentanoic acid Chemical compound OC(=O)CCCCN=[N+]=[N-] SBZDIRMBQJDCLB-UHFFFAOYSA-N 0.000 claims abstract description 8
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 125000000852 azido group Chemical group *N=[N+]=[N-] 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000178 monomer Substances 0.000 claims abstract description 3
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 27
- IVRMZWNICZWHMI-UHFFFAOYSA-N azide group Chemical group [N-]=[N+]=[N-] IVRMZWNICZWHMI-UHFFFAOYSA-N 0.000 claims description 22
- 239000006228 supernatant Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- 230000007935 neutral effect Effects 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000009830 intercalation Methods 0.000 abstract description 3
- 230000002687 intercalation Effects 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 description 19
- 229910021641 deionized water Inorganic materials 0.000 description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 239000007788 liquid Substances 0.000 description 16
- 229920000767 polyaniline Polymers 0.000 description 15
- -1 azido compound Chemical class 0.000 description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 230000014759 maintenance of location Effects 0.000 description 11
- 238000001291 vacuum drying Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- 229910021607 Silver chloride Inorganic materials 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 238000012983 electrochemical energy storage Methods 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 150000001540 azides Chemical class 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- 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
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Abstract
The invention relates to the field of supercapacitor electrode materials, and discloses an MXene-based flexible supercapacitor electrode material and a preparation method thereof. The preparation method comprises the following steps: preparing an MXene monolayer suspension; synthesizing tetraaniline by taking N-phenyl-1, 4-phenylenediamine as a monomer; dissolving 5-azido valeric acid, dicyclohexylcarbodiimide, trimethylamine, 4-dimethylaminopyridine and tetraaniline in a reaction solvent, and separating a reaction product after stirring for reaction to obtain modified tetraaniline containing azido groups; dissolving modified tetra-aniline containing azido groups in a solvent, dropwise adding MXene single-layer suspension into the solvent, stirring, performing ultraviolet irradiation treatment, centrifuging, washing with ethanol, washing with water, and performing suction filtration and drying on the obtained solution. The preparation method can realize stable combination between the intercalation agent and the MXene, and effectively improve the electrochemical performance of the MXene-based flexible supercapacitor electrode material.
Description
Technical Field
The invention relates to the field of supercapacitor electrode materials, in particular to an MXene-based flexible supercapacitor electrode material and a preparation method thereof.
Background
In recent years, wearable electronic equipment is rapidly developed, and further the demand of a flexible supercapacitor is stimulated, and the supercapacitor has the advantages of high power density, short charging time, good cycle performance and the like. Among them, an electrode material having a large volume capacity, high conductivity, and high electrochemical performance is indispensable for a supercapacitor. 2D materials with large electrochemically active surfaces have attracted extensive research interest, such as graphene, carbon nanotubes, etc., but are limited to carbon chemistry and are not capable of undergoing redox reactions with metals.
Two-dimensional material Ti 3 C 2 T x Mxene is a new 2D electrode material with great potential in supercapacitor applications. It has a high specific surface area, and can perform a rapid surface oxidation-reduction reaction through an effective specific surface area, thereby storing charges. The MXene sheets tend to re-stack during electrode fabrication, which severely reduces ion transport in the electrode structure. In order to solve the problem, researchers construct more laminar material structures, provide more paths for transporting and storing electrolyte ions, lead materials such as carbon nano tubes and graphene oxide, lead conductive polymers such as polypyrrole and polyaniline, lead materials such as metal oxide (molybdenum disulfide and manganese dioxide) and the like into MXene for compounding, effectively relieve self-stacking and improve electrochemical energy storage performance. Among them, polyaniline is widely used because of its high conductivity and high theoretical capacitance. However, the rigidity of polyaniline itself results in poor solubility in aqueous and organic solvents, limiting the complexing with many materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides an MXene-based flexible supercapacitor electrode material and a preparation method thereof. The preparation method can realize stable combination between the intercalation agent (tetra-aniline) and the MXene, and effectively improve the electrochemical performance of the MXene-based flexible supercapacitor electrode material.
The specific technical scheme of the invention is as follows:
in a first aspect, the invention provides a method for preparing an MXene-based flexible supercapacitor electrode material, which comprises the following steps:
(1) Preparing an MXene monolayer suspension;
(2) Synthesizing tetraaniline by taking N-phenyl-1, 4-phenylenediamine as a monomer;
(3) Dissolving 5-azido valeric acid, dicyclohexylcarbodiimide, trimethylamine, 4-dimethylaminopyridine and tetraaniline in a reaction solvent, and separating out a reaction product after stirring reaction to obtain modified tetraaniline containing azido groups;
(4) Dissolving modified tetraaniline containing an azide group in a solvent, dropwise adding an MXene single-layer suspension into the solvent, stirring the mixture, performing ultraviolet irradiation treatment, centrifuging, washing with ethanol, washing with water, and adding water to obtain an electrode material suspension;
under the irradiation of ultraviolet light, in the modified tetraaniline containing the azide group, the azide group is decomposed into nitrogen and nitrene, the nitrene is very active, and can be combined with H on MXene to form a stable covalent bond;
(5) And carrying out suction filtration on the electrode material suspension, and then drying the obtained film to obtain the MXene-based flexible supercapacitor electrode material.
The invention firstly prepares MXene monolayer suspension, then grafts polyaniline conjugated repetitive unit tetra-aniline with minimum polyaniline onto MXene nano-sheets through photochemical action of organic azide, and realizes the compounding of the tetra-aniline and the MXene.
The tetraaniline has the advantages of pseudocapacitance, high conductivity and the like, and can increase the interlayer spacing of the MXene after being stably combined with the MXene as an intercalation agent, promote the transportation of electrolyte ions, effectively increase the specific surface area and electrochemical active sites of the MXene, and further improve the electrochemical energy storage performance of the MXene. Compared with common polyaniline, the polyaniline (aniline tetramer) has a shorter chain length, and can reduce the volume degradation easily occurring in the repeated charge and discharge process.
In addition, the invention utilizes the photochemical action of amino and 5-azido valeric acid in the tetraaniline and the organic azido compound to enable the MXene and the tetraaniline to be combined in a covalent bond mode, thereby reducing the risk of falling off the tetraaniline, being beneficial to ensuring the synergy between the two and increasing the cycle stability during energy storage.
Preferably, the step (1) specifically includes the steps of: stirring LiF and hydrochloric acid vigorously for 30-40min to obtain a mixed solution; then Ti is added in 10-20min 3 AlC 2 Slowly adding the precursor into the mixed solution, and continuing stirring for reaction; after the reaction is completed, the mixture is centrifuged, washed with acid and washed with water to be neutral, then treated with ultrasonic, and finally centrifuged to collect supernatant, thus obtaining the MXene monolayer suspension.
Preferably, in the step (1), the temperature of the continuous stirring reaction is 40-45 ℃ and the time is 36-48h.
Preferably, in the step (1), the ultrasonic treatment is performed in an ice bath for 90-120min.
Preferably, the step (2) specifically includes the following steps: preparing N-phenyl-1, 4-phenylenediamine, ferric trichloride hexahydrate and hydrochloric acid into a reaction solution, reacting for 2-3 hours at 20-30 ℃, and separating and purifying the product to obtain the tetra-aniline.
Preferably, in the step (3), the temperature of the stirring reaction is 20-30 ℃ and the time is 36-48h.
Preferably, in the step (4), the mass ratio of the MXene to the modified tetraaniline containing the azide group is 1-9:1.
Preferably, in the step (4), the temperature of the stirring is 20-30 ℃ and the time is 3-6h.
Preferably, in the step (4), the ultraviolet irradiation treatment is performed for 30-90min.
In a first aspect, the invention provides an MXene-based flexible supercapacitor electrode material prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
(1) The invention selects the compound of the tetra-aniline and the MXene, and reduces the volume degradation which is easy to occur in the repeated charge and discharge process by utilizing the shorter chain length of the tetra-aniline;
(2) The invention adopts the composite of the tetraaniline and the MXene, increases the interlayer spacing of the MXene, promotes the transportation of electrolyte ions, increases the specific surface area and electrochemical active sites of the MXene, and improves the electrochemical energy storage performance;
(3) The invention utilizes the photochemical action of the organic azide to combine the tetra-aniline to the MXene nano-sheet, and the tetra-aniline and the MXene nano-sheet are combined in a covalent bond mode, so that the risk of falling off of the tetra-aniline is reduced, the synergy is ensured, and the cycle stability during energy storage is increased.
Detailed Description
The invention is further described below with reference to examples.
The following examples will enable those skilled in the art to more fully understand the present invention and are not intended to limit the same in any way.
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Stirring LiF and hydrochloric acid vigorously for 30-40min to obtain a mixed solution; then Ti is added in 10-20min 3 AlC 2 Slowly adding the precursor into the mixed solution, and continuously stirring at 40-45 ℃ for reaction for 36-48h; after the reaction is finished, centrifuging, pickling and washing to be neutral, performing ultrasonic treatment in ice bath for 90-120min, and finally centrifuging and collecting supernatant to obtain MXene single-layer suspension;
(2) Preparing N-phenyl-1, 4-phenylenediamine, ferric trichloride hexahydrate and hydrochloric acid into a reaction solution, reacting for 2-3 hours at 20-30 ℃, and separating and purifying the product to obtain the tetra-aniline;
(3) Dissolving 5-azido valeric acid, dicyclohexylcarbodiimide, trimethylamine, 4-dimethylaminopyridine and tetraaniline in a reaction solvent, stirring and reacting for 36-48h at 20-30 ℃, and separating out a reaction product to obtain modified tetraaniline containing azido groups;
(4) Dissolving modified tetraaniline containing an azide group in a solvent, dropwise adding an MXene single-layer suspension, wherein the mass ratio of the MXene to the modified tetraaniline containing the azide group is 1-9:1, stirring for 3-6h at 20-30 ℃, performing ultraviolet irradiation treatment for 30-90min, centrifuging, washing with ethanol, washing with water, and adding water to obtain an electrode material suspension;
(5) And carrying out suction filtration on the electrode material suspension, and then drying the obtained film to obtain the MXene-based flexible supercapacitor electrode material.
Example 1
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M hydrochloric acid were vigorously stirred in a polytetrafluoroethylene liner (volume 100 mL) for 30min, to obtain a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added into the mixed solution to avoid violent reactionAnd the risk of exotherm. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. Then centrifuging the reaction solution at 3500rpm for 5 times, washing with 1M HCl, washing with distilled water until the pH value of the supernatant is neutral, performing ultrasonic treatment in ice bath environment for 120min, centrifuging at 3500rpm for 20min, and collecting black supernatant to obtain MXene monolayer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) Preparation of tetra-aniline: 2.83g N-phenyl-1, 4-phenylenediamine powder was added to a 250 ml round bottom flask with 75ml of 1.0m hydrochloric acid and stirred rapidly for 30 minutes. 4.14g of ferric trichloride hexahydrate was dissolved in 75mL of 1.0M hydrochloric acid and quickly poured into a round bottom flask, followed by 75mL of 1.0M hydrochloric acid and stirred at room temperature of 25℃for 2h. The precipitate was then centrifuged at 9000rpm for 30min and washed 4 times with 0.1M hydrochloric acid. The precipitate was then mixed with 75mL of 2.0M ammonium hydroxide and 450mL of acetone for 30min to give a bright blue solution. Acetone was removed using a rotary evaporator. The dispersion was then centrifuged and washed 4 times with deionized water and the supernatant brought to neutral pH. The powder was collected, rinsed with ethanol and air dried for 12h at night to give the blue solid, tetra-aniline.
(3) Preparation of modified tetraaniline containing azide groups: 0.8238 g of 5-azidopentanoic acid, 0.786g of dicyclohexylcarbodiimide, 0.390g of trimethylamine, 0.433 g of 4-dimethylaminopyridine and 1.665g of tetraaniline were dissolved in 15mL of Dichloromethane (DCM) and stirred at room temperature for 48h. The reaction mixture was then washed with deionized water. And then carrying out vacuum drying to obtain the modified tetraaniline containing the azide group.
(4) The modified tetra-aniline containing the azide group is dissolved in ethanol to prepare a modified tetra-aniline ethanol solution with the concentration of 200 mug/mL. 9mL of the MXene monolayer suspension (3 mg/mL) was added dropwise to 15mL of the modified tetraaniline ethanol solution (200. Mu.g/mL), and the mixture was vigorously stirred at room temperature at 25℃for 3 hours. Exposing the solution to ultraviolet light for 30min, centrifuging the liquid, washing the liquid with ethanol for 6 times to remove unreacted modified tetraaniline containing azide groups, repeatedly washing the liquid with deionized water for 8 times, and adding deionized water to obtain an electrode material suspension.
(5) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. The mass capacitance was calculated as 357.7F/g by the area of the CV curve. The GCD curve shows nearly triangle symmetry, which shows that the GCD curve has good charge and discharge performance. The capacitance retention after 10000 GCD tests was 91.9%.
Example 2
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M hydrochloric acid were vigorously stirred in a polytetrafluoroethylene liner (volume 100 mL) for 30min, to obtain a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added to the mixture to avoid the risk of exothermic violent reactions. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. Then centrifuging the reaction solution at 3500rpm for 5 times, washing with 1M HCl, washing with distilled water until the pH value of the supernatant is neutral, performing ultrasonic treatment in ice bath environment for 120min, centrifuging at 3500rpm for 20min, and collecting black supernatant to obtain MXene monolayer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) Preparation of tetra-aniline: 2.83g N-phenyl-1, 4-phenylenediamine powder was added to a 250 ml round bottom flask with 75ml of 1.0m hydrochloric acid and stirred rapidly for 30 minutes. 4.14g of ferric trichloride hexahydrate was dissolved in 75mL of 1.0M hydrochloric acid and quickly poured into a round bottom flask, followed by 75mL of 1.0M hydrochloric acid and stirred at room temperature of 25℃for 2h. The precipitate was then centrifuged at 9000rpm for 30min and washed 4 times with 0.1M hydrochloric acid. The precipitate was then mixed with 75mL of 2.0M ammonium hydroxide and 450mL of acetone for 30min to give a bright blue solution. Acetone was removed using a rotary evaporator. The dispersion was then centrifuged and washed 4 times with deionized water and the supernatant brought to neutral pH. The powder was collected, rinsed with ethanol and air dried for 12h at night to give the blue solid, tetra-aniline.
(3) Preparation of modified tetraaniline containing azide groups: 0.8238 g of 5-azidopentanoic acid, 0.786g of dicyclohexylcarbodiimide, 0.390g of trimethylamine, 0.431g of 4-dimethylaminopyridine and 1.665g of tetraaniline were dissolved in 15mL of DCM and stirred at room temperature for 48h. The reaction mixture was then washed with deionized water. And then carrying out vacuum drying to obtain the modified tetraaniline containing the azide group.
(4) The modified tetra-aniline containing the azide group is dissolved in ethanol to prepare a modified tetra-aniline ethanol solution with the concentration of 200 mug/mL. 8mL of the Mxene monolayer suspension (3 mg/mL) was added dropwise to 30mL of the modified tetraaniline ethanol solution (200. Mu.g/mL) and stirred vigorously at room temperature for 4h at 25 ℃. Exposing the solution to ultraviolet light for 40min, centrifuging the liquid, washing the liquid with ethanol for 6 times to remove unreacted modified tetraaniline containing azide groups, repeatedly washing the liquid with deionized water for 8 times, and adding deionized water to obtain an electrode material suspension.
(5) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. Mass capacitance was calculated to be 336.7F/g by area of CV curve. The GCD curve shows nearly triangle symmetry, which shows that the GCD curve has good charge and discharge performance. The capacitance retention after 10000 GCD tests was 87.8%.
Example 3
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M saltThe acid was vigorously stirred in a polytetrafluoroethylene liner (volume 100 ml) for 30min to give a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added to the mixture to avoid the risk of exothermic violent reactions. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. Then centrifuging the reaction solution at 3500rpm for 5 times, washing with 1M HCl, washing with distilled water until the pH value of the supernatant is neutral, performing ultrasonic treatment in ice bath environment for 120min, centrifuging at 3500rpm for 20min, and collecting black supernatant to obtain MXene monolayer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) Preparation of tetra-aniline: 2.83g N-phenyl-1, 4-phenylenediamine powder was added to a 250 ml round bottom flask with 75ml of 1.0m hydrochloric acid and stirred rapidly for 30 minutes. 4.14g of ferric trichloride hexahydrate was dissolved in 75mL of 1.0M hydrochloric acid and quickly poured into a round bottom flask, followed by 75mL of 1.0M hydrochloric acid and stirred at room temperature of 25℃for 2h. The precipitate was then centrifuged at 9000rpm for 30min and washed 4 times with 0.1M hydrochloric acid. The precipitate was then mixed with 75mL of 2.0M ammonium hydroxide and 450mL of acetone for 30min to give a bright blue solution. Acetone was removed using a rotary evaporator. The dispersion was then centrifuged and washed 4 times with deionized water and the supernatant brought to neutral pH. The powder was collected, rinsed with ethanol and air dried for 12h at night to give the blue solid, tetra-aniline.
(3) Preparation of modified tetraaniline containing azide groups: 0.8238 g of 5-azidopentanoic acid, 0.786g of dicyclohexylcarbodiimide, 0.390g of trimethylamine, 0.431g of 4-dimethylaminopyridine and 1.665g of tetraaniline were dissolved in 15mL of DCM and stirred at room temperature for 48h. The reaction mixture was then washed with deionized water. And then carrying out vacuum drying to obtain the modified tetraaniline containing the azide group.
(4) The modified tetra-aniline containing the azide group is dissolved in ethanol to prepare a modified tetra-aniline ethanol solution with the concentration of 200 mug/mL. 7mL of the MXene monolayer suspension (3 mg/mL) was added dropwise to 45mL of the modified tetraaniline ethanol solution (200. Mu.g/mL), and the mixture was vigorously stirred at room temperature for 5 hours at 25 ℃. The solution was exposed to uv light for 60min, and then the liquid was centrifuged and washed with ethanol for 6 times to remove unreacted azide group-containing modified tetraaniline, and then repeatedly washed with deionized water for 8 times, and deionized water was added to obtain an electrode material suspension.
(5) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. The mass capacitance was calculated as 297.4F/g by the area of the CV curve. The GCD curve shows nearly triangle symmetry, which shows that the GCD curve has good charge and discharge performance. The capacitance retention after 10000 GCD tests was 80.6%.
Comparative example 1
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M hydrochloric acid were vigorously stirred in a polytetrafluoroethylene liner (volume 100 mL) for 30min, to obtain a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added to the mixture to avoid the risk of exothermic violent reactions. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. Then centrifuging the reaction solution at 3500rpm for 5 times, washing with 1M HCl, washing with distilled water until the pH value of the supernatant is neutral, performing ultrasonic treatment in ice bath environment for 120min, centrifuging at 3500rpm for 20min, and collecting black supernatant to obtain MXene monolayer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) Polyaniline is dissolved in N-methyl pyrrolidone to prepare polyaniline solution with the concentration of 200 mug/mL. 9mL of the MXene monolayer suspension (3 mg/mL) was added dropwise to 15mL of polyaniline solution (200. Mu.g/mL), and the mixture was vigorously stirred at room temperature for 3 hours at 25 ℃. And then centrifuging the liquid, washing the liquid with N-methyl pyrrolidone for 6 times, repeatedly washing the liquid with deionized water for 8 times, and adding the deionized water to obtain an electrode material suspension.
(3) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. The mass capacitance was calculated as 209.6F/g by the area of the CV curve. The capacitance retention after 10000 GCD tests was 71.2%.
Comparative example 2
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M hydrochloric acid were vigorously stirred in a polytetrafluoroethylene liner (volume 100 mL) for 30min, to obtain a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added to the mixture to avoid the risk of exothermic violent reactions. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. Then centrifuging the reaction solution at 3500rpm for 5 times, washing with 1M HCl, washing with distilled water until the pH value of the supernatant is neutral, performing ultrasonic treatment in ice bath environment for 120min, centrifuging at 3500rpm for 20min, and collecting black supernatant to obtain MXene monolayer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) Preparation of tetra-aniline: 2.83g N-phenyl-1, 4-phenylenediamine powder was added to a 250 ml round bottom flask with 75ml of 1.0m hydrochloric acid and stirred rapidly for 30 minutes. 4.14g of ferric trichloride hexahydrate was dissolved in 75mL of 1.0M hydrochloric acid and quickly poured into a round bottom flask, followed by 75mL of 1.0M hydrochloric acid and stirred at room temperature of 25℃for 2h. The precipitate was then centrifuged at 9000rpm for 30min and washed 4 times with 0.1M hydrochloric acid. The precipitate was then mixed with 75mL of 2.0M ammonium hydroxide and 450mL of acetone for 30min to give a bright blue solution. Acetone was removed using a rotary evaporator. The dispersion was then centrifuged and washed 4 times with deionized water and the supernatant brought to neutral pH. The powder was collected, rinsed with ethanol and air dried for 12h at night to give the blue solid, tetra-aniline.
(3) The tetra-aniline is dissolved in ethanol to prepare a tetra-aniline ethanol solution with the concentration of 200 mu g/mL. 9mL of the MXene monolayer suspension (3 mg/mL) was added dropwise to 15mL of a tetraaniline ethanol solution (200. Mu.g/mL) and stirred vigorously at room temperature for 3h at 25 ℃. And centrifuging the liquid, washing the liquid with ethanol for 6 times, repeatedly washing the liquid with deionized water for 8 times, and adding the deionized water to obtain an electrode material suspension.
(4) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
When the tetra-aniline and the MXene are stirred and mixed, the functional groups of the tetra-aniline and the MXene are kept stable under the condition of only physical stirring, do not generate chemical reaction, cannot form covalent bonds, and have poor stability. Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. The mass capacitance was calculated as 215.3F/g by the area of the CV curve. The capacitance retention after 10000 GCD tests was 74.5%.
Comparative example 3
An MXene-based flexible supercapacitor electrode material is prepared by the following steps:
(1) Preparation of MXene monolayer suspension: 2.3g LiF and 40mL 9M hydrochloric acid were vigorously stirred in a polytetrafluoroethylene liner (volume 100 mL) for 30min, to obtain a mixture. Then 2g Ti is added within 10min 3 AlC 2 The precursor is slowly added to the mixture to avoid the risk of exothermic violent reactions. The polytetrafluoroethylene liner was then placed in a 40 ℃ water bath and stirred continuously for 48 hours. After that, the reaction solution was centrifuged 5 times at 3500rpm, washed with 1M HCl, and then washed with distilled water untilThe pH value of the supernatant is neutral, ultrasonic treatment is carried out for 120min under ice bath environment, finally centrifugation is carried out for 20min at 3500rpm, and black supernatant is collected, thus obtaining MXene single-layer suspension, namely Ti 3 C 2 T x The concentration of the Mxene monolayer suspension is 3.0mg/mL.
(2) 9mL of the MXene monolayer suspension (3 mg/mL) was added dropwise to 15mL of ethanol solution and stirred vigorously at room temperature for 3h at 25 ℃. And centrifuging the liquid, washing the liquid with ethanol for 6 times, repeatedly washing the liquid with deionized water for 8 times, and adding the deionized water to obtain an electrode material suspension.
(3) And carrying out vacuum suction filtration on the electrode material suspension through a sand core funnel, and carrying out vacuum drying on the suction-filtered film at 60 ℃ for 3 hours to obtain the MXene-based flexible supercapacitor electrode material.
Cutting the prepared MXene-based flexible supercapacitor electrode material into 1X 1cm as a working electrode, silver/silver chloride as a reference electrode, and a platinum sheet electrode as a counter electrode, wherein 1M H is selected 2 SO 4 As an electrolyte solution. CV, GCD and cycle testing were performed by an electrochemical workstation. The mass capacitance was calculated to be 187.2F/g by the area of the CV curve. The capacitance retention after 10000 GCD tests was 63.8%.
The electrochemical properties of the electrode materials measured in examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1.
TABLE 1
| Mass capacitance (F/g) | Capacitance retention (%) | |
| Example 1 | 357.7 | 91.9 |
| Example 2 | 336.7 | 87.8 |
| Example 3 | 294.7 | 80.6 |
| Comparative example 1 | 215.3 | 74.5 |
| Comparative example 2 | 209.6 | 71.2 |
| Comparative example 3 | 187.2 | 63.8 |
As can be seen from table 1:
(1) The significantly higher mass capacitance and capacitance retention of examples 1-3 and comparative examples 1-2 compared to comparative example 3, demonstrates that the addition of polyaniline or an aniline oligomer significantly improves the energy storage properties of the MXene-based electrode material.
(2) Compared with comparative example 1, the mass capacitance and the capacitance retention rate of comparative example 2 are obviously higher, which indicates that the addition of the aniline oligomer tetra-aniline has superior energy storage effect compared with polyaniline. The reason is that polyaniline has higher rigidity than that of tetra-aniline, has poor dispersion, can not be well mixed with MXene uniformly, and affects electrochemical performance; while the molecular chain length of the polyaniline is shorter on the premise of having the advantages of the conductivity of the polyaniline and the like, the interlayer spacing of the MXene is easy to adjust, the dispersibility in water is better, and the energy storage effect of the composite material is well improved.
(3) The significantly higher mass capacitance and capacitance retention of examples 1-3 compared to comparative example 2 demonstrates that the photochemical action of the organic azide compound is used to bind the tetraphenylamine to the MXene nanoplatelets, enabling the MXene-based electrode materials to have better energy storage properties. The functional groups of the tetraaniline and the MXene are stable under the condition of only physical stirring, do not generate chemical reaction, cannot form covalent bonds and can only form hydrogen bonds, while the modified tetraaniline containing the azide groups is decomposed into nitrogen and nitrene under the irradiation of ultraviolet light, the nitrene is very active, can be combined with H on the MXene to form stable covalent bonds, can better promote charge transfer between MXene layers and increase more electrochemical active sites, and greatly promotes the electrochemical energy storage performance of the MXene-based electrode material.
(4) Compared with examples 2-3, the mass capacitance and the capacitance retention rate of example 1 are obviously higher, which indicates that the excessive addition of the modified tetraaniline containing azide groups is unfavorable for the electrochemical energy storage performance of the MXene-based electrode material. This is because excessive addition increases interlayer spacing, reduces charge transfer, and excessive phenylenediamine between layers reduces electrochemically active sites, affecting electrochemical energy storage properties.
Finally, it should be noted that the above list is only specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (7)
1. The preparation method of the MXene-based flexible supercapacitor electrode material is characterized by comprising the following steps of:
(1) The preparation method of the MXene monolayer suspension specifically comprises the following steps: stirring LiF and hydrochloric acid vigorously for 30-40min to obtain a mixed solution; then Ti is added in 10-20min 3 AlC 2 Slowly adding the precursor into the mixed solution, and continuing stirring for reaction; after the reaction is completed, centrifugal separation, acid washing and water washing are carried out untilPerforming neutral, performing ultrasonic treatment, and finally centrifuging to collect supernatant to obtain MXene single-layer suspension;
(2) Synthesizing tetraaniline by taking N-phenyl-1, 4-phenylenediamine as a monomer;
(3) Dissolving 5-azido valeric acid, dicyclohexylcarbodiimide, trimethylamine, 4-dimethylaminopyridine and tetraaniline in a reaction solvent, and separating out a reaction product after stirring reaction to obtain modified tetraaniline containing azido groups;
(4) Dissolving modified tetraaniline containing an azide group in a solvent, dropwise adding an MXene single-layer suspension into the solvent, stirring the mixture, performing ultraviolet irradiation treatment, centrifuging, washing with ethanol, washing with water, and adding water to obtain an electrode material suspension;
(5) Carrying out suction filtration on the electrode material suspension, and then drying the obtained film to obtain an MXene-based flexible supercapacitor electrode material;
in the step (4), the mass ratio of the MXene to the modified tetraaniline containing the azide group is 4-9:1, and the ultraviolet irradiation treatment time is 30-40min.
2. The process according to claim 1, wherein in step (1), the temperature of the stirring reaction is 40 to 45 ℃ for 36 to 48 hours.
3. The method of claim 1, wherein in step (1), the ultrasonic treatment is performed in an ice bath for 90 to 120 minutes.
4. The preparation method according to claim 1, wherein the step (2) specifically comprises the steps of: preparing N-phenyl-1, 4-phenylenediamine, ferric trichloride hexahydrate and hydrochloric acid into a reaction solution, reacting for 2-3 hours at 20-30 ℃, and separating and purifying the product to obtain the tetra-aniline.
5. The process according to claim 1, wherein in step (3), the temperature of the stirring reaction is 20 to 30℃for 36 to 48 hours.
6. The method according to claim 1, wherein in the step (4), the stirring is performed at a temperature of 20 to 30 ℃ for a time of 3 to 6 hours.
7. An MXene-based flexible supercapacitor electrode material made by the method of any one of claims 1-6.
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