CN110895998A - Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink - Google Patents
Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 98
- 239000003990 capacitor Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 41
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 238000007639 printing Methods 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 58
- 229910021389 graphene Inorganic materials 0.000 claims description 40
- 238000000137 annealing Methods 0.000 claims description 25
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 16
- 239000002041 carbon nanotube Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000011065 in-situ storage Methods 0.000 claims description 13
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
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- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 6
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- WEEGYLXZBRQIMU-UHFFFAOYSA-N 1,8-cineole Natural products C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 claims description 5
- WEEGYLXZBRQIMU-WAAGHKOSSA-N Eucalyptol Chemical compound C1C[C@H]2CC[C@]1(C)OC2(C)C WEEGYLXZBRQIMU-WAAGHKOSSA-N 0.000 claims description 5
- 229960005233 cineole Drugs 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
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- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
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- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims description 3
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- 229920001220 nitrocellulos Polymers 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 2
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Images
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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- 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
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses an electrode material ink, a preparation method and a method for preparing a micro super capacitor by using the electrode material ink, and belongs to the technical field of micro super capacitors. A preparation method of electrode material ink comprises the following steps: 1) adding a dispersing agent and an electrode material into an alcohol solution, and performing ultrasonic treatment to prepare a primary ultrasonic dispersion solution; 2) adding a target solvent into the primary ultrasonic dispersion liquid of the electrode material, and performing secondary ultrasonic treatment to prepare a secondary ultrasonic dispersion liquid; 3) and removing the alcohol solution in the secondary ultrasonic dispersion liquid to obtain the electrode material ink. By utilizing the preparation method, the ink with different viscosities and different liquidities can be prepared by adjusting the amounts of the electrode material and the solvent, the capacitors with different shapes and different sizes can be printed, and the preparation method does not contain toxic solvent and is suitable for large-scale production. The electrode material ink provided by the invention has the advantages that the electrode material is uniformly dispersed, the film forming property is good, and the printing can be carried out on different substrates.
Description
Technical Field
The invention belongs to the technical field of miniature super capacitors, and particularly relates to an electrode material ink, a preparation method and a method for preparing a miniature super capacitor by using the electrode material ink.
Background
As the demand for miniaturized portable electronic products increases, miniature energy storage devices are undergoing rapid development, and miniature supercapacitors play an irreplaceable role in energy storage of small electronic products due to their advantages, such as high power density and long cycle life. The micro super capacitor can be classified into a pseudo capacitor and a double electric layer capacitor according to different energy storage mechanisms, wherein electrode materials of the pseudo capacitor mainly comprise transition metal oxides, hydroxides, sulfides, conductive polymers and the like; the electrode material of the electric double layer capacitor mainly includes carbon-based materials including graphene, carbon nanotubes, carbon nanofibers, activated carbon, and the like. The micro super capacitor has a smaller energy storage capacity than the energy storage devices such as the micro lithium ion battery. The energy storage performance of the micro super capacitor is improved mainly by improving the aspects of selection of electrode materials, design of electrode material structures, shape design of the capacitor, selection of electrolyte and the like.
At present, the preparation method of the micro super capacitor mainly comprises laser engraving, screen printing, electrochemical deposition, ink-jet printing and the like, the laser engraving method is complex in process, electrodes are difficult to form large depth-width ratio, the electrodes are difficult to form large depth-width ratio when the super capacitor is prepared by the screen printing method, the electrochemical deposition method is difficult to carry out batch preparation and is not suitable for industrial production, and 3D printing is widely concerned due to the fact that the preparation cost is low, the preparation period is short, the super capacitor is suitable for large-scale production, and devices of various sizes and shapes can be printed.
The existing printing technology for preparing the miniature super capacitor mainly has the following problems: (1) the preparation of the electrode material ink is complex, for example, the preparation process of the electrode material ink disclosed in the invention patent CN104505265A needs long time, and the preparation steps are complicated; (2) the process of preparing the micro supercapacitor is complex, for example, in the invention patent CN103762093A, the process of preparing the micro supercapacitor needs to be repeatedly cured and packaged; (3) the requirements on the substrate material are strict, as in patent CN108538864A, the substrate of the printed micro-supercapacitor can only be a flexible substrate. For a micro-supercapacitor, the complexity of electrode material preparation and device assembly will seriously degrade the performance of the micro-supercapacitor, hindering its application.
Disclosure of Invention
The invention aims to overcome the defects that the existing electrode material ink is not uniformly dispersed and the prepared miniature super capacitor contains non-electrode material components, and provides the electrode material ink, a preparation method and a method for preparing the miniature super capacitor by using the electrode material ink.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of electrode material ink comprises the following steps:
1) adding a dispersing agent and an electrode material into an alcohol solution, and performing ultrasonic treatment to prepare a primary ultrasonic dispersion solution;
wherein the alcohol solution is one or more of methanol, ethanol, isopropanol and pentanol;
the dispersant is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, ethyl cellulose, cellulose acetate, cellulose nitrate or cellulose powder;
the electrode material is one or more of graphene, doped graphene, carbon nano tubes, doped carbon nano tubes, conductive carbon black and carbon nano fibers;
2) adding a target solvent into the primary ultrasonic dispersion liquid of the electrode material, and performing secondary ultrasonic treatment to prepare a secondary ultrasonic dispersion liquid;
the target solvent is one or more of ethylene glycol, terpineol, terpene-4-alcohol, eucalyptol, linalool and isopropanol;
wherein, in the secondary ultrasonic dispersion liquid, 1mL of target solvent is added into every 50-100mg of electrode material;
3) and removing the alcohol solution in the secondary ultrasonic dispersion liquid to obtain the electrode material ink.
Further, the alcohol liquid is removed by a rotary evaporation method in the step 3).
Further, the graphene in the step 1) is single-layer graphene and/or multi-layer graphene;
the doped graphene is hetero-atom doped graphene and/or graphene of in-situ grown transition metal oxide;
the doped carbon nanotube is a carbon nanotube in which a transition metal oxide is grown in situ.
Further, the hetero-atom doped graphene is nitrogen, sulfur, boron or fluorine doped graphene.
Further, the transition metal oxide in the graphene in which the transition metal oxide grows in situ is manganese dioxide, ferric oxide or nickel oxide;
the transition metal oxide in the carbon nano tube of the in-situ grown transition metal oxide is manganese dioxide, ferric oxide or nickel oxide.
Further, the mass ratio of the electrode material to the dispersant in the step 2) is (0.1-10): 2.
an electrode material ink prepared according to the preparation method.
A preparation method of a miniature super capacitor comprises the following specific operations:
printing the electrode material ink on a substrate by 3D printing, annealing to obtain an electrode material, and adding electrolyte to obtain a micro supercapacitor;
the annealing conditions are as follows: the temperature is 100-600 ℃, the time is 0.5-6h, and the atmosphere is air, nitrogen or argon.
Further, the substrate is a polyimide sheet, a nylon sheet, a polydimethylsiloxane sheet, a glass sheet or a silicon sheet.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the electrode material ink, the dispersing agent is firstly dissolved in the alcohol solution, the electrode material is added for dispersing by means of ultrasonic treatment, then the target solvent is added for secondary ultrasonic treatment, finally the alcohol solution is removed, the alcohol solution is used as the transition solvent, so that the electrode material is more uniformly dispersed, the addition of the dispersing agent is also beneficial to the film forming property of the ink, and the target solvent can increase the viscosity of the ink, so that the ink is more stable; after the alcohol solution is removed, the solvent in the electrode ink material is only the target solvent, so that the viscosity of the ink and the stability of the ink are increased; according to the preparation method, the ink with different viscosities and different liquidities can be prepared by adjusting the amounts of the electrode material and the solvent, the capacitors with different shapes and different sizes can be printed, and the preparation method does not contain toxic solvents and is suitable for large-scale production.
Further, the mass ratio of the electrode material to the dispersant is (0.1-10): 2, the mass ratio of the electrode material to the dispersing agent in the range can enable the electrode material to have excellent electrochemical performance, and if the mass ratio of the electrode material to the dispersing agent is too large, the electrode material is easily distributed unevenly; if the mass ratio of the electrode material to the dispersant is too small, the conductivity of the electrode tends to be low, and the electrochemical performance of the device tends to be low.
The electrode material ink provided by the invention has the advantages that the electrode material is uniformly dispersed, the film forming property is good, and the electrode material ink can be used for printing on different substrates.
According to the preparation method of the micro super capacitor, the electrodes in the preset shapes are obtained through 3D printing, the micro super capacitor obtained through annealing treatment only contains the electrode materials, the uniformly dispersed electrode materials are beneficial to transmission of electrolyte ions, the effective specific surface area of the electrode materials is increased, and the electrochemical performance of the micro capacitor is improved.
Drawings
FIG. 1 is a photograph of an electrode material ink prepared in example 1 of the present invention;
FIG. 2 is a photograph of a drawdown film on a glass substrate according to example 1 of the present invention;
FIG. 3 is a photograph of a drawdown film on an aluminum foil substrate according to example 1 of the present invention;
FIG. 4 is a photograph of a drawdown film on a polyimide substrate of example 1 of the present invention;
FIG. 5 is a scanning electron micrograph of a miniature supercapacitor electrode according to example 1 of the present invention;
FIG. 6 is a cyclic voltammogram of a miniature supercapacitor in example 2 of the present invention at different scan rates;
FIG. 7 is a constant current charging and discharging curve of the micro supercapacitor in example 2 of the present invention at different current densities;
FIG. 8 is a graph showing the relationship between the capacitance and the current density of the micro supercapacitor in example 2 of the present invention;
FIG. 9 is a scanning electron micrograph of a miniature supercapacitor electrode according to example 3 of the present invention;
FIG. 10 is a plot of cyclic voltammetry at different scan rates for a miniature supercapacitor in example 3 of the present invention;
FIG. 11 is a scanning electron micrograph of a miniature supercapacitor electrode according to example 4 of the present invention;
FIG. 12 is a plot of cyclic voltammetry at different scan rates for a miniature supercapacitor in example 5 of the present invention;
FIG. 13 is a constant current charging and discharging curve of the micro supercapacitor in example 5 of the present invention at different current densities;
FIG. 14 is a schematic flow chart of the present invention for printing a micro supercapacitor.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the invention provides an electrode material ink, a preparation method and a method for preparing a micro super capacitor by using the electrode material ink, which comprise the following specific embodiments:
example 1
Adding 10g of hydroxyethyl cellulose into 500mL of ethanol for dissolving, stirring and dissolving at room temperature to obtain ethanol solution, weighing 10g of reduced graphene oxide, adding into the ethanol solution, stirring at the room temperature at the rotating speed of 500rpm to obtain primary dispersion liquid, performing primary dispersion on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 60 minutes, adding 100mL of linalool, performing secondary ultrasonic, and performing ultrasonic treatment at the same ultrasonic power for 100 minutes;
removing ethanol from the dispersion liquid by using a rotary evaporator to obtain electrode material ink;
the prepared ink is coated on different substrates in a blade mode to obtain different films, and the coated films are dried and annealed to obtain films only containing graphene;
the ink prepared in example 1 is shown in fig. 1, which shows that large scale preparation is possible with this method, and fig. 2, fig. 3 and fig. 4 are films of the prepared ink drawn down on different substrates, which show good film formation on different substrates.
Printing electrode material ink on a polyimide substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and annealing to obtain an electrode only containing an active material.
Wherein the annealing process is to heat the dried micro super capacitor to 300 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and the annealing time is 2 h.
The scanning electron microscope picture of the electrode of the micro supercapacitor prepared in example 1 is shown in fig. 5, and it can be seen from the picture that the electrode only contains graphene and no other materials, which proves that after annealing treatment, the electrode is relatively pure and only contains active materials.
Example 2
Adding 150mg of hydroxymethyl cellulose into 30mL of methanol for dissolving, stirring and dissolving at room temperature to obtain methanol solution, weighing 7.5mg of nitrogen atom-doped reduced graphene oxide, adding the solution into the solution, stirring at the rotating speed of 500rpm at room temperature to obtain primary dispersion liquid, performing primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 20 minutes, adding 0.1mL of terpineol, performing secondary ultrasonic treatment, and performing ultrasonic treatment for 40 minutes under the same ultrasonic power.
And removing the methanol from the dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a polyimide substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and carrying out annealing treatment to ensure that the electrode material only contains an active material.
Wherein the annealing process is to heat the dried micro super capacitor to 400 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and the annealing time is 4 h.
The cyclic voltammetry curves of the device prepared in example 2 at different scan rates are shown in fig. 6, and it can be seen that the curve shape is not deformed and remains unchanged even at large scan ratesThe material is similar to rectangle, which shows that the prepared device has the capability of rapid charge and discharge. Fig. 7 is a constant current charge and discharge curve under different current densities, and the curve shows good linear relation and symmetry, which proves that the device has good reversibility and rapid charge and discharge characteristics. The relationship between the capacitance and the current density is shown in FIG. 8. it can be seen from FIG. 8 that the capacitance of the capacitor can reach 7.23mF/cm at low current density2Even under high current density, the capacitance of the micro-super capacitor can still reach 6.91mF/cm2The result shows that the prepared micro super capacitor has good rate performance.
Example 3
Adding 135mg of hydroxyethyl cellulose into 30mL of ethanol for dissolving, stirring and dissolving at room temperature to obtain ethanol solution, weighing 270mg of reduced graphene oxide, adding into the ethanol solution, stirring at the rotating speed of 500rpm at room temperature to obtain primary dispersion liquid, performing primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 10 minutes, adding 5mL of terpineol, performing secondary ultrasonic treatment, and performing ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain dispersed solution 1.
Adding 15mg of hydroxyethyl cellulose into 30mL of ethanol for dissolving, dissolving and stirring at room temperature to obtain ethanol solution, weighing 15mg of carbon nano tubes, adding the carbon nano tubes into the ethanol solution, stirring at 500rpm at room temperature to obtain primary dispersion liquid, carrying out primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 10 minutes, adding 0.3mL of terpineol, carrying out secondary ultrasonic treatment, and carrying out ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain dispersed solution 2.
Mixing the solution 1 and the solution 2 together, and carrying out ultrasonic treatment by using an ultrasonic disperser, wherein the ultrasonic power is 150W, and the ultrasonic time is 60 minutes.
And removing the ethanol from the dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a polyimide substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and carrying out annealing treatment to ensure that the electrode material only contains an active material.
Wherein the annealing process is to heat the dried micro super capacitor to 100 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and the annealing time is 6 h.
The scanning electron picture of the electrode of the micro supercapacitor prepared in example 3 is shown in fig. 9, and it can be seen from the picture that the electrode only contains graphene and carbon nanotubes, hydroxyethyl cellulose is completely removed after annealing treatment, and the carbon nanotubes are uniformly distributed without aggregation. The cyclic voltammograms at different scanning rates are shown in fig. 10, and it can be seen from the graph that even at a large scanning rate, a good rectangular shape can be maintained, which indicates that the prepared micro-supercapacitor has a good rapid charging and discharging capability.
Example 4
Adding 75mg of hydroxyethyl cellulose into 30mL of ethanol for dissolving, stirring and dissolving at room temperature to obtain ethanol solution, weighing 375mg of electrode material of manganese dioxide in-situ grown on graphene, adding the electrode material into the ethanol solution, stirring at 500rpm at room temperature to obtain primary dispersion liquid, performing primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 10 minutes, adding 3.75mL of terpineol, performing secondary ultrasonic treatment, and performing ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain dispersed solution 1.
Adding 75mg of hydroxyethyl cellulose into 30mL of ethanol for dissolving, stirring and dissolving at room temperature to obtain ethanol solution, weighing electrode materials on 75mg of redox graphene, adding the electrode materials into the ethanol solution, stirring at 500rpm at room temperature to obtain primary dispersion liquid, performing primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic time is 10 minutes, adding 1mL of eucalyptol, performing secondary ultrasonic treatment, and performing ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain dispersed solution 2.
Mixing the solution 1 and the solution 2 together, and carrying out ultrasonic treatment by using an ultrasonic disperser, wherein the ultrasonic power is 150W, and the ultrasonic time is 60 minutes.
And removing the ethanol from the dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a polyimide substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and carrying out annealing treatment to ensure that the electrode material only contains an active material.
The specific process of annealing is to heat the dried micro super capacitor to 600 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and the annealing time is 0.5 h.
The scanning electron picture of the electrode of the micro supercapacitor prepared in example 4 is shown in fig. 11, and it can be seen from the picture that graphene and redox graphene grown in situ by manganese dioxide are uniformly distributed and do not agglomerate.
Example 5
Adding 135mg of hydroxyethyl cellulose into 30mL of amyl alcohol for dissolving, stirring and dissolving at room temperature to obtain an isopropanol liquid, weighing 135mg of reduced graphene oxide, adding into the isopropanol liquid, stirring at 500rpm at room temperature to obtain a primary dispersion liquid, performing primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic treatment time is 10 minutes, adding 1.35mL of eucalyptol, performing secondary ultrasonic treatment, and performing ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain a dispersed solution 1.
Adding 15mg of hydroxyethyl cellulose into 30mL of amyl alcohol for dissolving, dissolving and stirring at room temperature to obtain an isopropanol liquid, weighing 45mg of conductive carbon black, adding the conductive carbon black into the solution, stirring at 500rpm at room temperature to obtain a primary dispersion liquid, carrying out primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 150W, the ultrasonic treatment time is 10 minutes, adding 0.5mL of eucalyptol, carrying out secondary ultrasonic treatment, and carrying out ultrasonic treatment for 20 minutes under the same ultrasonic power to obtain a dispersed solution 2.
Mixing the solution 1 and the solution 2 together, and carrying out ultrasonic treatment by using an ultrasonic disperser, wherein the ultrasonic power is 150W, and the ultrasonic time is 60 minutes.
And removing the amyl alcohol from the dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a polyimide substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and carrying out annealing treatment to ensure that the electrode material only contains an active material.
Wherein the annealing process is that the dried micro super capacitor is heated to 300 ℃ in the air atmosphere at the heating rate of 2 ℃/min, and the annealing time is 1 h.
The cyclic voltammetry curves at different scanning rates of the micro supercapacitor prepared in example 5 are shown in fig. 12, and it can be seen from the graph that the shape is rectangular, and even at a large scanning rate, the good rectangular shape can be still maintained, which shows that the prepared micro supercapacitor has good rapid charging and discharging capability. Fig. 13 is a constant current charge and discharge curve under different current densities, and the curve shows good linear relation and symmetry, which proves that the device has good reversibility and rapid charge and discharge characteristics.
Example 6
Adding 135mg of ethyl cellulose into a mixed solution of 15mL of amyl alcohol and 15mL of ethanol, dissolving, adding 35mg of reduced graphene oxide, 50mg of ferric oxide in-situ grown graphene and 50mg of nickel oxide in-situ grown carbon nano tube into an isopropanol solution, stirring at 600rpm at room temperature to obtain a primary dispersion solution, performing primary ultrasonic treatment on the primary dispersion solution by using an ultrasonic disperser, wherein the ultrasonic power is 150W, the ultrasonic time is 10 minutes to obtain a primary ultrasonic dispersion solution, adding 1.35mL of a mixed solution of eucalyptol-4-alcohol and ethylene glycol into the primary ultrasonic dispersion solution, performing secondary ultrasonic treatment, and performing ultrasonic treatment at the same ultrasonic power for 20 minutes to obtain a secondary ultrasonic dispersion solution;
and removing the amyl alcohol and the ethanol from the secondary ultrasonic dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a nylon film substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a vacuum environment, and annealing to ensure that the electrode material only contains active materials.
Example 7
Adding 35mg of cellulose acetate, 50mg of cellulose nitrate and 50mg of cellulose powder into a mixed solution of 15mL of amyl alcohol and 15mL of ethanol for dissolving, adding 35mg of sulfur-doped graphene, 35mg of boron-doped graphene, 35mg of fluorine-doped graphene and 30mg of nickel oxide in-situ grown graphene for dissolving, stirring at 400rpm at room temperature to obtain a primary dispersion liquid, and carrying out primary ultrasonic treatment on the primary dispersion liquid by using an ultrasonic dispersion instrument, wherein the ultrasonic power is 200W, and the ultrasonic treatment time is 8 minutes to obtain a primary ultrasonic dispersion liquid;
adding 2mL of mixed solution of cineole-4-ol and ethylene glycol into the primary ultrasonic dispersion liquid, and carrying out secondary ultrasonic treatment for 20 minutes under the same ultrasonic power;
and removing the amyl alcohol and the ethanol from the secondary ultrasonic dispersion liquid by using a rotary evaporator to obtain the electrode material ink.
Printing the electrode material ink on a nylon film substrate by using an ink-jet printing technology to form a miniature super capacitor, drying the printed miniature super capacitor in a nitrogen environment, and annealing to ensure that the electrode material only contains active materials.
Referring to fig. 14, fig. 14 is a schematic flow chart of printing a micro supercapacitor according to the present invention, in which the electrode material ink of the present invention is used as a raw material, an interdigital structure of the micro supercapacitor is printed on a substrate by using a printing technology, and an electrode material is obtained after annealing treatment, and then an electrolyte is added and an electrode is connected to prepare the micro supercapacitor.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. The preparation method of the electrode material ink is characterized by comprising the following steps of:
1) adding a dispersing agent and an electrode material into an alcohol solution, and performing ultrasonic treatment to prepare a primary ultrasonic dispersion solution;
wherein the alcohol solution is one or more of methanol, ethanol, isopropanol and pentanol;
the dispersant is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, ethyl cellulose, cellulose acetate, cellulose nitrate or cellulose powder;
the electrode material is one or more of graphene, doped graphene, carbon nano tubes, doped carbon nano tubes, conductive carbon black and carbon nano fibers;
2) adding a target solvent into the primary ultrasonic dispersion liquid of the electrode material, and performing secondary ultrasonic treatment to prepare a secondary ultrasonic dispersion liquid;
the target solvent is one or more of ethylene glycol, terpineol, terpene-4-alcohol, eucalyptol, linalool and isopropanol;
wherein, in the secondary ultrasonic dispersion liquid, 1mL of target solvent is added into every 50-100mg of electrode material;
3) and removing the alcohol solution in the secondary ultrasonic dispersion liquid to obtain the electrode material ink.
2. The method for preparing the electrode material ink according to claim 1, wherein the alcohol solution is removed in step 3) by rotary evaporation.
3. The method for preparing the electrode material ink according to claim 1, wherein the graphene in the step 1) is single-layer graphene and/or multi-layer graphene;
the doped graphene is hetero-atom doped graphene and/or graphene of in-situ grown transition metal oxide;
the doped carbon nanotube is a carbon nanotube in which a transition metal oxide is grown in situ.
4. The method for preparing the electrode material ink as claimed in claim 3, wherein the hetero-atom doped graphene is nitrogen-, sulfur-, boron-or fluorine-doped graphene.
5. The method for preparing the electrode material ink according to claim 3, wherein the transition metal oxide in the graphene in which the transition metal oxide is grown in situ is manganese dioxide, iron trioxide or nickel oxide;
the transition metal oxide in the carbon nano tube of the in-situ grown transition metal oxide is manganese dioxide, ferric oxide or nickel oxide.
6. The method for preparing the electrode material ink according to claim 1, wherein the mass ratio of the electrode material to the dispersant in the step 2) is (0.1 to 10): 2.
7. an electrode material ink prepared by the preparation method according to any one of claims 1 to 6.
8. A preparation method of a miniature super capacitor is characterized by comprising the following specific operations:
printing electrode material ink on a substrate by using 3D printing, annealing to obtain an electrode material, and adding electrolyte to obtain a micro supercapacitor;
the electrode material ink is the electrode material ink according to claim 7;
the annealing conditions are as follows: the temperature is 100-600 ℃, the time is 0.5-6h, and the atmosphere is air, nitrogen or argon.
9. The method of claim 8, wherein the substrate is a polyimide sheet, a nylon sheet, a polydimethylsiloxane sheet, a glass sheet, or a silicon sheet.
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