CN107026029A - A kind of graphene oxide doped Co anderson heteropoly acids prepare the method and its application of super capacitor material - Google Patents
A kind of graphene oxide doped Co anderson heteropoly acids prepare the method and its application of super capacitor material Download PDFInfo
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- CN107026029A CN107026029A CN201710332725.4A CN201710332725A CN107026029A CN 107026029 A CN107026029 A CN 107026029A CN 201710332725 A CN201710332725 A CN 201710332725A CN 107026029 A CN107026029 A CN 107026029A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 101
- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000002253 acid Substances 0.000 title claims abstract description 25
- 150000007513 acids Chemical class 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000002604 ultrasonography Methods 0.000 claims description 13
- 239000011964 heteropoly acid Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000005755 formation reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to super capacitor material field, the method that specifically a kind of graphene oxide doped Co anderson heteropoly acids prepare super capacitor material comprises the following steps：Co anderson heteropoly acids are taken to dissolve in the solution of graphene oxide, solution is stirred evenly using ultrasonic wave, mixed solution is put into pyroreaction kettle, reaction obtains graphene post, further take out graphene post, remove the ion dissociated in graphene, dry graphene, graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:1:1 ratio grinding, that is, be made super capacitor material；The present invention is compared with the existing technology, its easy control of reaction conditions, preparation process is relatively simple, obtained product quality stability is fine, be conducive to industrialized production, improve the chemical property of the grapheme material of ultracapacitor in itself and simplify its preparation technology, improve the chemical property of grapheme material.
Description
[technical field]
The present invention relates to super capacitor material field, specifically a kind of graphene oxide doped Co-anderson
Heteropoly acid prepares the method and its application of super capacitor material.
[background technology]
Ultracapacitor is also known as electrochemical capacitor, double layer capacitor, by realizing positive and negative charge point on interface
From carrying out energy storage.It is a kind of electrochemical element, and irreversible chemical reaction does not occur for its thermal energy storage process, therefore with outstanding
Cyclical stability；Its energy storage occur on interface, by diffusion limit smaller, therefore have higher energy density.From
Since the patent for the Section 1 ultracapacitor that nineteen fifty-seven declares, ultracapacitor is constantly weeded out the old and bring forth the new, at present not only technology day
Crescent is different, and application is also more and more extensive.
Graphene is found so far, in scientific research and industrial circle developing new direction.Graphene is most thin two-dimentional material
Material, with high intensity, great specific surface area and high conductance.It is super that graphene as these advantages possesses preparation
The ability of level capacitor, and capacitor performance can be greatly improved.At present, new material is paid attention in the research for improving capacitor performance
Material synthesis, and applied to the preparation of capacitor, energy storage and the energy density of ultracapacitor are improved with this.
Polyacid compound huge number, can be divided into heteropoly acid and the major class of isopolyacid two according to hetero atom is whether there is in its composition.
Heteropoly acid has various structure and composition, and wherein anderson types heteropoly acid has good redox ability.Therefore, if
Co-anderson heteropoly acids can be introduced during redox graphene, the ability by means of its charge and discharge electronics improves super electricity
Container energy storage, raising charge/discharge rates and cyclical stability, will have very important significance.
[content of the invention]
Present invention aim to solve above-mentioned deficiency and to provide a kind of graphene oxide doped Co-anderson miscellaneous
The method that polyacid prepares super capacitor material, improves the grapheme material of ultracapacitor chemical property in itself and letter
Change its preparation technology, and easy control of reaction conditions, preparation process is relatively simple, obtained product quality stability very well, has
Beneficial to industrialized production.
A kind of graphene oxide doped Co-anderson heteropoly acids are designed to achieve the above object prepares super capacitor equipment
The method of material, comprises the following steps：1) Co-anderson heteropoly acids are taken to dissolve in graphene oxide solution, in temperature 10-45
DEG C, ultrasonic mixing is uniform under power 100-200W, frequency 15-20Hz；2) mixed solution is put into pyroreaction kettle, HTHP
12h is reacted, redox graphene obtains graphene post；3) take out step 2) obtained by graphene post, soaked with deionized water
48h, removes the ion dissociated in graphene, dries graphene；4) graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:1:1 ratio
Example grinding, that is, be made super capacitor material.
Further, step 1) in, appropriate graphene oxide solution is first taken, deionized water is added, ultrasound dissipates oxidation stone
Black alkene, prepares 4g/L graphene oxide solution, then takes Co-anderson heteropoly acids to dissolve in the graphene oxide solution, should
The concentration of heteropoly acid is 0.1-0.8mol/L, and ultrasound stirs evenly 30-40min.
Further, step 1) in, the structure of the Co-anderson heteropoly acids adulterated is Anderson crystal formations.
Further, step 2) in, the temperature control of high-temperature high-voltage reaction is and every in the temperature rise period at 100-260 DEG C
Minute heating is no more than 10 DEG C.
Further, step 3) in, graphene post is washed with deionized more than 2 times.
Further, step 3) in, graphene is dried by the way of drying, the temperature control of drying is at 60-80 DEG C.
Further, step 3) in, graphene is dried by the way of lyophilized, lyophilized time control is in more than 48h.
Present invention also offers a kind of super capacitor material obtained using above-mentioned preparation method in ultracapacitor
The application of middle aspect.
The super capacitor material have improve ultracapacitor chemical property, the chemical property include than
Electric capacity, cyclical stability and charge/discharge rates.
The present invention is compared with the existing technology, sharp by taking Co-anderson heteropoly acids to dissolve in the solution of graphene oxide
Solution is stirred evenly with ultrasonic wave, mixed solution is put into pyroreaction kettle, reaction obtains graphene post, further takes out graphene post, go
Fall the ion dissociated in graphene, dry graphene, graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:1:1 ratio grinding, from
And super capacitor material is prepared, its easy control of reaction conditions, preparation process is relatively simple, obtained product quality stability
Very well, be conducive to industrialized production, improve the chemical property of the grapheme material of ultracapacitor in itself and simplify its system
Standby technique, improves the chemical property of grapheme material, is worthy of popularization.
[brief description of the drawings]
Fig. 1 is the IR Characterization figure of Co-anderson heteropoly acids of the present invention；
Fig. 2 is graphene oxide doped Co-anderson heteropoly acids capacitor (1 of the present invention:0.05) SEM figures；
Fig. 3 is graphene oxide doped Co-anderson heteropoly acids capacitor (1 of the present invention:0.1) SEM figures；
Fig. 4 is graphene oxide doped Co-anderson heteropoly acids capacitor (1 of the present invention:0.2) SEM figures；
Fig. 5 is the charge and discharge electrograph of super capacitor material in the embodiment of the present invention 2.
[embodiment]
The invention provides the side that a kind of graphene oxide doped Co-anderson heteropoly acids prepare super capacitor material
Method, comprises the following steps：1) Co-anderson heteropoly acids are taken to dissolve in graphene oxide solution, in 10-45 DEG C of temperature, power
Ultrasonic mixing is uniform under 100-200W, frequency 15-20Hz；2) mixed solution is put into pyroreaction kettle, high-temperature high-voltage reaction
12h, redox graphene obtains graphene post；3) take out step 2) obtained by graphene post, with deionized water soak 48h,
Remove the ion dissociated in graphene, dry graphene；4) graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:1:1 ratio is ground
Mill, that is, be made super capacitor material.Wherein, step 1) in, appropriate graphene oxide solution is first taken, deionized water is added, surpassed
Sound dissipates graphene oxide, prepares 4g/L graphene oxide solution, then take Co-anderson heteropoly acids to dissolve in the graphite oxide
In alkene solution, the concentration of the heteropoly acid is 0.1-0.8mol/L, and ultrasound stirs evenly 30-40min, it is ensured that Dispersion of Solute Matter is uniform；Mixed
The structure of miscellaneous Co-anderson heteropoly acids is Anderson crystal formations, and the Co-anderson heteropoly acids that adulterate are to improve super
The performance of capacitor.Step 2) in, the temperature control of high-temperature high-voltage reaction is and per minute in the temperature rise period at 100-260 DEG C
Heating is no more than 10 DEG C.Step 3) in, graphene post is washed with deionized more than 2 times, more than 48h is soaked, and dry stone
The mode of black alkene post is not limited；Mode according to drying dries graphene, and the temperature control of drying is at 60-80 DEG C；According to jelly
Dry mode dries graphene, then lyophilized time control is in more than 48h.
Present invention also offers a kind of super capacitor material obtained using above-mentioned preparation method in ultracapacitor
The application of middle aspect, the super capacitor material has the chemical property for improving ultracapacitor, such as specific capacitance, stable circulation
Property and charge/discharge rates.
Technical scheme is further described with reference to specific embodiment, but the invention is not restricted to following
Embodiment.
Embodiment 1
15ml graphene oxide solutions are taken, 85ml deionized waters are added, ultrasound is put into 30 minutes and dissipates graphene oxide.Claim
Co-anderson heteropoly acid 0.05g are taken, above-mentioned 25mL graphene oxide solution is dissolved in.Solution is in 10-45 DEG C of temperature, power
Ultrasound stirs evenly 30-40min under 100-200W, frequency 15-20Hz, it is ensured that Dispersion of Solute Matter is uniform；Mixed solution is put into high temperature anti-
Kettle is answered, high-temperature high-voltage reaction 12h is carried out at 180 DEG C, reaction obtains graphene post；Graphene post is taken out, is soaked with deionized water
48h is steeped, removes the ion dissociated in graphene, drying or lyophilized graphene；Graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:
1:1 ratio grinding, prepares super capacitor material.
Embodiment 2
15ml graphene oxide solutions are taken, 85ml deionized waters are added, ultrasound is put into 30 minutes and dissipates graphene oxide.Claim
Co-anderson heteropoly acid 0.1g are taken, above-mentioned 25mL graphene oxide solution is dissolved in.Solution is in 10-45 DEG C of temperature, power
Ultrasound stirs evenly 30-40min under 100-200W, frequency 15-20Hz, it is ensured that Dispersion of Solute Matter is uniform；Mixed solution is put into high temperature anti-
Kettle is answered, high-temperature high-voltage reaction 12h is carried out at 180 DEG C, reaction obtains graphene post；Graphene post is taken out, is soaked with deionized water
48h is steeped, removes the ion dissociated in graphene, drying or lyophilized graphene；Graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:
1:1 ratio grinding, prepares super capacitor material.Drawn a conclusion through charge-discharge test, the specific capacitance of the material reaches
1285C/g, such as Fig. 5.
Embodiment 3
15ml graphene oxide solutions are taken, 85ml deionized waters are added, ultrasound is put into 30 minutes and dissipates graphene oxide.Claim
Co-anderson heteropoly acid 0.2g are taken, above-mentioned 25mL graphene oxide solution is dissolved in.Solution is in 10-45 DEG C of temperature, power
Ultrasound stirs evenly 30-40min under 100-200W, frequency 15-20Hz, it is ensured that Dispersion of Solute Matter is uniform；Mixed solution is put into high temperature anti-
Kettle is answered, high-temperature high-voltage reaction 12h is carried out at 260 DEG C, reaction obtains graphene post；Graphene post is taken out, is soaked with deionized water
48h is steeped, removes the ion dissociated in graphene, drying or lyophilized graphene；Graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:
1:1 ratio grinding, prepares super capacitor material.
Embodiment 4
15ml graphene oxide solutions are taken, 85ml deionized waters are added, ultrasound is put into 30 minutes and dissipates graphene oxide.Claim
Co-anderson heteropoly acid 0.2g are taken, above-mentioned 25mL graphene oxide solution is dissolved in.Solution is in 10-45 DEG C of temperature, power
Ultrasound stirs evenly 30-40min under 100-200W, frequency 15-20Hz, it is ensured that Dispersion of Solute Matter is uniform；Mixed solution is put into high temperature anti-
Kettle is answered, high-temperature high-voltage reaction 12h is carried out at 100 DEG C, reaction obtains graphene post；Graphene post is taken out, is soaked with deionized water
48h is steeped, removes the ion dissociated in graphene, drying or lyophilized graphene；Graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:
1:1 ratio grinding, prepares super capacitor material.
In summary, the graphene super capacitor material of a kind of Co-anderson heteropoly acids doping of the present invention,
Among the above embodiments, observe obtained super capacitor material and be uniformly dispersed, and capacitor high rate performance is improved
A lot, its specific capacitance has reached 1285C/g, and course of reaction is simple, and preparation condition is easily controlled, it is easy to operated, can
Realize industrialized production.
The present invention is simultaneously not limited to the embodiments described above limitation, other any Spirit Essences and principle without departing from the present invention
Lower made change, modification, replacement, combination, simplification, should be equivalent substitute mode, be included in the protection model of the present invention
Within enclosing.
Claims (9)
1. a kind of method that graphene oxide doped Co-anderson heteropoly acids prepare super capacitor material, it is characterised in that
Comprise the following steps：
1) Co-anderson heteropoly acids are taken to dissolve in graphene oxide solution, in 10-45 DEG C of temperature, power 100-200W, frequency
Ultrasonic mixing is uniform under 15-20Hz；
2) mixed solution is put into pyroreaction kettle, high-temperature high-voltage reaction 12h, redox graphene obtains graphene post；
3) take out step 2) obtained by graphene post, with deionized water soak 48h, remove in graphene dissociate ion, dry
Graphene；
4) graphene, carbon black and polytetrafluoroethylene (PTFE) are pressed 8:1:1 ratio grinding, that is, be made super capacitor material.
2. the method as described in claim 1, it is characterised in that：Step 1) in, appropriate graphene oxide solution is first taken, addition is gone
Ionized water, ultrasound dissipates graphene oxide, prepares 4g/L graphene oxide solution, then take Co-anderson heteropoly acids to dissolve in
In the graphene oxide solution, the concentration of the heteropoly acid is 0.1-0.8mol/L, and ultrasound stirs evenly 30-40min.
3. the method as described in claim 1, it is characterised in that：Step 1) in, the knot of the Co-anderson heteropoly acids adulterated
Structure is Anderson crystal formations.
4. the method as described in claim 1, it is characterised in that：Step 2) in, the temperature control of high-temperature high-voltage reaction is in 100-
260 DEG C, and in the temperature rise period, heating per minute is no more than 10 DEG C.
5. the method as described in claim 1, it is characterised in that：Step 3) in, by graphene post be washed with deionized 2 times with
On.
6. the method as described in claim 1, it is characterised in that：Step 3) in, graphene is dried by the way of drying, is dried
Temperature control at 60-80 DEG C.
7. the method as described in claim 1, it is characterised in that：Step 3) in, graphene is dried by the way of lyophilized, is freezed
Time control in more than 48h.
8. a kind of graphene oxide doped Co-anderson heteropoly acids as any one of claim 1 to 7 prepare super
The application of the super capacitor material that the method for capacitor material is obtained aspect in ultracapacitor.
9. application as claimed in claim 8, it is characterised in that：The super capacitor material, which has, improves ultracapacitor
Chemical property, the chemical property includes specific capacitance, cyclical stability and charge/discharge rates.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107578924A (en) * | 2017-09-07 | 2018-01-12 | 上海应用技术大学 | A kind of electrode material for super capacitor based on graphene-supported Cr Anderson heteropoly acids and preparation method thereof |
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Application publication date: 20170808 |