CN109273279A - A kind of electrode material for super capacitor - Google Patents
A kind of electrode material for super capacitor Download PDFInfo
- Publication number
- CN109273279A CN109273279A CN201811418972.7A CN201811418972A CN109273279A CN 109273279 A CN109273279 A CN 109273279A CN 201811418972 A CN201811418972 A CN 201811418972A CN 109273279 A CN109273279 A CN 109273279A
- Authority
- CN
- China
- Prior art keywords
- ethyl alcohol
- presoma
- electrode material
- super capacitor
- sulfur doping
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003990 capacitor Substances 0.000 title claims abstract description 11
- 239000007772 electrode material Substances 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 12
- 239000011593 sulfur Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 20
- 229960004756 ethanol Drugs 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- GUUVPOWQJOLRAS-UHFFFAOYSA-N Diphenyl disulfide Chemical compound C=1C=CC=CC=1SSC1=CC=CC=C1 GUUVPOWQJOLRAS-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 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
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000002019 doping agent Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000013110 organic ligand Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 238000001816 cooling Methods 0.000 description 4
- 239000012621 metal-organic framework Substances 0.000 description 4
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000001338 self-assembly 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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of electrode material for super capacitor, it is using a kind of CO-MOF as presoma, select sulfur doping graphene as carrier and additive, gained is prepared by the way of calcining after sol precursor is freeze-dried, the spacial framework with high conductance can be formed in the composite, to substantially increase the high rate capability and cyclical stability of electrode material, have many advantages, such as that high volume and capacity ratio, good cycling stability and power density are high using the material as capacitor constructed by electrode.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of electrode material for super capacitor.
Background technique
Metal-organic framework object (MOFs) is to be self-assembly of by organic ligand and metal ion or cluster by coordinate bond
The hybrid inorganic-organic materials with molecule inner pore.In MOFs, the arrangement of organic ligand and metal ion or cluster has
Have apparent directionality, different frame pore structures can be formed, thus show different absorption properties, optical property,
Electromagnetic property.It has high porosity, low-density, bigger serface, duct rule, aperture is adjustable and topological structure is various
The advantages that property and Scalability.
Supercapacitor is a kind of model electrochemical energy storage device between conventional capacitive and battery, wherein development
High performance electrode material is one of the important research direction for realizing high-performance super capacitor.The study found that one or more miscellaneous
Atom (nitrogen, boron, sulphur) doped graphene being capable of significant raising performance of the supercapacitor.
Summary of the invention
To solve the above problems, the present invention provides a kind of electrode material for super capacitor.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of electrode material for super capacitor, as obtained by following steps preparation:
It S1, by cobalt nitrate and terephthalic acid (TPA) organic ligand is in molar ratio the ratio mixed dissolution of 1:1 in 60mL N, N-
In dimethylformamide, after ultrasonic disperse, solution is transferred in 100mL polytetrafluoroethylene (PTFE) autoclave, at 110~130 DEG C
36~48h is reacted, is then slowly cooled to room temperature, after filtering, solid is washed 3 times with dehydrated alcohol, dry 4 at 50~60 DEG C
~6h is to get presoma；
S2,100mg graphene oxide is taken, is dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, is added
50mg diphenyl disulfide dopant, magnetic agitation to mixture place it in the tube furnace full of argon gas in after drying regime,
500~600 DEG C are heat-treated 2~4 hours, then respectively clean products therefrom deionized water and ethyl alcohol 3 times, are placed in 50 in baking oven
~60 DEG C of low temperature dryings, obtain sulfur doping graphene；
S3,100mg sulfur doping graphene is taken to be added in the ethyl alcohol of 120~150mL, after ultrasonic vibration 3 hours, by forerunner
Body is added to 1.5h is sufficiently stirred in said mixture after, mixed liquor is progressively heated at 60~80 DEG C, makes ethyl alcohol and deionization
Water constantly volatilizees, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally
Presoma is placed in microwave tube type oven, in N2Under protective condition, 1000 DEG C of holding 3h are risen to 3 DEG C/min heating rate, and
After be naturally cooling to room temperature to get.
The invention has the following advantages:
Using a kind of CO-MOF as presoma, select sulfur doping graphene as carrier and additive, it can be in composite material
It is middle to form the spacial framework with high conductance, so that the high rate capability and circulation that substantially increase electrode material are surely
It is qualitative, there is high volume and capacity ratio, good cycling stability and power density height etc. by capacitor constructed by electrode of the material
Advantage.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment 1
A kind of electrode material for super capacitor, as obtained by following steps preparation:
S1, by 2.91g cobalt nitrate hexahydrate and 1.66g terephthalic acid (TPA) mixed dissolution in 60mL N,N-dimethylformamide
In, after ultrasonic disperse, solution is transferred in 100mL polytetrafluoroethylene (PTFE) autoclave, 48h is reacted at 110 DEG C, it is then slowly cold
But to room temperature, after filtering, solid is washed 3 times with dehydrated alcohol, and dry 6h is at 50 DEG C to get presoma；
S2,100mg graphene oxide is taken, is dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, is added
50mg diphenyl disulfide dopant, magnetic agitation to mixture place it in the tube furnace full of argon gas in after drying regime,
500 DEG C are heat-treated 4 hours, then respectively clean products therefrom deionized water and ethyl alcohol 3 times, are placed in 50 DEG C of low temperature in baking oven and dry
It is dry, obtain sulfur doping graphene；
S3, take 100mg sulfur doping graphene to be added in the ethyl alcohol of 120mL, after ultrasonic vibration 3 hours, by presoma plus
Enter after 1.5h is sufficiently stirred into said mixture, mixed liquor is progressively heated at 60 DEG C, waves ethyl alcohol and deionized water constantly
Hair, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally
Presoma is placed in microwave tube type oven, in N2Under protective condition, 1000 DEG C of holding 3h are risen to 3 DEG C/min heating rate, and
After be naturally cooling to room temperature to get.
Embodiment 2
S1, by 2.91g cobalt nitrate hexahydrate and 1.66g terephthalic acid (TPA) mixed dissolution in 60mL N,N-dimethylformamide
In, after ultrasonic disperse, solution is transferred in 100mL polytetrafluoroethylene (PTFE) autoclave, 42h is reacted at 120 DEG C, it is then slowly cold
But to room temperature, after filtering, solid is washed 3 times with dehydrated alcohol, and dry 5h is at 55 DEG C to get presoma；
S2,100mg graphene oxide is taken, is dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, is added
50mg diphenyl disulfide dopant, magnetic agitation to mixture place it in the tube furnace full of argon gas in after drying regime,
550 DEG C are heat-treated 2.5 hours, then respectively clean products therefrom deionized water and ethyl alcohol 3 times, are placed in 55 DEG C of low temperature in baking oven
Drying, obtains sulfur doping graphene；
S3, take 100mg sulfur doping graphene to be added in the ethyl alcohol of 135mL, after ultrasonic vibration 3 hours, by presoma plus
Enter after 1.5h is sufficiently stirred into said mixture, mixed liquor is progressively heated at 70 DEG C, waves ethyl alcohol and deionized water constantly
Hair, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally
Presoma is placed in microwave tube type oven, in N2Under protective condition, 1000 DEG C of holding 3h are risen to 3 DEG C/min heating rate, and
After be naturally cooling to room temperature to get.
Embodiment 3
S1, by 2.91g cobalt nitrate hexahydrate and 1.66g terephthalic acid (TPA) mixed dissolution in 60mL N,N-dimethylformamide
In, after ultrasonic disperse, solution is transferred in 100mL polytetrafluoroethylene (PTFE) autoclave, 36h is reacted at 130 DEG C, it is then slowly cold
But to room temperature, after filtering, solid is washed 3 times with dehydrated alcohol, and dry 4h is at 60 DEG C to get presoma；
S2,100mg graphene oxide is taken, is dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, is added
50mg diphenyl disulfide dopant, magnetic agitation to mixture place it in the tube furnace full of argon gas in after drying regime,
600 DEG C are heat-treated 2 hours, then respectively clean products therefrom deionized water and ethyl alcohol 3 times, are placed in 60 DEG C of low temperature in baking oven and dry
It is dry, obtain sulfur doping graphene；
S3, take 100mg sulfur doping graphene to be added in the ethyl alcohol of 150mL, after ultrasonic vibration 3 hours, by presoma plus
Enter after 1.5h is sufficiently stirred into said mixture, mixed liquor is progressively heated at 80 DEG C, waves ethyl alcohol and deionized water constantly
Hair, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally
Presoma is placed in microwave tube type oven, in N2Under protective condition, 1000 DEG C of holding 3h are risen to 3 DEG C/min heating rate, and
After be naturally cooling to room temperature to get.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of electrode material for super capacitor, which is characterized in that as obtained by following steps preparation:
It S1, is in molar ratio the ratio mixed dissolution of 1:1 by cobalt nitrate and terephthalic acid (TPA) organic ligand in 60mL N, N- diformazan
In base formamide, after ultrasonic disperse, solution is transferred in 100mL polytetrafluoroethylene (PTFE) autoclave, is reacted at 110~130 DEG C
Then 36~48h is slowly cooled to room temperature, after filtering, solid is washed 3 times with dehydrated alcohol, dry 4 at 50~60 DEG C~
6h is to get presoma；
S2,100mg graphene oxide is taken, is dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, 50mg is added
Diphenyl disulfide dopant, magnetic agitation to mixture place it in the tube furnace full of argon gas, 500 in after drying regime
~600 DEG C are heat-treated 2~4 hours, then respectively clean products therefrom deionized water and ethyl alcohol 3 times, be placed in 50 in baking oven~
60 DEG C of low temperature dryings, obtain sulfur doping graphene；
S3, take 100mg sulfur doping graphene to be added in the ethyl alcohol of 120~150mL, after ultrasonic vibration 3 hours, by presoma plus
Enter after 1.5h is sufficiently stirred into said mixture, mixed liquor is progressively heated at 60~80 DEG C, makes ethyl alcohol and deionized water not
Disconnected volatilization, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally will before
It drives body to be placed in microwave tube type oven, in N2Under protective condition, 1000 DEG C of holding 3h are risen to 3 DEG C/mi n heating rate, then certainly
So be cooled to room temperature to get.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811418972.7A CN109273279A (en) | 2018-11-26 | 2018-11-26 | A kind of electrode material for super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811418972.7A CN109273279A (en) | 2018-11-26 | 2018-11-26 | A kind of electrode material for super capacitor |
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| Publication Number | Publication Date |
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| CN109273279A true CN109273279A (en) | 2019-01-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811418972.7A Pending CN109273279A (en) | 2018-11-26 | 2018-11-26 | A kind of electrode material for super capacitor |
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| CN (1) | CN109273279A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110060875A (en) * | 2019-04-29 | 2019-07-26 | 南京工业大学 | Co-based nanosheet array electrode for supercapacitor and preparation method thereof |
| CN111477471A (en) * | 2020-04-25 | 2020-07-31 | 榆林学院 | Preparation method of coal tar-based electrode material |
| CN112863901A (en) * | 2021-03-03 | 2021-05-28 | 郑州航空工业管理学院 | Preparation method of supercapacitor slurry |
| CN116675223A (en) * | 2023-08-03 | 2023-09-01 | 国联汽车动力电池研究院有限责任公司 | Porous composite anode material, preparation method thereof and low-temperature battery |
Citations (4)
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| CN104475172A (en) * | 2014-11-21 | 2015-04-01 | 东华大学 | Preparation method and application of three-dimensional porous heteroatom-doped graphene |
| CN105366664A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Production method for sulfur-doped graphene |
| CN107195875A (en) * | 2017-04-26 | 2017-09-22 | 复旦大学 | A kind of three-dimensional grapheme cladding MOF composite electrode material and preparation method thereof |
| CN107215863A (en) * | 2017-04-14 | 2017-09-29 | 浙江工业大学 | The method that one kind prepares the composite porous hydrogels of graphene/MOF and aeroge |
-
2018
- 2018-11-26 CN CN201811418972.7A patent/CN109273279A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366664A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Production method for sulfur-doped graphene |
| CN104475172A (en) * | 2014-11-21 | 2015-04-01 | 东华大学 | Preparation method and application of three-dimensional porous heteroatom-doped graphene |
| CN107215863A (en) * | 2017-04-14 | 2017-09-29 | 浙江工业大学 | The method that one kind prepares the composite porous hydrogels of graphene/MOF and aeroge |
| CN107195875A (en) * | 2017-04-26 | 2017-09-22 | 复旦大学 | A kind of three-dimensional grapheme cladding MOF composite electrode material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110060875A (en) * | 2019-04-29 | 2019-07-26 | 南京工业大学 | Co-based nanosheet array electrode for supercapacitor and preparation method thereof |
| CN111477471A (en) * | 2020-04-25 | 2020-07-31 | 榆林学院 | Preparation method of coal tar-based electrode material |
| CN112863901A (en) * | 2021-03-03 | 2021-05-28 | 郑州航空工业管理学院 | Preparation method of supercapacitor slurry |
| CN116675223A (en) * | 2023-08-03 | 2023-09-01 | 国联汽车动力电池研究院有限责任公司 | Porous composite anode material, preparation method thereof and low-temperature battery |
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Application publication date: 20190125 |