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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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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 OR LIGHT-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
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 |
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| 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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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 base nano-chip arrays electrode and preparation method thereof for supercapacitor |
| 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 |
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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 base nano-chip arrays electrode and preparation method thereof for supercapacitor |
| 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 |