CN105374574A - Preparation method and application of cobalt hydroxide/graphene flexible electrode material - Google Patents
Preparation method and application of cobalt hydroxide/graphene flexible electrode material Download PDFInfo
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- CN105374574A CN105374574A CN201510990677.9A CN201510990677A CN105374574A CN 105374574 A CN105374574 A CN 105374574A CN 201510990677 A CN201510990677 A CN 201510990677A CN 105374574 A CN105374574 A CN 105374574A
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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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
-
- 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
- H01G11/84—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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparation method and application of a cobalt hydroxide/graphene flexible electrode material and mainly solves the problems that a conductive film material prepared through a conventional method is low in specific capacitance and poor in mechanical property. The preparation method comprises the following steps: preparing bacterial cellulose pulp; preparing a cobalt hydroxide/graphene composite, carrying out vacuum filtration on the bacterial cellulose pulp to form a film, adding cobalt hydroxide/graphene composite dispersion liquid, and continuously carrying out suction filtration and drying, so as to obtain the cobalt hydroxide/graphene flexible electrode material. The cobalt hydroxide/graphene flexible electrode material is applied to supercapacitors. The electrode active material is high in specific capacitance and excellent in flexible electrode mechanical property. The supercapacitors prepared from the electrode material have a good capacitive character. The invention belongs to the technical field of nanometer materials.
Description
Technical field
The present invention relates to preparation method and the application thereof of a kind of cobalt hydroxide/Graphene flexible electrode material.
Background technology
Ultracapacitor combines the advantage of battery and conventional dielectric capacitor, and its energy density and power density have filled up the blank between battery and conventional dielectric capacitor.
Ultracapacitor can be divided into electrochemical capacitor in double electrode layer and fake capacitance capacitor by mechanism.Wherein by increasing the surface area of electrode material and reducing the thickness of electric double layer, the specific capacity of capacitor can be improved.Grapheme material chemically stable, conductance are high, and theoretical specific surface area is high.Relative to double electric layer capacitor, pseudocapacitors can be reacted by faraday, provides higher capacitance.Transition group metallic oxide or hydroxide can produce good fake capacitance, provide higher capacitance.There are relatively preferably high rate performance and cyclical stability.Cobalt hydroxide has layer structure and larger interlamellar spacing, has high theoretical specific capacity, high specific area and fast ion insert extrusion rate, become a kind of outstanding electrode material.But the material specific capacity often prepared is very low.
Along with development that is flexible, flexible electronic device, exploitation has the important directions that the flexible electrode material bending stability has become current energy storage area research.Relative to metal oxide and hydroxide thereof, in early stage electrode production process, often need to add binding agent, hinder the contact of part electrolyte and active material, add the internal resistance of electrode, add the fast transfer of ion and electronics.
Summary of the invention
The present invention is the problem that will solve conducting membrane material specific capacitance prepared by existing method low and cycle performance and poor mechanical property, provides preparation method and the application thereof of a kind of cobalt hydroxide/Graphene flexible electrode material.
The preparation method of the present invention's a kind of cobalt hydroxide/Graphene flexible electrode material, carries out according to the following steps:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing deacidification, then in deionized water dispersed, then transfer to the stirring of refiner high speed, obtain substrate bacteria cellulose slurry;
Two, by graphene oxide, be scattered in distilled water, obtain graphene oxide dispersion; Be dissolved in distilled water by cobalt salt, then join in graphene oxide dispersion, ultrasonic disperse is even, then adds ammoniacal liquor, transfers in reactor after mixing, and heating, obtains cobalt hydroxide graphene composite material;
Three, by bacteria cellulose slurry vacuum filtration film forming, then add cobalt hydroxide graphene composite material and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make cobalt hydroxide/Graphene flexible electrode material;
In wherein cobalt hydroxide/Graphene flexible electrode material, after cobalt hydroxide and vacuum filtration, the mass ratio of bacteria cellulose is (0.1 ~ 6): 1; In step 2, the ratio of graphene oxide and cobalt salt is 1mg:(0.001mmol ~ 0.3mmol); The mass volume ratio of graphene oxide and ammoniacal liquor is 1mg:(0.001 ~ 0.1) mL; Wherein said ammoniacal liquor is the ammoniacal liquor of 25wt%.
Beneficial effect of the present invention:
(1) bacteria cellulose aboundresources, environmental friendliness, has hyperfine network structure and extraordinary mechanical property.Large quantity research has shown that the material with carbon element such as bacteria cellulose and Graphene has extraordinary adhesion.Utilize its feature, load hydrogen cobalt oxide graphene composite material, makes materials serve synergy, remains the mechanical property of the excellence of flexible material and the high ratio capacitance of cobalt hydroxide.Bacteria cellulose contains a large amount of hydroxyls simultaneously, in the application of water-based ultracapacitor, has good hydrophily, decreases impedance.Bacteria cellulose aboundresources, with low cost, cobalt hydroxide ratio capacitance is high, and Graphene has excellent conductivity and also improves good electric double layer capacitance simultaneously.Utilize the synergy of material, prepared the flexible material of high specific capacitance and mechanical property, ratio capacitance can reach 847F/g, is applied to ultracapacitor;
(2) preparation technology is simple, and the prices of raw and semifnished materials are cheap;
(3) be directly used as electrode of super capacitor and there is good capacitive character.
Accompanying drawing explanation
The stereoscan photograph of the cobalt hydroxide that Fig. 1 and Fig. 2 obtains for embodiment 1/Graphene flexible electrode material;
Cyclic voltammetry curve under the different scanning speed of the work electrode prepared with cobalt hydroxide/Graphene flexible electrode material that Fig. 3 obtains for embodiment 1 in 6M potassium hydroxide electrolyte; Wherein a is 20mV/s, b be 50mV/s, c is 100mV/s;
The stereoscan photograph of the cobalt hydroxide that Fig. 4 obtains for embodiment 2/Graphene flexible electrode material;
Cyclic voltammetry curve under the different scanning speed of the work electrode prepared with cobalt hydroxide/Graphene flexible electrode material that Fig. 5 obtains for embodiment 2 in 6M potassium hydroxide electrolyte; Wherein a is 20mV/s, b be 50mV/s, c is 100mV/s.
Embodiment
Embodiment one: the preparation method of present embodiment a kind of cobalt hydroxide/Graphene flexible electrode material, carry out according to the following steps:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing deacidification, then in deionized water dispersed, then transfer to the stirring of refiner high speed, obtain substrate bacteria cellulose slurry;
Two, by graphene oxide, be scattered in distilled water, obtain graphene oxide dispersion; Be dissolved in distilled water by cobalt salt, then join in graphene oxide dispersion, ultrasonic disperse is even, then adds ammoniacal liquor, transfers in reactor after mixing, and heating, obtains cobalt hydroxide graphene composite material;
Three, by bacteria cellulose slurry vacuum filtration film forming, then add cobalt hydroxide graphene composite material and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make cobalt hydroxide/Graphene flexible electrode material;
In wherein cobalt hydroxide/Graphene flexible electrode material, after cobalt hydroxide and vacuum filtration, the mass ratio of bacteria cellulose is (0.1 ~ 6): 1; In step 2, the ratio of graphene oxide and cobalt salt is 1mg:(0.001mmol ~ 0.3mmol); The mass volume ratio of graphene oxide and ammoniacal liquor is 1mg:(0.001 ~ 0.1) mL; Wherein said ammoniacal liquor is the ammoniacal liquor of 25wt%.
The beneficial effect of present embodiment:
(1) bacteria cellulose aboundresources, environmental friendliness, has hyperfine network structure and extraordinary mechanical property.Large quantity research has shown that the material with carbon element such as bacteria cellulose and Graphene has extraordinary adhesion.Utilize its feature, load hydrogen cobalt oxide graphene composite material, makes materials serve synergy, remains the mechanical property of the excellence of flexible material and the high ratio capacitance of cobalt hydroxide.Bacteria cellulose contains a large amount of hydroxyls simultaneously, in the application of water-based ultracapacitor, has good hydrophily, decreases impedance.Bacteria cellulose aboundresources, with low cost, cobalt hydroxide ratio capacitance is high, and Graphene has excellent conductivity and also improves good electric double layer capacitance simultaneously.Utilize the synergy of material, prepared the flexible material of high specific capacitance and mechanical property, ratio capacitance can reach 847F/g, is applied to ultracapacitor;
(2) preparation technology is simple, and the prices of raw and semifnished materials are cheap;
(3) be directly used as electrode of super capacitor and there is good capacitive character.
Embodiment two: present embodiment and embodiment one unlike: described ultrasonic power is 1000w, and frequency is 30KHz.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the condition of the supersound washing described in step one is ultrasonic time 1 ~ 10h.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the speed of the high-speed stirred described in step one is 8000 ~ 15000r/min, mixing time 3 ~ 30min.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the cobalt salt described in step 2 is cobalt acetate, cobalt chloride, cobaltous sulfate or cobalt nitrate.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the reactor described in step 2 is liner tetrafluoro high-temperature high-pressure reaction kettle.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the temperature heated in step 2 is 90 ~ 200 DEG C, and the reaction time is 2h ~ 15h.Other is identical with one of embodiment one to six.
Embodiment eight: the present embodiment cobalt hydroxide/application of Graphene flexible electrode material refers to and is applied in ultracapacitor.
Embodiment nine: present embodiment and embodiment eight unlike: this flexible electrode material is applied in ultracapacitor as positive electrode.Other is identical with embodiment eight.
Beneficial effect of the present invention is verified by following examples:
Embodiment 1: the preparation method of the present embodiment a kind of cobalt hydroxide/Graphene flexible electrode material, carry out according to the following steps:
One, 5g bacteria cellulose is immersed in deionized water for ultrasonic washing 3h, then in deionized water dispersed, then transfer to the stirring of refiner high speed, obtain substrate bacteria cellulose slurry;
Two, by 30mg graphene oxide, be scattered in distilled water, obtain graphene oxide dispersion; 0.4mmol cobaltous sulfate is dissolved in distilled water, then joins in graphene oxide dispersion, ultrasonic 30min, then the ammoniacal liquor of 0.1mL25wt% is added, transfer in liner tetrafluoro high-temperature high-pressure reaction kettle after stirring 30min, be heated to 150 DEG C of reaction 4h, obtain cobalt hydroxide graphene composite material;
Three, by bacteria cellulose slurry vacuum filtration film forming, then add cobalt hydroxide graphene composite material and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make cobalt hydroxide/Graphene flexible electrode material;
The quality of the bacteria cellulose substrate in cobalt hydroxide/Graphene flexible electrode material after vacuumize is 0.15g.
Obtained cobalt hydroxide/Graphene flexible electrode material is cut into 1cm × 2cm rectangle, is directly used as ultracapacitor work electrode, platinized platinum, as to electrode, with mercury/mercuric oxide electrode for reference electrode, tests the capacitance characteristic of flexible electrode material.Test specimens product are labeled as COGO-BC-1.
The flexible electrode material that the present embodiment obtains is tested.Cobalt hydroxide nano material and graphene uniform disperse as seen from Figure 1, can find out that cobalt hydroxide nano material presents sheet clearly by Fig. 2.Demonstrating the scanning potential window of cobalt hydroxide graphene composite material that difference sweeps speed in Fig. 3 is 0.2 ~ 0.75V.There is obvious redox peak.Along with the increase of sweep speed, response current increases, and shows good high rate performance.The flexible electrode material that the present embodiment obtains is when 2mV/s, and ratio capacitance can reach 847F/g.
Embodiment 2: the preparation method of the present embodiment a kind of cobalt hydroxide/Graphene flexible electrode material, carry out according to the following steps:
One, 4g bacteria cellulose is immersed in deionized water for ultrasonic washing 3h, then in deionized water dispersed, then transfer to the stirring of refiner high speed, obtain substrate bacteria cellulose slurry;
Two, by 40mg graphene oxide, be scattered in distilled water, obtain graphene oxide dispersion; 0.35mmol cobaltous sulfate is dissolved in distilled water, join again in graphene oxide dispersion, ultrasonic 30min, then the ammoniacal liquor of 0.18mL25wt% is added, transfer in liner tetrafluoro high-temperature high-pressure reaction kettle after stirring 30min, be heated to 170 DEG C of reaction 3h, obtain cobalt hydroxide graphene composite material;
Three, by bacteria cellulose slurry vacuum filtration film forming, then add cobalt hydroxide graphene composite material and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make cobalt hydroxide/Graphene flexible electrode material;
The quality of the bacteria cellulose substrate in cobalt hydroxide/Graphene flexible electrode material after vacuumize is 0.12g.
Obtained cobalt hydroxide/Graphene flexible electrode material is cut into 1cm × 1.5cm rectangle, directly be used as ultracapacitor work electrode, platinized platinum, as to electrode, with mercury/mercuric oxide electrode for reference electrode, tests the capacitance characteristic of flexible electrode material electrode material.Test specimens product are labeled as COGO-BC-2.
Sheet attitude cobalt hydroxide nano material composition flower dress as seen from Figure 4, and more dispersed with Graphene;
Demonstrating the scanning potential window of cobalt hydroxide graphene composite material that difference sweeps speed in Fig. 5 is 0.2 ~ 0.75V.There is obvious redox peak.Along with the increase of sweep speed, response current increases, and shows good high rate performance.
Embodiment 1 ~ 2 cobalt hydroxide specific capacitance is high, and Graphene has excellent conductivity and also improves good electric double layer capacitance simultaneously.Utilize the synergy of material, the flexible electrode material having prepared high specific capacitance and mechanical property is applied in ultracapacitor has good capacitive character; Preparation technology is simple, and the prices of raw and semifnished materials are cheap.
Claims (9)
1. a preparation method for cobalt hydroxide/Graphene flexible electrode material, is characterized in that the method is carried out according to the following steps:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing deacidification, then in deionized water dispersed, then transfer to the stirring of refiner high speed, obtain substrate bacteria cellulose slurry;
Two, by graphene oxide, be scattered in distilled water, obtain graphene oxide dispersion; Be dissolved in distilled water by cobalt salt, then join in graphene oxide dispersion, ultrasonic disperse is even, then adds ammoniacal liquor, transfers in reactor after mixing, and heating, obtains cobalt hydroxide graphene composite material;
Three, by bacteria cellulose slurry vacuum filtration film forming, then add cobalt hydroxide graphene composite material and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make cobalt hydroxide/Graphene flexible electrode material;
In wherein cobalt hydroxide/Graphene flexible electrode material, after cobalt hydroxide and vacuum filtration, the mass ratio of bacteria cellulose is (0.1 ~ 6): 1; In step 2, the ratio of graphene oxide and cobalt salt is 1mg:(0.001mmol ~ 0.3mmol); The mass volume ratio of graphene oxide and ammoniacal liquor is 1mg:(0.001 ~ 0.1) mL; Wherein said ammoniacal liquor is the ammoniacal liquor of 25wt%.
2. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, it is characterized in that described ultrasonic frequency be ultrasonic power is 1000w, frequency is 30KHz.
3. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, is characterized in that the condition of the supersound washing described in step one is ultrasonic time 1 ~ 10h.
4. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, is characterized in that the speed of the high-speed stirred described in step one is 8000 ~ 15000r/min, mixing time 3 ~ 30min.
5. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, is characterized in that the cobalt salt described in step 2 is cobalt acetate, cobalt chloride, cobaltous sulfate or cobalt nitrate.
6. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, is characterized in that the reactor described in step 2 is anticorrosion high temperature high voltage resistant reactor.
7. the preparation method of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 1, it is characterized in that the temperature heated in step 2 is 90 ~ 200 DEG C, the reaction time is 2h ~ 15h.
8. the application of cobalt hydroxide/Graphene flexible electrode material that obtains of preparation method as claimed in claim 1, is characterized in that this flexible electrode material is applied in ultracapacitor.
9. the application of a kind of cobalt hydroxide/Graphene flexible electrode material according to claim 8, is characterized in that this flexible electrode material is applied to ultracapacitor as positive electrode.
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Cited By (5)
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CN106920932A (en) * | 2017-03-10 | 2017-07-04 | 上海应用技术大学 | A kind of leaf of bamboo shape Co (OH)2/ graphene combination electrode material and preparation method thereof |
CN109772179A (en) * | 2018-12-14 | 2019-05-21 | 华南理工大学 | A method of it is prepared and is formed a film using electro-deposition cobalt hydroxide nanometer sheet |
CN112185714A (en) * | 2020-10-12 | 2021-01-05 | 广西大学 | Cellulose nanofibril/carbon nanotube/cobaltosic oxide/cobalt-nickel double hydroxide flexible electrode and preparation method thereof |
CN113394028A (en) * | 2021-06-17 | 2021-09-14 | 辽宁工程技术大学 | Preparation of Co by gas phase diffusion3O4Method for compounding supercapacitor material with graphene |
CN114743800A (en) * | 2022-04-25 | 2022-07-12 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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CN106920932A (en) * | 2017-03-10 | 2017-07-04 | 上海应用技术大学 | A kind of leaf of bamboo shape Co (OH)2/ graphene combination electrode material and preparation method thereof |
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CN109772179B (en) * | 2018-12-14 | 2021-09-21 | 华南理工大学 | Method for preparing film by utilizing electrodeposition cobalt hydroxide nanosheet |
CN112185714A (en) * | 2020-10-12 | 2021-01-05 | 广西大学 | Cellulose nanofibril/carbon nanotube/cobaltosic oxide/cobalt-nickel double hydroxide flexible electrode and preparation method thereof |
CN112185714B (en) * | 2020-10-12 | 2022-01-04 | 广西大学 | Cellulose nanofibril/carbon nanotube/cobaltosic oxide/cobalt-nickel double hydroxide flexible electrode and preparation method thereof |
CN113394028A (en) * | 2021-06-17 | 2021-09-14 | 辽宁工程技术大学 | Preparation of Co by gas phase diffusion3O4Method for compounding supercapacitor material with graphene |
CN114743800A (en) * | 2022-04-25 | 2022-07-12 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
CN114743800B (en) * | 2022-04-25 | 2023-07-21 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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