CN107170589A - A kind of MnO2It is the preparation method of tri compound electrode material for super capacitor - Google Patents
A kind of MnO2It is the preparation method of tri compound electrode material for super capacitor Download PDFInfo
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- CN107170589A CN107170589A CN201710244672.0A CN201710244672A CN107170589A CN 107170589 A CN107170589 A CN 107170589A CN 201710244672 A CN201710244672 A CN 201710244672A CN 107170589 A CN107170589 A CN 107170589A
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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
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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
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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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
- H01G11/46—Metal oxides
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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
- H01G11/48—Conductive polymers
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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
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
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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
- H01G11/84—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 belongs to electrode material for super capacitor preparation field, and in particular to a kind of design preparation method of the ternary nano composite material with core nucleocapsid heterojunction structure.The cobaltosic oxide prepared using hydro-thermal method is kernel, the polyaniline of constant potential electrodeposition process electrochemical polymerization is outer core, manganese dioxide prepared by hydro-thermal method is shell, a kind of electrode material for super capacitor with good chemical property is made, the process is simple, with low cost, it is easy to control, it is environmentally safe, with good application value.
Description
Technical field
The present invention relates to a kind of preparation method of ternary nano composite material, refer in particular to cobaltosic oxide (Co3O4) it is interior
Core, polyaniline (PANI) is outer core, manganese dioxide (MnO2) prepared for the ternary nano composite material of core-nucleocapsid structure of shell.
Background technology
As energy stores/conversion equipment of environmental protection, ultracapacitor is widely used in each side of human lives
Face, also causes the research interest of numerous scholars.The key factor for determining performance of the supercapacitor is exactly the quality of electrode material, because
This, the research of electrode material is also the emphasis of ultracapacitor of the exploitation with more dominance energy.Electrode material for super capacitor master
There is transition metal oxide (RuO2、MnO2、NiO、Co3O4Deng), conducting polymer (polyaniline, polypyrrole, polythiophene etc.) with
And carbon-based material (graphene, CNT etc.) three major types.Wherein transition metal oxide has higher theoretical specific capacitance, can
To produce electric capacity by the redox reaction of Rapid reversible, energy is stored, but electric conductivity is poor to cause its actual specific capacitance
It is not high, by itself and conducting polymer, compound its electric conductivity of raising of carbon-based material, this problem can be solved well.
In the research of electrode material, the nano composite material with core shell heterojunction structure can combine different materials because of it
The advantage of material, shows good performance and attracts attention, the focus as research.In transition metal oxide, RuO2Property
Can be preferably but expensive and have pollution to environment.
The content of the invention
For problems of the prior art, the present invention has selected relatively low cost, aboundresources and free of contamination routine
Material C o3O4And MnO2, by itself and electric conductivity preferably and the polyaniline that is relatively less oxidized easily is combined, successfully devise
One seed nucleus-core-shell structure copolymer heterojunction structure.Using nickel foam as collector, Co prepared by hydro-thermal method3O4Nano-wire array as kernel, and
A part of electric capacity is provided, in Co3O4Potentiostatic electrodeposition last layer polyaniline film stores a part of electric charge as outer core on skeleton
And the effective approach of offer is quickly transmitted for electronics, material conductivity is improved, manganese dioxide is as outer made from last hydro-thermal method
Shell, further improves the capacitive property of material, so as to obtain may be used as the ternary nano composite material of electrode of super capacitor
Co3O4/PANI/MnO2。
The present invention is prepared for a kind of cobaltosic oxide prepared using hydro-thermal method as kernel, and constant potential electrodeposition process electrochemistry is gathered
The polyaniline of conjunction is outer core, and manganese dioxide prepared by hydro-thermal method is the ternary nano composite wood with core-nucleocapsid structure of shell
Material, method is simple, and cost is relatively low, and chemical property is good, is a kind of good electrode material for super capacitor.
Technical scheme is as follows：
A kind of ternary nano composite material Co as electrode of super capacitor3O4/PANI/MnO2Preparation method, specifically
Comprise the following steps：
(1) Co is grown in nickel foam3O4It is used as kernel：
Using nickel foam as substrate, it is dipped in precursor solution, is placed in reactor and carries out hydro-thermal reaction, hydro-thermal reaction
After end；Product is ultrasonic in deionized water, then deionized water, alcohol flushing are used respectively, dry, calcined in Muffle furnace；
Obtain with Co3O4Nickel foam；
The precursor solution be cobalt nitrate hexahydrate, ammonium fluoride, urea and a certain amount of surfactant be dissolved in from
The mixed liquor of sub- water composition；
Cobalt nitrate hexahydrate, ammonium fluoride, the ratio of the substance withdrawl syndrome of urea are 1 in the precursor solution：2：5, it is used
Surfactant is cetyl trimethylammonium bromide (CTAB), surfactant qualities used：The volume of deionized water is
0.15g：30mL.
(2) by step (1) obtain with Co3O4Nickel foam, be dipped in the deposition liquid being made up of dilute sulfuric acid and aniline,
One layer of polyaniline film of electrochemical deposition is as outer core at room temperature, and product is rinsed with water, is obtained with Co3O4And polyaniline film
Nickel foam；
(3) by step (2) obtain with Co3O4Nickel foam with polyaniline film is substrate, is dipped in liquor potassic permanganate
In, it is placed in reactor and carries out hydro-thermal reaction, prepares MnO2Shell, after hydro-thermal reaction terminates；Product is surpassed in deionized water
Sound, then deionized water, alcohol flushing, drying for standby are used respectively.
In step (1), the temperature of the hydro-thermal reaction is 120 DEG C, and the time is 10h；The product surpasses in deionized water
Sound 1min；The drying temperature is 60 DEG C；The calcining heat is 350 DEG C, calcination time 3h.
In step (2), the composition of the deposition liquid of the electrochemical deposition polyaniline contains 0.25M sulfuric acid and 0.1M aniline；
The electrochemical deposition sedimentation time 120~300s, 0.6~1.0V of sedimentation potential；
In step (3), liquor potassic permanganate concentration used is 0.02M；The temperature of the hydro-thermal reaction is 120 DEG C, hydro-thermal
Reaction time is 4h；By product ultrasound 1min in deionized water, drying temperature is 60 DEG C.
Beneficial effects of the present invention are：
(1) present invention is using nickel foam as substrate, and design has prepared one kind with Co made from hydro-thermal method3O4Nano-wire array
For kernel, the polyaniline film of electrochemical deposition is outer core, MnO made from hydro-thermal method2For core-core-shell structure copolymer heterojunction structure of shell,
Electro-chemical test is carried out to it, good capacitive property, high rate performance and stable circulation performance is shown, is a kind of super well
Level capacitor electrode material.
(2) preparation method that the present invention is provided is simple, and cost is relatively low.
Brief description of the drawings
Fig. 1：A is electronic scanner microscope (SEM) figure of step 1 in embodiment 1~4, and b is step 2 in embodiment 2
SEM schemes, and c, d are the SEM figures of the different enlargement ratios of step 3 in embodiment 2.
Fig. 2 is transmission electron microscope (TEM) figure of step 3 in embodiment 2.
Embodiment
With reference to specific implementation example, the present invention will be further described, so that those skilled in the art more fully understand
The present invention, but the invention is not limited in following examples.
Embodiment 1
1st, using nickel foam as substrate, by cobalt nitrate hexahydrate, ammonium fluoride, urea according to substance withdrawl syndrome 1:2:5 ratio
It is dissolved in 30mL deionized waters, and adds 0.15g CTAB, is configured to precursor solution, in 120 DEG C of hydro-thermal reaction 10h, from
Room temperature so is cooled to, by product ultrasound 1min, then use deionized water, alcohol flushing respectively in deionized water, after 60 DEG C of dryings,
3h is calcined at 350 DEG C.Its SEM as shown in Figure 1a, aoxidizes the average diameter 50-80nm of cobalt nanowire, surface light
It is sliding, kernel can be used as.
2nd, with Co3O4Nickel foam be working electrode, platinum electrode is used as ginseng as auxiliary electrode, saturated calomel electrode
Than electrode, in the deposition liquid containing 0.25M sulfuric acid and 0.1M aniline, electrochemical deposition polyaniline film, sedimentation potential 0.6V,
Sedimentation time 300s, deionized water and alcohol flushing are used by product respectively.
3rd, will be with Co3O4It is molten that the nickel foam of nano wire and polyaniline film is put into the potassium permanganate that 25mL concentration is 0.02M
In liquid, in 120 DEG C of hydro-thermal reaction 4h, by product ultrasound 1min in deionized water, then deionized water, alcohol flushing are used respectively,
60 DEG C of dryings.
Embodiment 2
1st, using nickel foam as substrate, by cobalt nitrate hexahydrate, ammonium fluoride, urea according to substance withdrawl syndrome 1:2:5 ratio
It is dissolved in 30mL deionized waters, and adds 0.15g CTAB, is configured to precursor solution, in 120 DEG C of hydro-thermal reaction 10h, from
Room temperature so is cooled to, by product ultrasound 1min, then use deionized water, alcohol flushing respectively in deionized water, after 60 DEG C of dryings,
3h is calcined at 350 DEG C.Its SEM is as shown in Figure 1a.
2nd, with Co3O4Nickel foam be working electrode, platinum electrode is used as ginseng as auxiliary electrode, saturated calomel electrode
Than electrode, in the deposition liquid containing 0.25M sulfuric acid and 0.1M aniline, electrochemical deposition polyaniline film, sedimentation potential 0.8V,
Sedimentation time 240s, deionized water and alcohol flushing are used by product respectively.Its SEM is as shown in Figure 1 b.Electrochemistry
After deposition, the nanowire diameter layer of transparent shape film that become big, many, illustrates that polyaniline outer core is deposited successfully in figure, but it does not have table
Face form does not have significant change.
3rd, will be with Co3O4It is molten that the nickel foam of nano wire and polyaniline film is put into the potassium permanganate that 25mL concentration is 0.02M
In liquid, in 120 DEG C of hydro-thermal reaction 4h, by product ultrasound 1min in deionized water, then deionized water, alcohol flushing are used respectively,
60 DEG C of dryings.Its SEM flower ball-shaped material as shown in Fig. 1 c, d is generated on nano wire, is illustrated outside manganese dioxide
Shell is successfully prepared, and its transmission electron microscope shows core-core-shell structure copolymer knot as shown in Fig. 2 consistent with SEM result
Structure design is successfully prepared.
Embodiment 3
1st, using nickel foam as substrate, by cobalt nitrate hexahydrate, ammonium fluoride, urea according to substance withdrawl syndrome 1:2:5 ratio
It is dissolved in 30mL deionized waters, and adds 0.15g CTAB, is configured to precursor solution, in 120 DEG C of hydro-thermal reaction 10h, from
Room temperature so is cooled to, by product ultrasound 1min, then use deionized water, alcohol flushing respectively in deionized water, after 60 DEG C of dryings,
3h is calcined at 350 DEG C.Its SEM is as shown in Figure 1a.
2nd, with Co3O4Nickel foam be working electrode, platinum electrode is used as ginseng as auxiliary electrode, saturated calomel electrode
Than electrode, in the deposition liquid containing 0.25M sulfuric acid and 0.1M aniline, electrochemical deposition polyaniline film, sedimentation potential 1.0V,
Sedimentation time 240s, deionized water and alcohol flushing are used by product respectively.
3rd, will be with Co3O4It is molten that the nickel foam of nano wire and polyaniline film is put into the potassium permanganate that 25mL concentration is 0.02M
In liquid, in 120 DEG C of hydro-thermal reaction 4h, by product ultrasound 1min in deionized water, then deionized water, alcohol flushing are used respectively,
60 DEG C of dryings.
Embodiment 4
1st, using nickel foam as substrate, by cobalt nitrate hexahydrate, ammonium fluoride, urea according to substance withdrawl syndrome 1:2:5 ratio
It is dissolved in 30mL deionized waters, and adds 0.15g CTAB, is configured to precursor solution, in 120 DEG C of hydro-thermal reaction 10h, from
Room temperature so is cooled to, by product ultrasound 1min, then use deionized water, alcohol flushing respectively in deionized water, after 60 DEG C of dryings,
3h is calcined at 350 DEG C.Its SEM is as shown in Figure 1a.
2nd, with Co3O4Nickel foam be working electrode, platinum electrode is used as ginseng as auxiliary electrode, saturated calomel electrode
Than electrode, in the deposition liquid containing 0.25M sulfuric acid and 0.1M aniline, electrochemical deposition polyaniline film, sedimentation potential 1.0V,
Sedimentation time 120s, deionized water and alcohol flushing are used by product respectively.
3rd, will be with Co3O4It is molten that the nickel foam of nano wire and polyaniline film is put into the potassium permanganate that 25mL concentration is 0.02M
In liquid, in 120 DEG C of hydro-thermal reaction 4h, by product ultrasound 1min in deionized water, then deionized water, alcohol flushing are used respectively,
60 DEG C of dryings.
Claims (5)
1. a kind of MnO2It is the preparation method of tri compound electrode material for super capacitor, it is characterised in that use hydro-thermal method and perseverance
Current potential electrodeposition process prepares the ternary nano composite material with core-core-shell structure copolymer heterojunction structure, specifically includes following steps：
(1) Co is grown in nickel foam3O4It is used as kernel：
Using nickel foam as substrate, it is dipped in precursor solution, is placed in reactor and carries out hydro-thermal reaction, hydro-thermal reaction terminates
Afterwards；Product is ultrasonic in deionized water, then deionized water, alcohol flushing are used respectively, dry, calcined in Muffle furnace；Obtain
With Co3O4Nickel foam；
The precursor solution is that cobalt nitrate hexahydrate, ammonium fluoride, urea and a certain amount of surfactant are dissolved in deionized water
The mixed liquor of composition；
(2) by step (1) obtain with Co3O4Nickel foam, be dipped in the deposition liquid being made up of dilute sulfuric acid and aniline, room temperature
Lower one layer of polyaniline film of electrochemical deposition is as outer core, and product is rinsed with water, is obtained with Co3O4With the bubble of polyaniline film
Foam nickel；
(3) by step (2) obtain with Co3O4Nickel foam with polyaniline film is substrate, is dipped in liquor potassic permanganate,
It is placed in reactor and carries out hydro-thermal reaction, prepares MnO2Shell, after hydro-thermal reaction terminates；Product is ultrasonic in deionized water,
Use deionized water, alcohol flushing, drying for standby respectively again.
2. MnO according to claim 12It is the preparation method of tri compound electrode material for super capacitor, its feature exists
In in step (1), the temperature of the hydro-thermal reaction is 120 DEG C, and the time is 10h；The product is ultrasonic in deionized water
1min；The drying temperature is 60 DEG C；The calcining heat is 350 DEG C, calcination time 3h.
3. MnO according to claim 12It is the preparation method of tri compound electrode material for super capacitor, its feature exists
In cobalt nitrate hexahydrate, ammonium fluoride, the ratio of the substance withdrawl syndrome of urea are 1 in the precursor solution：2：5, surface used is lived
Property agent be cetyl trimethylammonium bromide (CTAB), surfactant qualities used：The volume of deionized water is 0.15g：
30mL。
4. MnO according to claim 12It is the preparation method of tri compound electrode material for super capacitor, its feature exists
In in step (2), the composition of the deposition liquid of the electrochemical deposition polyaniline contains 0.25M sulfuric acid and 0.1M aniline；The electricity
Chemical deposition 120~300s of sedimentation time, 0.6~1.0V of sedimentation potential.
5. MnO according to claim 12It is the preparation method of tri compound electrode material for super capacitor, its feature exists
In in step (3), liquor potassic permanganate concentration used is 0.02M；The temperature of the hydro-thermal reaction is 120 DEG C, during hydro-thermal reaction
Between be 4h；By product ultrasound 1min in deionized water, drying temperature is 60 DEG C.
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Cited By (6)
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| CN110136993A (en) * | 2019-05-08 | 2019-08-16 | 武汉大学 | A method of super capacitor electrode slice is prepared using hydro-thermal method |
| CN110797201A (en) * | 2018-08-01 | 2020-02-14 | 天津大学 | Polyaniline-manganese dioxide composite material, preparation method thereof and application thereof in electrochemical energy storage field |
| CN110970228A (en) * | 2018-09-30 | 2020-04-07 | 天津大学 | Asymmetric super capacitor |
| CN111009422A (en) * | 2019-12-10 | 2020-04-14 | 中北大学 | Nickel-based NiCo with core-shell structure2O4Preparation method of polyaniline nano material |
| CN111986929A (en) * | 2020-07-31 | 2020-11-24 | 江苏大学 | Preparation method of cobalt manganate/nickel sulfide core-shell array structure electrode material |
| CN112216528A (en) * | 2020-10-12 | 2021-01-12 | 多助科技(武汉)有限公司 | Method for preparing electrode plate of high-voltage water-system supercapacitor by hydrothermal method |
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| CN111009422A (en) * | 2019-12-10 | 2020-04-14 | 中北大学 | Nickel-based NiCo with core-shell structure2O4Preparation method of polyaniline nano material |
| CN111986929A (en) * | 2020-07-31 | 2020-11-24 | 江苏大学 | Preparation method of cobalt manganate/nickel sulfide core-shell array structure electrode material |
| CN112216528A (en) * | 2020-10-12 | 2021-01-12 | 多助科技(武汉)有限公司 | Method for preparing electrode plate of high-voltage water-system supercapacitor by hydrothermal method |
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| CN107170589B (en) | 2018-10-09 |
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