CN107275107A - A kind of combination electrode material and Preparation method and use - Google Patents
A kind of combination electrode material and Preparation method and use Download PDFInfo
- Publication number
- CN107275107A CN107275107A CN201710356070.4A CN201710356070A CN107275107A CN 107275107 A CN107275107 A CN 107275107A CN 201710356070 A CN201710356070 A CN 201710356070A CN 107275107 A CN107275107 A CN 107275107A
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- Prior art keywords
- combination electrode
- electrode material
- feco
- carbon cloth
- hydro
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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
- H01G11/30—Electrodes characterised by their material
-
- 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
- H01G11/46—Metal oxides
-
- 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
-
- 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 present invention relates to a kind of combination electrode material and Preparation method and use.Ferrous sulfate, cabaltous nitrate hexahydrate, urea and the ammonium fluoride solution soluble in water that is configured to are mixed, then insert carbon cloth, after first time hydro-thermal reaction terminates, washs, dry, obtain loading FeCo2O4The carbon cloth of predecessor；The above-mentioned carbon cloth for loading predecessor is inserted in liquor potassic permanganate again, after second of hydro-thermal reaction terminates, washing, dry, calcining have produced in load FeCo2O4@MnO2The carbon cloth of combination electrode material.Ternary metal oxide FeCo2O4With higher electric conductivity, surface-active site is not only increased as skeleton, and be the MnO for being grown in its surface2There is provided the connection of effective electronics, MnO is greatly solved2The problem of electric conductivity is low, and this combination electrode material as positive electrode when be prepared into Asymmetric Supercapacitor, with higher power density and energy density.
Description
Technical field
The invention belongs to metal oxide nano-material synthesis technical field, refer in particular to close using simple and quick hydrothermal method
Into a kind of FeCo2O4@MnO2Combination electrode material, FeCo is prepared into using it2O4@MnO2//AC Asymmetric Supercapacitors
(ASC), can lightening LED lamp bubble.
Background technology
Since the new century, with the continuous consumption of the non-renewable energy resources such as coal, oil and natural gas, fossil fuel combustion
The environmental problem such as greenhouse effects becomes increasingly conspicuous caused by burning, the aggravation of contradictions between economic development and energy resource supply, so in order to
Improve the ecological environment, realize the sustainable development of society, it is to solve renewable energy power generation to enter to develop efficient energy storage device
The effective way of net problem, it is considered to be the strategic technology of support Renewable Energy Development, has obtained national governments and enterprise
The extensive concern on boundary.
Carbon cloth has the advantages that simple cheap, preparation technology, high conductivity and chemical property are stable, is a kind of preferable
Electrode base material；It is the development side of following flexible electrode and flexible electronic devices and its flexible, mechanical performance is high
To.
Cobalt acid iron (FeCo2O4) it is a kind of ternary metal oxide electrode material, its specific capacitance is far longer than absorbent charcoal material
The electric double layer capacitance on surface, and there is the features such as good electric conductivity and easy preparation.
Manganese dioxide (MnO2) it is binary metal oxide material that is a kind of critically important and being widely used, it is inexpensive low
Poison, and with high fake capacitance and it is environment-friendly the features such as, be prepared into nanostructured, not only with specific surface area it is high,
The characteristics of cation and short electric transmission path, and the impact of crooked pressure can be slowed down so that MnO2It can apply to soft
Property energy storage electrode material.
The content of the invention
Present invention aims at provide a kind of simple FeCo2O4@MnO2The synthetic method of combination electrode material.
The present invention is realized by following steps：
(1) by ferrous sulfate (FeSO4·7H2O), cabaltous nitrate hexahydrate (Co9 (NO3)2·6H2O), urea (CO (NH2)2)
With ammonium fluoride (NH4F it is) soluble in water to be configured to solution mixing, then carbon cloth is inserted, after first time hydro-thermal reaction terminates, wash
Wash, dry, obtain loading FeCo2O4The carbon cloth of predecessor；The above-mentioned carbon cloth for loading predecessor is inserted into liquor potassic permanganate again
In, after second of hydro-thermal reaction terminates, washing, dry, calcining have produced in load FeCo2O4@MnO2The carbon of combination electrode material
Cloth.
The ratio between described ferrous sulfate, cabaltous nitrate hexahydrate, amount of material of urea and ammonium fluoride are：1:2:5:2.
The concentration of the liquor potassic permanganate is 0.05M.
The condition of the first time hydro-thermal reaction is：Hydro-thermal reaction 7h under conditions of 140 DEG C.
The condition of second of hydro-thermal reaction is：Hydro-thermal reaction 6h under conditions of 140 DEG C.
The calcination condition is：2h is calcined under conditions of 400 DEG C.
(2) using instruments such as X-ray diffractometer (XRD), transmission electron microscope (TEM), x-ray photoelectron spectroscopy instrument to product
Structural analysis is carried out, the research of chemical property is carried out to product using CHI 760E types electrochemical workstations.
(4) when the combination electrode material prepared using the present invention is as positive pole, using activated carbon (AC) as negative pole, system
It is standby into Asymmetric Supercapacitor (ASC) when, two above-mentioned ASC of series connection charge 40s under conditions of 3.2V, can point
Bright LED bulb.
FeCo prepared by the present invention2O4@MnO2Combination electrode material, ternary metal oxide FeCo2O4With higher
Electric conductivity, not only increases surface-active site, and be the MnO for being grown in its surface as skeleton2There is provided effective electricity
Son connection, greatly solves MnO to a certain extent2The problem of electric conductivity is low, and this combination electrode material is used as positive pole
When material is prepared into Asymmetric Supercapacitor, with higher power density and energy density, therefore the composite
There are certain potentiality in energy storage field.
Beneficial effect
Utilize the FeCo prepared by simple hydrothermal synthesis method2O4@MnO2Combination electrode material be ultracapacitor just
Pole, the advantages of material has good charge-discharge characteristic, preferable cycle performance.Present invention process is simple, and repeatability is high, and
The inexpensive low toxicity of material therefor, the reaction time is shorter, so as to reduce the cost of energy consumption and reaction, is easy to a large amount of productions, prepares
Asymmetric Supercapacitor can Reusability, circulation 5000 times after, still with 90.1% capability retention, meet ring
The friendly requirement in border.
Brief description of the drawings
Fig. 1 is FeCo2O4@MnO2X-ray diffraction analysis figure (XRD) figure of combination electrode.
Fig. 2 is FeCo2O4With FeCo2O4@MnO2ESEM (SEM) figure of combination electrode.
Fig. 3 is FeCo2O4@MnO2The sign of chemical property of the combination electrode in two electrode systems.Fig. 3 (a) is
FeCo2O4@MnO2Three is compressed together by combination electrode as positive pole, activated carbon (AC) as negative pole, filter paper as barrier film
It is prepared into FeCo2O4@MnO2The rough schematic of //AC Asymmetric Supercapacitors, Fig. 3 (b) is FeCo2O4@MnO2Combination electrode
Cyclic voltammetry (CV) curve map of different scanning rates in 1.6V electrochemical window, Fig. 3 (c) is FeCo2O4@MnO2Compound electric
Pole is under 1.6V voltage, crossing current discharge and recharge (GCD) curve map under different current densities, and Fig. 3 (d) is the asymmetric super electricity
Container is in 25mA cm-2Current density under circulate 5000 times, still can with 90.1% capability retention figure.Built-in figure
For by two FeCo2O4@MnO2//AC Asymmetric Supercapacitors are chained together, under 3.2V voltage, use CHI 760E
The picture for the white bulbs of a LED that type electrochemical workstation charging 40s can be lighted.
Embodiment
Embodiment 1FeCo2O4@MnO2The preparation of combination electrode material
(1) carbon cloth is cut out into appropriately sized (1 × 1cm), and according to acetone, ethanol, the order of water cleans carbon cloth to remove carbon
The greasy dirt on cloth surface.
(2) by 1mmol ferrous sulfate (ferrous sulfate 7H2O), 2mmol cabaltous nitrate hexahydrates (Co (NO3)2·6H2O)、
5mmol urea (CO (NH2)2) and 2mmol ammonium fluorides (NH4F) be dissolved in 30ml deionized waters, stirring 30min after, then with it is upper
State the carbon cloth cleaned up to be transferred in the lump in the reactor of 50ml polytetrafluoroethyllining linings, constant temperature at a temperature of being warming up to 140 DEG C
7h, natural cooling takes out carbon cloth, is washed, dried with distillation water-ethanol.
(3) configuration 30mL 0.05M potassium permanganate (KMnO4) solution.
(4) solution configured in carbon cloth resulting in above-mentioned (2) and (3) is inserted into 50ml polytetrafluoroethyllining linings
In reactor, constant temperature 6h at a temperature of being warming up to 140 DEG C, natural cooling washs drying.
(5) carbon cloth obtained above is inserted in Muffle furnace, 400 DEG C of calcining 2h, obtains being grown in the FeCo on carbon cloth2O4@
MnO2Combination electrode.
It is a further object of the invention to provide prepared FeCo2O4@MnO2Combination electrode steeps for lightening LED lamp
Using.
Cobalt acid iron (FeCo2O4)@manganese dioxide (MnO2) combination electrode performance of the supercapacitor testing procedure it is as follows：
Activated carbon (AC), acetylene black, polytetrafluoroethylene (PTFE) (PVDF) are compared 8 with mass fraction first：1：1 ratio mixing is equal
It is even, with 1-METHYLPYRROLIDONE solution dissolve above-mentioned powder, and above-mentioned well mixed powder is applied to a piece of clean up
In (1 × 1cm) nickel foam, then this nickel foam dried.This FeCo2O4@MnO2Combination electrode is above-mentioned to scribble work as positive pole
Property the mixed-powder such as charcoal nickel foam as negative pole, 3M KOH are as electrolyte, with CHI 760E type electrochemical workstations, carry out
Cyclic voltammetry scanning and the test of crossing current discharge and recharge.Above-mentioned both positive and negative polarity is used into filter paper interval again, system in lithium battery case is compressed in
It is standby into an easy FeCo2O4@MnO2//AC Asymmetric Supercapacitors.Two FeCo2O4@MnO2The asymmetric super electricity of //AC
Container is chained together, using electrochemical workstation, and charging can light a white LED for 40s seconds under 3.2V voltage
Bulb.
Embodiment 2FeCo2O4@MnO2The phenetic analysis of combination electrode material
The thing phase of combination electrode in the present invention, structure and performance characterization are by x-ray diffractometer, Flied emission scanning electricity
Mirror (SEM) and CHI 760E types electrochemical workstation are determined.
As shown in figure 1, as can be seen from the figure FeCo2O4, MnO2Two kinds of materials are successfully synthesized.
As shown in Fig. 2 it can be seen that FeCo from figure (a)2O4It is the structure of nanometer sheet, it can be seen that MnO from figure (b)2
Small nanometer sheet is successfully grown in FeCo2O4The surface of nanometer sheet, forms a kind of core shell structure.
Embodiment 3FeCo2O4The analysis of the chemical property of@MnO2 combination electrode materials and its practical application
As shown in figure 3, as can be seen from the figure when using FeCo2O4@MnO2This composite is positive pole, and AC is as negative
Pole, when being fabricated to Asymmetric Supercapacitor (ASC), with electrochemical properties such as preferable discharge and recharges.Series connection two is above-mentioned
ASC, the 40s that charged under 3.2V voltage can successfully light White LED bulb.
Claims (7)
1. a kind of combination electrode material, it is characterised in that preparation method is as follows：By ferrous sulfate (FeSO4·7H2O), six hydration
Cobalt nitrate (Co9 (NO3)2·6H2O), urea (CO (NH2)2) and ammonium fluoride (NH4It is F) soluble in water to be configured to solution mixing,
Carbon cloth is inserted again, after first time hydro-thermal reaction terminates, washs, dry, and obtains loading FeCo2O4The carbon cloth of predecessor；Again will be above-mentioned
The carbon cloth for loading predecessor is inserted in liquor potassic permanganate, after second of hydro-thermal reaction terminates, and washing, dry, calcining are produced
It is supported on the FeCo on carbon cloth2O4@MnO2Combination electrode material.
2. a kind of combination electrode material as claimed in claim 1, it is characterised in that described ferrous sulfate, six nitric hydrates
The ratio between amount of material of cobalt, urea and ammonium fluoride is：1:2:5:2.
3. a kind of combination electrode material as claimed in claim 1, it is characterised in that the concentration of the liquor potassic permanganate is
0.05M。
4. a kind of combination electrode material as claimed in claim 1, it is characterised in that the condition of the first time hydro-thermal reaction
For：Hydro-thermal reaction 7h under conditions of 140 DEG C.
5. a kind of combination electrode material as claimed in claim 1, it is characterised in that the condition of second of hydro-thermal reaction
For：Hydro-thermal reaction 6h under conditions of 140 DEG C.
6. a kind of combination electrode material as claimed in claim 1, it is characterised in that the calcination condition is：400 DEG C of condition
Lower calcining 2h.
7., using activated carbon (AC) as negative pole, it is prepared into as positive pole using combination electrode material as claimed in claim 1
When one Asymmetric Supercapacitor (ASC), two above-mentioned ASC of series connection charge 40s under conditions of 3.2V, can light
LED bulb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710356070.4A CN107275107A (en) | 2017-05-16 | 2017-05-16 | A kind of combination electrode material and Preparation method and use |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710356070.4A CN107275107A (en) | 2017-05-16 | 2017-05-16 | A kind of combination electrode material and Preparation method and use |
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| Publication Number | Publication Date |
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| CN107275107A true CN107275107A (en) | 2017-10-20 |
Family
ID=60065337
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| CN201710356070.4A Pending CN107275107A (en) | 2017-05-16 | 2017-05-16 | A kind of combination electrode material and Preparation method and use |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108364804A (en) * | 2018-02-08 | 2018-08-03 | 吉林加合安高能电容有限公司 | A kind of solid state battery anode production processes and application |
| CN108831751A (en) * | 2018-06-13 | 2018-11-16 | 安徽理工大学 | One kind is with FeCo2O4For the Micron-nano composites and its preparation method and application of substrate |
| CN109179406A (en) * | 2018-10-23 | 2019-01-11 | 西安交通大学 | A kind of coal slime activation prepares the method for active carbon and its application in supercapacitor |
| CN109637824A (en) * | 2018-11-27 | 2019-04-16 | 山东大学 | A kind of New Co Fe for supercapacitor2S4Nanometer sheet/nickel foam composite material and preparation method |
| CN109659147A (en) * | 2018-12-19 | 2019-04-19 | 哈尔滨师范大学 | One kind preparing FeCo based on foam nickel base2S4The method of nano-chip arrays |
| CN109712818A (en) * | 2019-01-04 | 2019-05-03 | 内蒙古大学 | A kind of manganese-base oxide composite and flexible electrode material and preparation method thereof |
| CN109950508A (en) * | 2019-04-08 | 2019-06-28 | 朱焕光 | A kind of carbon cloth flexible lithium ion battery negative electrode material and preparation method thereof |
| CN109943187A (en) * | 2019-02-20 | 2019-06-28 | 常州凯奥机电科技有限公司 | A kind of composite heat resistance salt tolerant enamel |
| CN110818031A (en) * | 2019-10-31 | 2020-02-21 | 燕山大学 | Preparation method of composite metal oxide functional electrode |
| CN113113612A (en) * | 2021-04-08 | 2021-07-13 | 福州大学 | Cationic group carbon cloth current collector and preparation method thereof |
| CN113690059A (en) * | 2021-08-19 | 2021-11-23 | 辽宁大学 | FeCo2O4// AC water system asymmetric photo-assisted supercapacitor and preparation method thereof |
| CN114525551A (en) * | 2022-03-24 | 2022-05-24 | 湖南祯晟炭素实业有限公司 | Preparation method of carbon composite material for aluminum electrolysis cell cathode integrated molding |
| CN115445619A (en) * | 2022-08-30 | 2022-12-09 | 湖南工商大学 | Preparation method of iron-doped cobaltosic oxide electrode and arsenic-polluted water body treatment method |
-
2017
- 2017-05-16 CN CN201710356070.4A patent/CN107275107A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| KAIBING XU: "Hierarchical mesoporous NiCo2O4@MnO2 core shell nanowire arrays on nickel foam for aqueous asymmetric supercapacitors", 《ELECTROCHIMICA ACTA》 * |
| LIANG HUANG: "Hierarchical core-shell NiCo2O4@NiMoO4 nanowires grown on carbon cloth as integrated electrode for high-performance supercapacitors", 《SCIENTIFIC REPORTS》 * |
| LIANG HUANG: "Hierarchical NiCo2O4@MnO2 core–shell heterostructured nanowire arrays on Ni foam as high-performance supercapacitor electrodes", 《CHEMCOMM》 * |
| LIYANG LIN: "Hierarchical three-dimensional FeCo2O4@MnO2 core-shell nanosheet arrays on nickel foam for high-performance supercapacitor", 《ELECTROCHIMICA ACTA》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108364804A (en) * | 2018-02-08 | 2018-08-03 | 吉林加合安高能电容有限公司 | A kind of solid state battery anode production processes and application |
| CN108831751A (en) * | 2018-06-13 | 2018-11-16 | 安徽理工大学 | One kind is with FeCo2O4For the Micron-nano composites and its preparation method and application of substrate |
| CN109179406A (en) * | 2018-10-23 | 2019-01-11 | 西安交通大学 | A kind of coal slime activation prepares the method for active carbon and its application in supercapacitor |
| CN109637824A (en) * | 2018-11-27 | 2019-04-16 | 山东大学 | A kind of New Co Fe for supercapacitor2S4Nanometer sheet/nickel foam composite material and preparation method |
| CN109659147A (en) * | 2018-12-19 | 2019-04-19 | 哈尔滨师范大学 | One kind preparing FeCo based on foam nickel base2S4The method of nano-chip arrays |
| CN109712818A (en) * | 2019-01-04 | 2019-05-03 | 内蒙古大学 | A kind of manganese-base oxide composite and flexible electrode material and preparation method thereof |
| CN109943187A (en) * | 2019-02-20 | 2019-06-28 | 常州凯奥机电科技有限公司 | A kind of composite heat resistance salt tolerant enamel |
| CN109950508A (en) * | 2019-04-08 | 2019-06-28 | 朱焕光 | A kind of carbon cloth flexible lithium ion battery negative electrode material and preparation method thereof |
| CN110818031A (en) * | 2019-10-31 | 2020-02-21 | 燕山大学 | Preparation method of composite metal oxide functional electrode |
| CN113113612A (en) * | 2021-04-08 | 2021-07-13 | 福州大学 | Cationic group carbon cloth current collector and preparation method thereof |
| CN113113612B (en) * | 2021-04-08 | 2022-09-23 | 福州大学 | Cationic group carbon cloth current collector and preparation method thereof |
| CN113690059A (en) * | 2021-08-19 | 2021-11-23 | 辽宁大学 | FeCo2O4// AC water system asymmetric photo-assisted supercapacitor and preparation method thereof |
| CN113690059B (en) * | 2021-08-19 | 2023-01-17 | 辽宁大学 | FeCo 2 O 4 // AC water system asymmetric photo-assisted supercapacitor and preparation method thereof |
| CN114525551A (en) * | 2022-03-24 | 2022-05-24 | 湖南祯晟炭素实业有限公司 | Preparation method of carbon composite material for aluminum electrolysis cell cathode integrated molding |
| CN114525551B (en) * | 2022-03-24 | 2022-10-11 | 湖南祯晟炭素实业有限公司 | Preparation method of carbon composite material for aluminum electrolysis cell cathode integrated molding |
| CN115445619A (en) * | 2022-08-30 | 2022-12-09 | 湖南工商大学 | Preparation method of iron-doped cobaltosic oxide electrode and arsenic-polluted water body treatment method |
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Application publication date: 20171020 |