CN103107025A - Preparation method of supercapacitor electrode material NiCo2O4 - Google Patents
Preparation method of supercapacitor electrode material NiCo2O4 Download PDFInfo
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- CN103107025A CN103107025A CN2013100589115A CN201310058911A CN103107025A CN 103107025 A CN103107025 A CN 103107025A CN 2013100589115 A CN2013100589115 A CN 2013100589115A CN 201310058911 A CN201310058911 A CN 201310058911A CN 103107025 A CN103107025 A CN 103107025A
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- 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 of supercapacitor electrode material NiCo2O4. The preparation method comprises: (1) hexahydrated nickel nitrate Ni (NO3) 2 6H2O, hexahydrated cobalt nitrate Co (NO3) 2 6H2O and ureophil in a molar ratio of 1:2:1-10 are added to a mixed solution of ethanol and water, stirred and dissolved so as to obtain a mixed solution; and (2) a hydrothermal reaction is conducted to the mixed solution, the reaction temperature is from 90 DEG C and 200 DEG C, the reaction time is from 3h to 48 h, the mixed solution is cooled to the room temperature so as to obtain the NiCo2O4 by centrifuging, and then the NiCo2O4 is washed, dried and calcined so that the material NiCo2O4 is obtained. The materials obtained through the preparation method are high in specific capacitance and good in electrochemical stability and are excellent supercapacitor electrode materials. The preparation method has the advantages of being simple, green and environment-friendly and low in cost.
Description
Technical field
The invention belongs to the preparation field of electrode material, particularly a kind of electrode material for super capacitor NiCo
2O
4The preparation method.
Background technology
The energy is the material base of human survival and development, and facing mankind serious energy scarcity at present.Day by day serious along with the continuous consumption of the fast development of global economy, fossil energy, environmental pollution studied a kind of efficient, low cost, environmental friendliness, high performance energy conversion and stocking system and seemed more and more important.Electrochemical capacitor also claims ultracapacitor, it is a kind of capacitor more excellent than traditional capacitor on performance, large one more than the order of magnitude of the energy Ratios traditional physical capacitor that can store due to this novel energy device, have again simultaneously the advantages such as power density is high, the charging interval is short, long service life, be widely used in fields such as automobile, electric power, railway, communication, national defence, consumer electronics products, thereby caused the extensive concern of researcher.
Electrochemical capacitor can be divided into two classes according to charge storage mechanism: a class is electrochemical capacitor in double electrode layer, and the electrode material of such capacitor is mainly material with carbon element; Another kind of is the Faraday pseudo-capacitance device, and the electrode material of such capacitor is mainly transition metal oxide.Material with carbon element has that high-specific surface area, cost are low, the advantage such as have extended cycle life, but it is than the low business development that seriously limits the carbon-based electrode material of electric capacity; Therefore transition metal oxide is considered to optimal electrode material owing to having high ratio electric capacity and excellent cyclic reversibility.Cobalt acid nickel (NiCo
2O
4) because tool conducts electricity very well, low cost, controlled surface and structural behaviour, environmental friendliness the most important thing is, NiCo
2O
4Have very high theory than electric capacity, these advantages make NiCo
2O
4Become a kind of ideal electrode material that can satisfy practical application.Till research in front, prepared the NiCo of multiple different-shape and structure
2O
4Electrode material, but the ratio electric capacity that obtains is all smaller.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of electrode material for super capacitor NiCo
2O
4The preparation method, the method can significantly improve NiCo
2O
4Ratio electric capacity and the cyclical stability of electrode material simultaneously can be simple, fast, prepare on a large scale this material and satisfy practical application.
A kind of electrode material for super capacitor NiCo of the present invention
2O
4The preparation method, comprising:
(1) with mol ratio be the Nickelous nitrate hexahydrate Ni (NO of 1:2:1-10
3)
26H
2O, cabaltous nitrate hexahydrate Co (NO
3)
26H
2O and urea add in the mixed solution of second alcohol and water, and stirring and dissolving obtains mixed solution;
(2) above-mentioned mixed solution carries out hydro-thermal reaction, and reaction temperature is 90-200 ℃, and the reaction time is 3-48h, is cooled to room temperature, the centrifugal NiCo that obtains
2O
4, then washing, dry, calcining namely get electrode material for super capacitor.
In described step (1), in the mixed solution of second alcohol and water, volume ratio is 0-1: 1.
In described step (2), hydro-thermal reaction is carried out in the 60mL hydrothermal reaction kettle, and the reactor compactedness is 80%.
In described step (2), washing is for washing with deionized water and ethanol respectively.
In described step (2), calcining heat is 200-400 ℃, and calcination time is 20-500min.
Electrode material for super capacitor NiCo in described step (2)
2O
4To connect into line by single nano particle to be self-assembled into spherical structure.
Beneficial effect
(1) NiCo for preparing of method of the present invention
2O
4Electrode material is that single nano particle connects into line and is self-assembled into spherical structure, not only has than high specific capacitance, has simultaneously good electrochemical stability, is a kind of good electrode material for super capacitor;
(2) NiCo of the present invention
2O
4Simple, the environmental protection of preparation method, cost low, solved NiCo
2O
4The problem of the large-scale application difficulty in the ultracapacitor industry.
Description of drawings
Fig. 1 is the NiCo of embodiment 1 preparation
2O
4Electrode material low power SEM picture;
Fig. 2 is the NiCo of embodiment 1 preparation
2O
4Electrode material high power TEM picture;
Fig. 3 is the NiCo of embodiment 1 preparation
2O
4Electrode material electro-chemical test picture.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) take raw material Nickelous nitrate hexahydrate Ni (NO
3)
26H
2O, Co (NO
3)
26H
2The mol ratio of O and urea is that 1:2:1 is dissolved in the second alcohol and water, and stirs, and makes mixed solution; Wherein, the volume of described ethanol and water is respectively 15,35ml;
(2) above-mentioned mixed solution is poured in the polytetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, under 100 ℃ of conditions, reaction is 6 hours, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into Muffle furnace 250 ℃ of calcinings 120 minutes; Resulting final black sample is ultracapacitor NiCo
2O
4Electrode material.
Embodiment 2
(1) take raw material Nickelous nitrate hexahydrate Ni (NO
3)
26H
2O, Co (NO
3)
26H
2The mol ratio of O and urea is that 1:2:2 is dissolved in the second alcohol and water, and stirs, and makes mixed solution; Wherein, the volume of described ethanol and water is respectively 10,40ml; (2) above-mentioned mixed solution is poured in the polytetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, under 150 ℃ of conditions, reaction is 24 hours, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into Muffle furnace 300 ℃ of calcinings 60 minutes; Resulting final black sample is ultracapacitor NiCo
2O
4Electrode material.
(1) take raw material Nickelous nitrate hexahydrate Ni (NO
3) 26H
2O, Co (NO
3)
26H
2The mol ratio of O and urea is that 1:2:4 is dissolved in the second alcohol and water, and stirs, and makes mixed solution; Wherein, the volume of described ethanol and water is respectively 5,45ml;
(2) above-mentioned mixed solution is poured in the polytetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, under 200 ℃ of conditions, reaction is 24 hours, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into Muffle furnace 350 ℃ of calcinings 120 minutes; Resulting final black sample is ultracapacitor NiCo
2O
4Electrode material.
Claims (6)
1. electrode material for super capacitor NiCo
2O
4The preparation method, comprising:
(1) with mol ratio be the Nickelous nitrate hexahydrate Ni (NO of 1:2:1-10
3)
26H
2O, cabaltous nitrate hexahydrate Co (NO
3)
26H
2O and urea add in the mixed solution of second alcohol and water, and stirring and dissolving obtains mixed solution;
(2) above-mentioned mixed solution carries out hydro-thermal reaction, and reaction temperature is 90-200 ℃, and the reaction time is 3-48h, is cooled to room temperature, the centrifugal NiCo that obtains
2O
4, then washing, dry, calcining namely get electrode material for super capacitor.
2. a kind of electrode material for super capacitor NiCo according to claim 1
2O
4The preparation method, it is characterized in that: in the mixed solution of second alcohol and water, volume ratio is 0-1: 1 in described step (1).
3. a kind of electrode material for super capacitor NiCo according to claim 1
2O
4The preparation method, it is characterized in that: hydro-thermal reaction is carried out in the 60mL hydrothermal reaction kettle in described step (2), and the reactor compactedness is 80%.
4. a kind of electrode material for super capacitor NiCo according to claim 1
2O
4The preparation method, it is characterized in that: washing is for washing with deionized water and ethanol respectively in described step (2).
5. a kind of electrode material for super capacitor NiCo according to claim 1
2O
4The preparation method, it is characterized in that: calcining heat is 200-400 ℃ in described step (2), and calcination time is 20-500min.
6. a kind of electrode material for super capacitor NiCo according to claim 1
2O
4The preparation method, it is characterized in that: electrode material for super capacitor NiCo in described step (2)
2O
4To connect into line by single nano particle to be self-assembled into spherical structure.
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
| CN103594246A (en) * | 2013-11-21 | 2014-02-19 | 东华大学 | Preparation method for electrode material of porous NiCo2O4 nanowire array supercapacitor |
| CN103606467A (en) * | 2013-11-21 | 2014-02-26 | 东华大学 | Preparation method for NiCo2O4/MnO2/AC water system asymmetric super capacitor |
| CN103979618A (en) * | 2014-05-05 | 2014-08-13 | 同济大学 | Synthetic method for nickel cobaltate nano-material used for supercapacitor |
| CN104211128A (en) * | 2014-09-05 | 2014-12-17 | 南开大学 | Preparation method of one-dimensional NiCo2O4 nanorod as supercapacitor material |
| CN104659360A (en) * | 2015-03-19 | 2015-05-27 | 武汉大学 | Nickel-cobalt oxide electrode material as well as preparation method and applications thereof |
| CN104766725A (en) * | 2015-03-12 | 2015-07-08 | 广东工业大学 | Preparation method for electrode material used for supercapacitor and application of electrode material |
| CN105448527A (en) * | 2015-11-24 | 2016-03-30 | 青岛能迅新能源科技有限公司 | Electrode material for super capacitor and preparation method for the same |
| CN106006763A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Method for preparing nickel cobaltate nanocrystalline assembly |
| CN106128801A (en) * | 2016-06-08 | 2016-11-16 | 东华大学 | A kind of ultracapacitor NiCo2o4the preparation method of based composites |
| CN106698527A (en) * | 2016-11-25 | 2017-05-24 | 江苏大学 | Hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as solvent system |
| CN106935870A (en) * | 2017-04-01 | 2017-07-07 | 青岛大学 | A kind of preparation and application that nickel cobalt oxide catalyst is prepared based on water-in-oil inverse micro emulsion method |
| CN106938859A (en) * | 2017-04-01 | 2017-07-11 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
| CN107180704A (en) * | 2017-05-16 | 2017-09-19 | 江苏大学 | A kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt |
| CN107177053A (en) * | 2017-05-22 | 2017-09-19 | 陕西科技大学 | Sour nickel silicon carbide fibre multi-scale reinforcing body enhancing polyimide resin based structures absorbing material of a kind of cobalt and preparation method thereof |
| CN107473273A (en) * | 2017-08-02 | 2017-12-15 | 东北大学秦皇岛分校 | Three-dimensional structure micron order cobalt acid Ni cluster, preparation method and the usage |
| CN107658145A (en) * | 2017-09-29 | 2018-02-02 | 山东大学 | A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method and application |
| CN108807001A (en) * | 2018-07-25 | 2018-11-13 | 安阳师范学院 | Spherical cobalt acid nickel-ceria combination electrode material of multilevel hierarchy and preparation method thereof |
| CN109003838A (en) * | 2018-07-27 | 2018-12-14 | 重庆三峡学院 | A kind of nanosphere electrode and preparation method thereof |
| CN113213555A (en) * | 2021-05-19 | 2021-08-06 | 国网天津市电力公司电力科学研究院 | Needle-like NiCo2O4Preparation method of super-electric material |
| CN115745024A (en) * | 2022-11-28 | 2023-03-07 | 桂林理工大学 | Preparation method of spinel oxide nickel cobaltate |
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| CN102108552A (en) * | 2010-11-15 | 2011-06-29 | 复旦大学 | Method for preparing NiCo2O4 nanocrystal film and application of the film in preparing semiconductor optoelectronic devices |
| CN102259936A (en) * | 2011-07-13 | 2011-11-30 | 中国科学院电工研究所 | Preparation method of nano nickel cobalt oxide |
| CN102745752A (en) * | 2012-07-02 | 2012-10-24 | 同济大学 | Method of synthesizing mesoporous nickel cobalt oxide nanowire using hydrothermal method and application thereof |
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2013
- 2013-02-25 CN CN201310058911.5A patent/CN103107025B/en not_active Expired - Fee Related
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| CN102108552A (en) * | 2010-11-15 | 2011-06-29 | 复旦大学 | Method for preparing NiCo2O4 nanocrystal film and application of the film in preparing semiconductor optoelectronic devices |
| CN102259936A (en) * | 2011-07-13 | 2011-11-30 | 中国科学院电工研究所 | Preparation method of nano nickel cobalt oxide |
| CN102745752A (en) * | 2012-07-02 | 2012-10-24 | 同济大学 | Method of synthesizing mesoporous nickel cobalt oxide nanowire using hydrothermal method and application thereof |
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| CN103440998B (en) * | 2013-08-21 | 2016-05-04 | 吉林大学 | A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof |
| CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
| CN103594246A (en) * | 2013-11-21 | 2014-02-19 | 东华大学 | Preparation method for electrode material of porous NiCo2O4 nanowire array supercapacitor |
| CN103606467A (en) * | 2013-11-21 | 2014-02-26 | 东华大学 | Preparation method for NiCo2O4/MnO2/AC water system asymmetric super capacitor |
| CN103979618A (en) * | 2014-05-05 | 2014-08-13 | 同济大学 | Synthetic method for nickel cobaltate nano-material used for supercapacitor |
| CN104211128A (en) * | 2014-09-05 | 2014-12-17 | 南开大学 | Preparation method of one-dimensional NiCo2O4 nanorod as supercapacitor material |
| CN104766725B (en) * | 2015-03-12 | 2017-06-20 | 广东工业大学 | A kind of preparation method and applications for electrode material for super capacitor |
| CN104766725A (en) * | 2015-03-12 | 2015-07-08 | 广东工业大学 | Preparation method for electrode material used for supercapacitor and application of electrode material |
| CN104659360A (en) * | 2015-03-19 | 2015-05-27 | 武汉大学 | Nickel-cobalt oxide electrode material as well as preparation method and applications thereof |
| CN105448527A (en) * | 2015-11-24 | 2016-03-30 | 青岛能迅新能源科技有限公司 | Electrode material for super capacitor and preparation method for the same |
| CN105448527B (en) * | 2015-11-24 | 2018-02-06 | 青岛能迅新能源科技有限公司 | A kind of electrode material for ultracapacitor and preparation method thereof |
| CN106006763A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Method for preparing nickel cobaltate nanocrystalline assembly |
| CN106128801A (en) * | 2016-06-08 | 2016-11-16 | 东华大学 | A kind of ultracapacitor NiCo2o4the preparation method of based composites |
| CN106698527A (en) * | 2016-11-25 | 2017-05-24 | 江苏大学 | Hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as solvent system |
| CN106935870A (en) * | 2017-04-01 | 2017-07-07 | 青岛大学 | A kind of preparation and application that nickel cobalt oxide catalyst is prepared based on water-in-oil inverse micro emulsion method |
| CN106938859A (en) * | 2017-04-01 | 2017-07-11 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
| CN106935870B (en) * | 2017-04-01 | 2018-01-02 | 青岛大学 | A kind of preparation and application that nickel cobalt oxide catalyst is prepared based on water-in-oil inverse micro emulsion method |
| CN106938859B (en) * | 2017-04-01 | 2018-02-16 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
| CN107180704A (en) * | 2017-05-16 | 2017-09-19 | 江苏大学 | A kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt |
| CN107177053A (en) * | 2017-05-22 | 2017-09-19 | 陕西科技大学 | Sour nickel silicon carbide fibre multi-scale reinforcing body enhancing polyimide resin based structures absorbing material of a kind of cobalt and preparation method thereof |
| CN107473273A (en) * | 2017-08-02 | 2017-12-15 | 东北大学秦皇岛分校 | Three-dimensional structure micron order cobalt acid Ni cluster, preparation method and the usage |
| CN107658145A (en) * | 2017-09-29 | 2018-02-02 | 山东大学 | A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method and application |
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| CN108807001A (en) * | 2018-07-25 | 2018-11-13 | 安阳师范学院 | Spherical cobalt acid nickel-ceria combination electrode material of multilevel hierarchy and preparation method thereof |
| CN109003838A (en) * | 2018-07-27 | 2018-12-14 | 重庆三峡学院 | A kind of nanosphere electrode and preparation method thereof |
| CN113213555A (en) * | 2021-05-19 | 2021-08-06 | 国网天津市电力公司电力科学研究院 | Needle-like NiCo2O4Preparation method of super-electric material |
| CN115745024A (en) * | 2022-11-28 | 2023-03-07 | 桂林理工大学 | Preparation method of spinel oxide nickel cobaltate |
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