CN106564968A - Preparation method for nickel cobaltite electrode material with high specific surface area - Google Patents
Preparation method for nickel cobaltite electrode material with high specific surface area Download PDFInfo
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- CN106564968A CN106564968A CN201611012439.1A CN201611012439A CN106564968A CN 106564968 A CN106564968 A CN 106564968A CN 201611012439 A CN201611012439 A CN 201611012439A CN 106564968 A CN106564968 A CN 106564968A
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- electrode material
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- surface area
- specific surface
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000007772 electrode material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 14
- 229910052963 cobaltite Inorganic materials 0.000 title abstract 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 229910005949 NiCo2O4 Inorganic materials 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 claims abstract description 5
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 13
- 239000010941 cobalt Substances 0.000 claims description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 8
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical class O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract 6
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 235000013495 cobalt Nutrition 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 229910003266 NiCo Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- -1 polyethylene ketopyrrolidine Polymers 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method for a nickel cobaltite electrode material with a high specific surface area. The preparation method comprises the following steps of: dissolving nickel acetate tetrahydrate Ni(AC)2.4H2O, cobalt acetate tetrahydrate Co(AC)2.4H2O and polyvinylpyrrolidone PVP into a solvent and sufficiently stirring to obtain a mixture; enabling the mixture to react for 1-5 hours under a condition with temperature ranging from 150 DEG C to 180 DEG C; and centrifuging the mixture, washing the mixture, drying the mixture and roasting the mixture to obtain the nickel cobaltite electrode material. The method can be used for preparing the NiCo2O4 electrode material with the high specific surface area, has a practical application prospect; and the prepared electrode material has excellent electrochemical performances.
Description
Technical field
The invention belongs to the preparation field of electrode material, more particularly to a kind of system of high-specific surface area cobalt acid nickel electrode material
Preparation Method.
Background technology
Ultracapacitor is considered as in future electronic device most promising energy conversion of future generation and storage facilities, tool
The advantages of having the cycle life of high power density, fast charging and discharging speed and length.Electrode material is to determine ultracapacitor
One of key factor of energy, according to the difference of electrochemical energy storage mechanism, electrode material mainly has material with carbon element, conducting polymer and mistake
Cross metal-oxide this three class.Transition metal oxide is than material with carbon element and conducting polymer due to receiving with higher specific capacitance
To the concern of numerous scientific research personnel.In numerous transition metal oxide electrode materials, cobalt acid nickel Co2O4Due to than single
Oxide has higher electrical conductivity and electro-chemical activity and is considered as a class high-performance super capacitor electrode material.To mesh
Before till, the NiCo of different structure2O4Electrode material has been prepared out and have studied their performance.The present invention is prepared for
The NiCo of high-specific surface area2O4Electrode material, shows excellent chemical property；Synthetic method is simple, and environmental protection is beneficial to
It is extensive to prepare, with critically important application prospect.
The content of the invention
The technical problem to be solved is to provide a kind of preparation method of high-specific surface area cobalt acid nickel electrode material,
Synthetic method of the present invention is simple, environmental protection, can large area prepare cobalt acid nickel Co2O4Material；(2) NiCo prepared by2O4Material
Material is with higher specific surface area；(3)NiCo2O4Under the electric current density of 2A/g, its specific capacitance is up to 1635F/g to electrode material.
A kind of high-specific surface area NiCo of the present invention2O4The preparation method of electrode material, including：
By nickel acetate tetrahydrate Ni (AC)2·4H2O, four acetate hydrates cobalt Co (AC)2·4H2O and polyvinylpyrrolidone
During PVP is dissolved in solvent and being sufficiently stirred for, then 1-5h being reacted under the conditions of 150-180 DEG C, be centrifuged, washing is dried, calcining,
Obtain final product NiCo2O4Electrode material；Wherein Ni (AC)2·4H2O and Co (AC)2·4H2The ratio of O moles is 1:2.
The solvent is ethylene glycol.
The polyvinylpyrrolidone PVP and Ni (AC)2·4H2The mass ratio of O is 1:5～5:1.
The amount of preferably polyethylene ketopyrrolidine is 0.01-0.5g.
The washing is respectively deionized water and washing with alcohol 3-5 time.
The calcining is 200-500 DEG C, calcines 60-300min.
Beneficial effect
(1) synthetic method of the present invention is simple, environmental protection, can prepare cobalt acid nickel Co on a large scale2O4Material；
(2) the cobalt acid nickel Co prepared by the present invention2O4Material has higher specific surface area 112.8m2/g；
(3) NiCo of the invention2O4Electrode material has excellent chemical property, under the electric current density of 2A/g, its ratio
Electric capacity may be up to 1635F/g.
Description of the drawings
Fig. 1 is the scanning electron microscope (a, b) and transmission electron microscope (c, d) of the NiCo2O4 samples of the preparation of embodiment 1 in the present invention
Figure；
Fig. 2 is the specific surface area figure of the NiCo2O4 samples of the preparation of embodiment 1 in the present invention；Wherein illustration is integrated for hole body
Butut；
Fig. 3 is the chemical property figure of the NiCo2O4 samples of the preparation of embodiment 1 in the present invention；Wherein a:Cyclic voltammetric, b
Constant current charge-discharge, c specific capacitances, d AC impedances, e stability, f electric transmission schematic diagrams.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can be made various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) weigh nickel acetate tetrahydrate (Ni (AC)2·4H2O), four acetate hydrate cobalts (Co (AC)2·4H2) and polyethylene O
During ketopyrrolidine (0.1g) is dissolved in ethylene glycol (50mL) and it is sufficiently stirred for.Wherein Ni (AC)2·4H2O and Co (AC)2·4H2O
Mole is respectively 1mmol and 2mmol.
(2) above-mentioned mixed solution is transferred in there-necked flask, is reacted 2 hours at 170 DEG C；Product obtained by centrifugation,
Deionized water and alcohol solvent washing respectively, and be dried.
(3) material of above-mentioned preparation is put in Muffle furnace and is calcined, calcination time is 120 minutes, and calcining heat is 300
℃。
The specific surface area of the electrode material of above-mentioned preparation has reached 112.8m2/ g, under 2A/g electric current densities, specific capacitance reaches
1635F/g is arrived, with relatively low internal resistance and excellent cyclical stability.
Embodiment 2
(1) weigh nickel acetate tetrahydrate (Ni (AC)2·4H2O), four acetate hydrate cobalts (Co (AC)2·4H2) and polyethylene O
During ketopyrrolidine (0.01g) is dissolved in ethylene glycol (50mL amount supplement) and it is sufficiently stirred for.Wherein Ni (AC)2·4H2O and Co
(AC)2·4H2O moles are respectively 0.5mmol and 1mmol.
(2) above-mentioned mixed solution is transferred in there-necked flask, is reacted 4 hours at 150 DEG C；Product obtained by centrifugation,
Deionized water and alcohol solvent washing respectively, and be dried.
(3) material of above-mentioned preparation is put in Muffle furnace and is calcined, calcination time is 180 minutes, and calcining heat is 200
℃。
Claims (4)
1. the preparation method of a kind of high-specific surface area cobalt acid nickel electrode material, including：
By nickel acetate tetrahydrate Ni (AC)2·4H2O, four acetate hydrates cobalt Co (AC)2·4H2O and polyvinylpyrrolidone PVP are molten
Solution is in solvent and is sufficiently stirred for, and then reacts 1-5h under the conditions of 150-180 DEG C, centrifugation, and washing is dried, and calcining is obtained final product
NiCo2O4Electrode material；Wherein Ni (AC)2·4H2O and Co (AC)2·4H2The ratio of O moles is 1:2.
2. the preparation method of a kind of high-specific surface area cobalt acid nickel electrode material according to claim 1, it is characterised in that：Institute
Solvent is stated for ethylene glycol.
3. the preparation method of a kind of high-specific surface area cobalt acid nickel electrode material according to claim 1, it is characterised in that：Institute
State polyvinylpyrrolidone PVP and Ni (AC)2·4H2The mass ratio of O is 1:5～5:1.
4. the preparation method of a kind of high-specific surface area cobalt acid nickel electrode material according to claim 1, it is characterised in that：Institute
Calcining is stated for 200-500 DEG C, 60-300min is calcined.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012439.1A CN106564968A (en) | 2016-11-17 | 2016-11-17 | Preparation method for nickel cobaltite electrode material with high specific surface area |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012439.1A CN106564968A (en) | 2016-11-17 | 2016-11-17 | Preparation method for nickel cobaltite electrode material with high specific surface area |
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| Publication Number | Publication Date |
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| CN106564968A true CN106564968A (en) | 2017-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611012439.1A Pending CN106564968A (en) | 2016-11-17 | 2016-11-17 | Preparation method for nickel cobaltite electrode material with high specific surface area |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910963A (en) * | 2018-06-25 | 2018-11-30 | 青岛大学 | A kind of Fe, Ni replace altogether cobalt-based spinel-type absorbing material and its preparation method and application |
| CN111029565A (en) * | 2019-12-20 | 2020-04-17 | 淮北师范大学 | Lithium ion battery cathode material NiCo2O4Preparation method of porous nanosheet |
| CN111653786A (en) * | 2020-06-28 | 2020-09-11 | 厦门大学 | Transition metal-based lithium-sulfur battery positive electrode material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104773764A (en) * | 2015-03-30 | 2015-07-15 | 北京化工大学 | Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres |
| CN105399151A (en) * | 2015-11-24 | 2016-03-16 | 青岛能迅新能源科技有限公司 | Preparation method of NiCo2O4 nano-material |
| CN105439213A (en) * | 2015-11-24 | 2016-03-30 | 青岛能迅新能源科技有限公司 | Nanometer nickel cobaltite and preparation method thereof |
-
2016
- 2016-11-17 CN CN201611012439.1A patent/CN106564968A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104773764A (en) * | 2015-03-30 | 2015-07-15 | 北京化工大学 | Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres |
| CN105399151A (en) * | 2015-11-24 | 2016-03-16 | 青岛能迅新能源科技有限公司 | Preparation method of NiCo2O4 nano-material |
| CN105439213A (en) * | 2015-11-24 | 2016-03-30 | 青岛能迅新能源科技有限公司 | Nanometer nickel cobaltite and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| KAIBING XU ET AL.: "Facile synthesis of hierarchical mesoporous NiCo2O4 nanoflowers with large specific surface area for high-performance supercapacitors", 《MATERIALS LETTERS》 * |
| YIRONG ZHU ET AL.: "An electrochemical exploration of hollow NiCo2O4 submicrospheres and its capacitive performances", 《JOURNAL OF POWER SOURCES》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910963A (en) * | 2018-06-25 | 2018-11-30 | 青岛大学 | A kind of Fe, Ni replace altogether cobalt-based spinel-type absorbing material and its preparation method and application |
| CN108910963B (en) * | 2018-06-25 | 2020-07-17 | 青岛大学 | Fe and Ni co-substituted cobalt-based spinel type wave-absorbing material and preparation method and application thereof |
| CN111029565A (en) * | 2019-12-20 | 2020-04-17 | 淮北师范大学 | Lithium ion battery cathode material NiCo2O4Preparation method of porous nanosheet |
| CN111653786A (en) * | 2020-06-28 | 2020-09-11 | 厦门大学 | Transition metal-based lithium-sulfur battery positive electrode material and preparation method thereof |
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