CN104701036A - Research of super-capacitor electrode material based on graded flowerlike NiCo2O4 - Google Patents
Research of super-capacitor electrode material based on graded flowerlike NiCo2O4 Download PDFInfo
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- CN104701036A CN104701036A CN201510135896.9A CN201510135896A CN104701036A CN 104701036 A CN104701036 A CN 104701036A CN 201510135896 A CN201510135896 A CN 201510135896A CN 104701036 A CN104701036 A CN 104701036A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 24
- 239000003990 capacitor Substances 0.000 title claims abstract description 14
- 229910005949 NiCo2O4 Inorganic materials 0.000 title abstract 4
- 239000000758 substrate Substances 0.000 claims abstract description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 4
- 229910017709 Ni Co Inorganic materials 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 7
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011530 conductive current collector Substances 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 238000001338 self-assembly Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000011230 binding agent Substances 0.000 abstract 1
- 239000006258 conductive agent Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 abstract 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 22
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 150000004706 metal oxides Chemical class 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910003266 NiCo Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 241000257465 Echinoidea Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
-
- 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
- H01G11/84—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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a super-capacitor electrode material based on graded flowerlike NiCo2O4. The super-capacitor electrode material is graded flowerlike NiCo2O4 which is directly grown on the nickel mesh of a conductive substrate by a hydrothermal method. The flowerlike structure prepared by the method for preparing NiCo2O4 is formed by assembling nanometer sheets, and in-situ growth on the three-dimensional nickel mesh is realized by selecting experiment conditions; the preparation process is easy to operate and products are regular in shape; because the electrode material directly grows on the conductive substrate, thereby avoiding to add a conductive agent and a binding agent, greatly reducing electrode impedance, increasing the contact action between the graded structure electrode material and the conductive substrate, and increasing osmosis of electrolyte by loosely assembling the nanometer sheets.
Description
Technical field
The invention belongs to ultracapacitor device technical field, be specifically related to classification flower-shape Ni Co
2o
4the research of electrode material for super capacitor.
Background technology
Along with the arrival of world energy sources crisis, the power supply unit (such as ultracapacitor, lithium ion battery etc.) of production and manufacturing property brilliance becomes more and more important.Transition metal oxide because of its various valence electron structure, abundant physics and chemistry character, and the focus becoming current research in the application in the fields such as photoelectricity, catalysis, magnetic and ultracapacitor.
The electro-chemical activity of electrode material directly determines the capacitive property of device, and therefore, the exploitation of active electrode material just becomes the emphasis of ECs investigation and application.Usually, the electrode material for ECs comprises Carbon Materials, metal oxide and conducting polymer three major types.The electric double layer stored energy (electric double layer capacitance) that carbon material electrode is formed by the interface of electrolyte and electrode; Metal oxide and conducting polymer materials electrode then obtain faraday's electric capacity (fake capacitance) by the redox reaction of Rapid reversible, and this faraday's electric capacity is generally much larger than the electric double layer capacitance that Carbon Materials obtains.As ECs electrode material use metal oxide containing precious metals (as RuO
2) there is very excellent electrochemical capacitance, but the price of costliness and hypertoxicity restrict its application as electrochemical capacitor electrode material and commercialization greatly, and researcher attempts preparing cobalt oxide (Co by distinct methods
3o
4), nickel oxide (NiO), tin oxide (SnO
2) and manganese oxide (MnO
x) etc. base metal oxide, as the substitute of metal oxide containing precious metals, the specific capacity of electrode, efficiency for charge-discharge and long circulation life significantly improve.
The metal oxide electrode material specific capacity about one-component of nearest report increases to some extent, but lower cycle life, poor conductivity and high-rate characteristics hinder electrode material application in practice, therefore, recently several fake capacitance metal oxide Composite is caused the attention of vast researcher, particularly synthesize the NiCo of various patterns cheap and easy to get
2o
4electrode material, research shows the synergy that this material has good charge-conduction ability and electro-chemical activity, particularly nickel and cobalt ions and produces in charge and discharge process can provide abundanter fake capacitance reactivity point, improves the chemical property of electrode.
In recent years, various method has good pattern and the adjustable NiCo of function for controlling to synthesize
2o
4electrode material, in the patterns such as nano-wire array, nanometer sheet, sea urchin shape, the rare report of porous material that classification is flower-shaped, wherein with easy, energy-conservation, efficient synthetic method, precisely controls synthesis transition metal oxide and still needs further exploration.The present invention adopts at conductive substrates surface in situ growing metal oxide electrode material, effectively can improve the diffusion mass transfer performance that active material utilization is high, increase active surface, improve material.
Summary of the invention
The present invention is by the classification flower-shape Ni Co of growth in situ on conductive current collector nickel screen
2o
4be applied to electrode material for super capacitor, provide a kind of preparation method simple and the fake capacitance electrode material had compared with height ratio capacity and better stability.
For solving the problems of the technologies described above, the present invention takes following technical scheme: a kind of classification flower-shape Ni Co
2o
4electrode material for super capacitor, the electrode system of described ultracapacitor comprises conductive current collector, electrode active material layers, electrolyte and barrier film, and conductive substrates is 3D nickel screen.
The preparation method of ultracapacitor cobaltosic oxide of the present invention, adopts hydro thermal method growth in situ classification flower-shape Ni Co on conductive substrates nickel screen
2o
4as the negative electrode of ultracapacitor, specifically comprise the steps: that (1) is by cobalt nitrate and nickel nitrate, mol ratio 1:(2-4), complexing agent ammonium fluoride 4 mmol and alkaline precipitating agent urea 8 mmol, in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, and the conductive substrates after washing be placed in solution, hydrothermal temperature is 100 DEG C ~ 130 DEG C, and the time is 5h.React rear taking-up substrate and carried out washing and vacuumize, having obtained the precursor be grown directly upon in conductive substrates; (2) heat-treated in air atmosphere by precursor, heat treated temperature is 200 DEG C ~ 600 DEG C, namely obtains described based on classification flower-shape Ni Co
2o
4electrode material for super capacitor.
Classification flower-shape Ni Co
2o
4stability in conductive substrates is tested by the method for ultrasonic vibration.
Hydro thermal method prepares NiCo
2o
4in process, in order to obtain regular appearance, in conjunction with firmly array structure, the placement location of conductive substrates and method have larger impact, and the conducting surface of conductive substrates is placed in reactor downwards, and are 45 ° ~ 75 ° with the interior angle of bottom.
Accompanying drawing explanation
Fig. 1 is classification flower-shape Ni Co prepared in embodiment 1
2o
4low power stereoscan photograph.
Fig. 2 is classification flower-shape Ni Co prepared in embodiment 1
2o
4high power stereoscan photograph.
Fig. 3 is classification flower-shape Ni Co prepared in embodiment 1
2o
4the cyclic voltammetry curve of electrode.
Fig. 4 is classification flower-shape Ni Co prepared in embodiment 1
2o
4the charging and discharging curve of electrode.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention and effect are further described.But the concrete grammar used, formula and explanation are not limitation of the present invention.
Embodiment 1: by 1mmol cobalt nitrate, 2mmol nickel nitrate, 4 mmol ammonium fluorides and 8 mmol urea in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, 120 DEG C of reaction 5h, and the conductive substrates nickel screen after washing is placed in solution, react rear taking-up substrate and carried out washing and vacuumize, obtain the precursor of cobaltosic oxide, by cobaltosic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain classification flower-shape Ni Co
2o
4.
Embodiment 2: by 1mmol cobalt nitrate, 3mmol nickel nitrate, 4 mmol ammonium fluorides and 8 mmol urea in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, 120 DEG C of reaction 5h, and the conductive substrates nickel screen after washing is placed in solution, react rear taking-up substrate and carried out washing and vacuumize, obtain the precursor of cobaltosic oxide, by cobaltosic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain classification flower-shape Ni Co
2o
4.
Embodiment 3: by 1mmol cobalt nitrate, 4mmol nickel nitrate, 4 mmol ammonium fluorides and 8 mmol urea in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, 120 DEG C of reaction 5h, and the conductive substrates nickel screen after washing is placed in solution, react rear taking-up substrate and carried out washing and vacuumize, obtain the precursor of cobaltosic oxide, by cobaltosic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain classification flower-shape Ni Co
2o
4.
Embodiment 4: by 1mmol cobalt nitrate, 2mmol nickel nitrate, 4 mmol ammonium fluorides and 8 mmol urea in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, 130 DEG C of reaction 5h, and the conductive substrates nickel screen after washing is placed in solution, react rear taking-up substrate and carried out washing and vacuumize, obtain the precursor of cobaltosic oxide, by cobaltosic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain classification flower-shape Ni Co
2o
4.
Embodiment 5: by 1mmol cobalt nitrate, 2mmol nickel nitrate, 4 mmol ammonium fluorides and 8 mmol urea in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, 140 DEG C of reaction 5h, and the conductive substrates nickel screen after washing is placed in solution, react rear taking-up substrate and carried out washing and vacuumize, obtain the precursor of cobaltosic oxide, by cobaltosic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain classification flower-shape Ni Co
2o
4.
Claims (6)
1. one kind based on classification flower-shape Ni Co
2o
4electrode for super capacitor material, the electrode system of described ultracapacitor comprises conductive current collector, electrode active material layers, electrolyte and barrier film, is characterized in that, described electrode active material is the classification flower-shape Ni Co be grown directly upon on conductive current collector nickel screen
2o
4.
2. according to claim 1 based on classification flower-shape Ni Co
2o
4electrode for super capacitor material, it is characterized in that, described classification flower-shape Ni Co
2o
4be formed by the self assembly of classification micron film, micron film height is 3-5 μm.
3. one kind based on classification flower-shape Ni Co
2o
4electrode for super capacitor material, it is characterized in that comprising the steps: cobalt nitrate and nickel nitrate, mol ratio 1:(2-4), complexing agent ammonium fluoride 4 mmol and alkaline precipitating agent urea 8 mmol, in distilled water ultrasonic mix after, move in the autoclave of polytetrafluoro liner, and the conductive substrates after washing is placed in solution, hydrothermal temperature is 100 DEG C ~ 130 DEG C, and the time is 5h.
4. reacted rear taking-up substrate and carried out washing and vacuumize, having obtained the precursor be grown directly upon in conductive substrates.
5. according to right 3 based on classification flower-shape Ni Co
2o
4electrode for super capacitor material, it is characterized in that ammonium fluoride is conducive to the precipitation of two metal ion species as complexing agent.
6. according to right 3 based on classification flower-shape Ni Co
2o
4electrode for super capacitor material, it is characterized in that the conducting surface of conductive substrates is placed in reactor downwards, and be 45 ° ~ 75 ° with the interior angle of bottom.
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Cited By (18)
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CN104979098A (en) * | 2015-07-20 | 2015-10-14 | 苏州大学 | Counter electrode of dye-sensitized solar cell, preparation method thereof and application |
CN105013491A (en) * | 2015-07-06 | 2015-11-04 | 中山大学 | Novel efficient formaldehyde catalyst and preparation method thereof |
CN105374576A (en) * | 2015-08-07 | 2016-03-02 | 北京石油化工学院 | Method for preparing nanometer nickel cobaltate used as super capacitor electrode material |
CN105551832A (en) * | 2016-01-13 | 2016-05-04 | 吉林化工学院 | Research on one-step synthetic NiO/Co<3>O<4> composite electrode material |
CN106011911A (en) * | 2016-05-26 | 2016-10-12 | 重庆大学 | Method of partial vulcanization to improve oxygen evolution electrode performance of metal hydroxide |
CN106219616A (en) * | 2016-07-18 | 2016-12-14 | 合肥工业大学 | A kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof |
CN107045945A (en) * | 2017-05-04 | 2017-08-15 | 重庆石墨烯研究院有限公司 | A kind of super capacitor anode based on conductive substrates direct growth nitrogen-doped carbon cobalt compound microplate array and preparation method thereof |
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CN107591251A (en) * | 2017-07-14 | 2018-01-16 | 电子科技大学 | A kind of soap-free emulsion polymeization formulation NiCo2O4@NiMoO4Core-shell nano chip arrays material and preparation method thereof |
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CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
CN109261168A (en) * | 2018-10-16 | 2019-01-25 | 陕西科技大学 | A kind of Ni of vanadium modification3S2Nano-bar array electrode material and preparation method thereof |
CN110040789A (en) * | 2019-04-17 | 2019-07-23 | 天津大学 | A kind of preparation method of nickel ferrite based magnetic loaded microballoon electrode material for super capacitor |
CN110040789B (en) * | 2019-04-17 | 2021-11-02 | 天津大学 | Preparation method of nickel ferrite microsphere supercapacitor electrode material |
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