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 PDF

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Publication number
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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China
Prior art keywords
shape
electrode
electrode material
classification
flower
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CN201510135896.9A
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Chinese (zh)
Inventor
韩丹丹
徐鹏程
史晋宜
沈启慧
于江微
张立平
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Jilin Institute of Chemical Technology
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Jilin Institute of Chemical Technology
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Priority to CN201510135896.9A priority Critical patent/CN104701036A/en
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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
    • 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 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

Based on classification flower-shape Ni Co 2o 4the research of electrode material for super capacitor
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.
CN201510135896.9A 2015-03-27 2015-03-27 Research of super-capacitor electrode material based on graded flowerlike NiCo2O4 Pending CN104701036A (en)

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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
CN107195471A (en) * 2017-06-01 2017-09-22 上海应用技术大学 A kind of preparation method of the Ni-based combination electrode materials of porous C oAl@
CN107244700A (en) * 2017-06-16 2017-10-13 合肥工业大学 It is a kind of for fluorination hydroxyl nickel cobalt nano material of ultracapacitor and preparation method thereof
CN107316755A (en) * 2017-05-23 2017-11-03 山东大学 A kind of binary cobalt-nickel oxide raw powder's production technology
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
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
CN107899580A (en) * 2017-10-18 2018-04-13 安徽职业技术学院 A kind of preparation method of cobalt acid nickel nanostructured hierarchical array electro-catalysis analysis oxygen material
CN108807013A (en) * 2018-03-26 2018-11-13 西北工业大学 Porous flower-shape Ni Co2O4/Co3O4The preparation method of/NiO electrode material for super capacitor
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
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
CN114804219A (en) * 2022-04-04 2022-07-29 渤海大学 Flower-shaped transition metal oxide assembled by two-dimensional porous nanosheets and preparation method and application thereof

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CN105013491A (en) * 2015-07-06 2015-11-04 中山大学 Novel efficient formaldehyde catalyst and preparation method thereof
CN104979098A (en) * 2015-07-20 2015-10-14 苏州大学 Counter electrode of dye-sensitized solar cell, preparation method thereof and application
CN104979098B (en) * 2015-07-20 2018-08-21 苏州大学 The preparation method to electrode of dye-sensitized solar cells
CN105374576B (en) * 2015-08-07 2018-02-23 北京石油化工学院 A kind of preparation method of nano nickel cobalt oxide for electrode material for super capacitor
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
CN106011911B (en) * 2016-05-26 2018-04-17 重庆大学 A kind of method that partial vulcanization improves metal hydroxides analysis oxygen electrode performance
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
CN106219616B (en) * 2016-07-18 2019-02-19 合肥工业大学 A kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof
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Application publication date: 20150610