CN105679549A - Preparation of Co3O4@NiO core-shell nanowire array electrode material - Google Patents

Preparation of Co3O4@NiO core-shell nanowire array electrode material Download PDF

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Publication number
CN105679549A
CN105679549A CN201610019229.9A CN201610019229A CN105679549A CN 105679549 A CN105679549 A CN 105679549A CN 201610019229 A CN201610019229 A CN 201610019229A CN 105679549 A CN105679549 A CN 105679549A
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electrode
nano
nio
shell
core
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韩丹丹
其他发明人请求不公开姓名
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Jilin Institute of Chemical Technology
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Jilin Institute of Chemical Technology
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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
    • H01G11/24—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 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
    • H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
    • 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 supercapacitor electrode material of of a Co3O4@NiO core-shell nanowire array. According to the supercapacitor electrode material, NiO directly grows on the Co3O4 nanowire array prepared in advance by an electrodeposition method; the top end of the compounded nanowire array is a flat end; and entering of an electrolyte is facilitated, so that the core-shell material is fully utilized. Meanwhile, in-situ growth on a three-dimensional nickel screen is achieved by selecting experiment conditions. The preparation process is simple and convenient to operate; and the product is regular in shape and form. The electrode material directly grows on a conductive substrate; and addition of a conductive agent or an adhesive is avoided, so that the impedance of a resistor is greatly reduced; the defects of the materials are compensated by combination of different component materials; the electrode material has a synergetic effect; and improvement of the electrochemical properties of the electrode is facilitated.

Description

Co3O4The preparation of NiO core-shell nano linear array electrode material
Technical field
The invention belongs to ultracapacitor device technical field, be specifically related to Co3O4The research of NiO core-shell nano linear array electrode material for super capacitor.
Background technology
Along with the arrival of world energy sources crisis, produce and the power supply unit (such as ultracapacitor, lithium ion battery etc.) of manufacturing property brilliance becomes more and more important. Transition metal oxide is because of its various valence electron structure, abundant physics and chemical property, and the application in fields such as photoelectricity, catalysis, magnetic and ultracapacitors becomes the focus of current research.
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 research and application. The electrode material being commonly used for ECs includes Carbon Materials, metal-oxide and conducting polymer three major types. Electric double layer storage energy (electric double layer capacitance) that carbon material electrode is formed by the interface of electrolyte with 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 typically much deeper than the electric double layer capacitance that Carbon Materials obtains. As ECs electrode material use metal oxide containing precious metals (such as RuO2) there is very excellent electrochemical capacitance, but the price of costliness and hypertoxicity restrict it significantly as the application of electrochemical capacitor electrode material and commercialization, and researcher is attempted preparing cobalt oxide (Co by distinct methods3O4), nickel oxide (NiO), stannum oxide (SnO2) and manganese oxide (MnOx) etc. base metal oxide, as the succedaneum 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 report increases to some extent recently, but the self-defect of single metal oxide materials such as low conductivity, the defects such as crystalline structure is limited, and specific capacity is relatively low are still the key that restriction high performance electrode material is applied further. Therefore, by two or more material organic composite in different forms, design synthesizes the heterojunction structure composite oxide of metal of novel in shape, Stability Analysis of Structures, height ratio capacity, utilize the cooperative effect of its generation, making up self-defect, the tool of constructing realizing high efficiency energy storage components and parts is of great significance by this. H.J.Fan et al. is at various 1D metal-oxide (TiO2, NiO and Co3O4) granule surface contral synthesis conductive polymer polyanaline, two kinds of inorganic/organic materials combine with hydrophobic solvent effect and electrostatic interaction, enhance the mechanical stability of 1D nano material, alleviate in charge and discharge process because the material structure caused by electrode volumetric expansion destroys, improve the cycle life of electrode.As can be seen here, by single 1D metal oxide electrode material Composite, it is achieved Stability Analysis of Structures, bigger serface, loose structure and high reaction activity point electrode material construct be comprehensively improve electrode electro Chemical performance key. The nano array structure of Heterogeneous Composite transition metal oxide disclosure satisfy that the needs that electrode pair structure stability and each component are modified mutually.
In recent years, various methods are used for controlling synthesis and have good pattern and the adjustable nuclear shell structure nano linear array of function, mainly include chemical precipitation, oxidation, based on wet chemical and some physical techniques such as sputtering and pulsed laser deposition etc. of sacrificing template, these process in, structure complexity, regular appearance, well-crystallized, excellent electrochemical performance heterojunction structure composite have been reported. But, with synthetic method easy, energy-conservation, efficient, it is precisely controlled synthesis transition metal oxide or hydroxide core-shell nano array still needs to further exploration. Adopt and grow metal oxide electrode material at conductive substrates surface in situ, active material utilization height can be effectively improved, increase active surface, improve the diffusion mass transfer performance of material. Therefore, we attempt adopting two step solwution methods, select suitable reaction condition, control the heterojunction structure nucleocapsid metal oxide nano-wire array of synthesis regular appearance in conductive substrates, are expected to comprehensively improve the chemical property of metal oxide composite electrode material.
Therefore, this research adopts and grows metal oxide electrode material at conductive substrates surface in situ, can be effectively improved active material utilization height, increases active surface, improve the diffusion mass transfer performance of material. And attempt by electrodeposition process at Cobalto-cobaltic oxide surface deposited oxide nickel presoma, and obtain Co through calcining3O4NiO core-shell nano linear array.
Summary of the invention
The present invention is using on conductive current collector nickel screen, growth in situ cobaltosic oxide nano line is as skeleton, and electro-deposition obtains Co3O4NiO core-shell nano linear array, it is provided that a kind of preparation method is simple and has the fake capacitance composite oxide electrode material of high specific capacity and better stability.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that:
A kind of Co3O4The electrode material for super capacitor of NiO core-shell nano linear array, it is 3D nickel screen that the electrode system of described ultracapacitor includes conductive current collector, electrolyte and conductive substrates.
The present invention adopts hydro-thermal method growth in situ Co on conductive substrates nickel screen3O4Nano-wire array, as skeleton, after electro-deposition, calcining generates Co3O4NiO core-shell nano linear array, as the negative electrode of ultracapacitor, specifically includes following steps: (1) Co3O4The preparation of nano wire, by the uniform ultrasonic mixing in distilled water of 1-5mmol cobalt nitrate, 2-10mmol ammonium fluoride and 6-30mmol carbamide, this solution is moved in the autoclave of polytetrafluoro liner, 110-150 DEG C of reaction 2-8h, and the conductive substrates nickel foam after washing is placed in solution, take out substrate after having reacted and carry out washing and vacuum drying, obtain the precursor of Cobalto-cobaltic oxide, by Cobalto-cobaltic oxide precursor 350 DEG C of heat treatment 1.5h in air atmosphere, obtain the cobaltosic oxide nano linear array that top is tip; (2) Co3O4The preparation of NiO core-shell nano linear array, above-mentioned Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.1-0.5M nickel nitrate solution 30-50mL, after adopting cyclic voltammetry (-1.1V～-0.5V) to sweep speed circulation 15min-2h with 5-50mV/s, take out sample, and use distilled water wash.Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains the Co that top is flush end3O4NiO core-shell nano linear array combination electrode material.
Gained Co3O4NiO core-shell nano linear array stability in conductive substrates is tested by the method for ultrasonic vibration.
Hydro-thermal method prepares Co3O4Process in, in order to obtain regular appearance, the array structure being firmly combined with, placement location and the method for conductive substrates have large effect, are placed in reactor downwards by the conducting surface of conductive substrates, and are 45 ° ~ 75 ° with the interior angle of bottom.
Accompanying drawing explanation
Co prepared in Fig. 1 embodiment 13O4The XRD spectra of NiO core-shell nano linear array.
Co prepared in Fig. 2 embodiment 13O4The stereoscan photograph of nano-wire array.
Co prepared in Fig. 3 embodiment 13O4The stereoscan photograph of NiO core-shell nano linear array.
Co prepared in Fig. 4 embodiment 13O4NiO core-shell nano linear array difference sweeps the cyclic voltammetry curve of speed.
Co prepared in Fig. 5 embodiment 13O4The charging and discharging curve of NiO core-shell nano linear array.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme and effect are further described. But, the concrete grammar, formula and the explanation that use are not limitation of the present invention.
Embodiment 1: by Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.3M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 1h with 10mV/s, take out sample, and use distilled water wash. Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.
Embodiment 2: by Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.1M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 1h with 10mV/s, take out sample, and use distilled water wash. Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.
Embodiment 3: by Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.5M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 1h with 5mV/s, take out sample, and use distilled water wash. Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.
Embodiment 4: by Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.3M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 30min with 20mV/s, take out sample, and use distilled water wash.Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.
Embodiment 5: by Co3O4Nano-wire array sample is as working electrode, (saturated calomel electrode) SCE is as reference electrode, platinum is as to electrode, electric depositing solution is 0.3M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 2h with 50mV/s, take out sample, and use distilled water wash. Sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.

Claims (4)

1. one kind based on Co3O4NiO core-shell nano linear array electrode for super capacitor material, the electrode system of described ultracapacitor includes conductive current collector, electrode active material layers, electrolyte, it is characterized in that, described electrode active material is the Co being grown directly upon on conductive current collector nickel screen3O4NiO core-shell nano linear array.
2. Co according to claim 13O4NiO core-shell nano linear array electrode for super capacitor material, it is characterised in that described nano-wire array skeleton is Co3O4Nano wire, shell is the core-shell material of porous nano-sheet NiO, and nano-wire array top is flush end, and diameter is 100-150nm.
3. the Co according to right 33O4The electrode for super capacitor material of NiO core-shell nano linear array, it is characterised in that Combined Mining three-electrode system, cyclic voltammetry, potential range is-1.1V～-0.5V.
4. a Co3O4The electrode for super capacitor material of NiO core-shell nano linear array, it is characterised in that following steps: Co3O4Nano-wire array adopts hydro-thermal method to be grown directly upon in nickel foam conductive substrates, and placement location and the method for conductive substrates have large effect, are placed in reactor downwards by the conducting surface of conductive substrates, and is 45 ° ~ 75 ° with the interior angle of bottom, by Co3O4Nano-wire array sample is as working electrode, electric depositing solution is 0.1-0.5M nickel nitrate solution 50mL, adopting cyclic voltammetry current potential is-1.1V～-0.5V, after sweeping speed circulation 30min-2h with 5-50mV/s, take out sample, and with distilled water wash, sample is again annealed in tube furnace, at N at 300 DEG C2In protection, 10 DEG C/min heating rate is warming up to 300 DEG C, is incubated 1.5h, is cooled to 60 DEG C with 3 DEG C/min rate of temperature fall, obtains Co3O4NiO core-shell nano linear array combination electrode material.
CN201610019229.9A 2016-01-13 2016-01-13 Preparation of Co3O4@NiO core-shell nanowire array electrode material Pending CN105679549A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105958059A (en) * 2016-07-18 2016-09-21 合肥工业大学 Three-dimensional Cu/Co3O4 multi-stage nanowire array and preparation method and application thereof
CN106449132A (en) * 2016-09-23 2017-02-22 安徽师范大学 Mesoporous Co3O4 nano-wire @ NiCo2O4 nanoplate graded core-shell array material, preparation method and application
CN109828009A (en) * 2019-01-29 2019-05-31 吉林大学 A kind of H based on metal oxide semiconductor films material2S gas sensor and preparation method thereof
CN111195518A (en) * 2020-01-10 2020-05-26 兰州大学 NiO/Co3O4Preparation method and application thereof

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CN102522218A (en) * 2011-12-14 2012-06-27 温州大学 Nano nickel oxide/graphene composite electrode material as well as preparation method and application thereof
CN104681299A (en) * 2015-03-27 2015-06-03 吉林化工学院 Supercapacitor electrode material of cobaltosic oxide porous nanowire array, and preparation method thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105958059A (en) * 2016-07-18 2016-09-21 合肥工业大学 Three-dimensional Cu/Co3O4 multi-stage nanowire array and preparation method and application thereof
CN105958059B (en) * 2016-07-18 2018-11-02 合肥工业大学 A kind of three-dimensional Cu/Co3O4Multi-stage nano linear array and its preparation method and application
CN106449132A (en) * 2016-09-23 2017-02-22 安徽师范大学 Mesoporous Co3O4 nano-wire @ NiCo2O4 nanoplate graded core-shell array material, preparation method and application
CN106449132B (en) * 2016-09-23 2018-08-17 安徽师范大学 A kind of mesoporous Co3O4Nano wire@NiCo2O4Nanometer sheet is classified nucleocapsid array material, preparation method and application
CN109828009A (en) * 2019-01-29 2019-05-31 吉林大学 A kind of H based on metal oxide semiconductor films material2S gas sensor and preparation method thereof
CN109828009B (en) * 2019-01-29 2021-08-13 吉林大学 H based on metal oxide semiconductor thin film material2S gas sensor and preparation method thereof
CN111195518A (en) * 2020-01-10 2020-05-26 兰州大学 NiO/Co3O4Preparation method and application thereof
CN111195518B (en) * 2020-01-10 2022-11-25 兰州大学 NiO/Co 3 O 4 Preparation method and application thereof

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