CN106960730A - A kind of high stability nickel cobalt double-hydroxide electrode material and preparation method thereof - Google Patents
A kind of high stability nickel cobalt double-hydroxide electrode material and preparation method thereof Download PDFInfo
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- CN106960730A CN106960730A CN201710049840.0A CN201710049840A CN106960730A CN 106960730 A CN106960730 A CN 106960730A CN 201710049840 A CN201710049840 A CN 201710049840A CN 106960730 A CN106960730 A CN 106960730A
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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
- H01G11/30—Electrodes characterised by their material
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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
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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
- H01G11/84—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
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- 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 belongs to super capacitor material field, and in particular to high stability super capacitor anode material nickel cobalt double-hydroxide (NiCo DH) and preparation method thereof；The material is a kind of three-dimensional flower-shaped micro-sphere structure assembled by ultrathin nanometer piece, belongs to α type lamellar compounds, and interlamellar spacing isThe nanometer sheet thickness for constituting microballoon is less than 10nm.Material prepares and uses nickel salt, and cobalt salt is presoma, and urea is precipitating reagent, is synthesized in atmospheric conditions by microwave synthesizer, and the sample preparation time significantly reduces, and synthesis condition is gentle, Simple energy-saving, the potentiality with industry amplification.The α phase NiCo DH of synthesis show high specific capacitance (1120F g as super capacitor anode material‑1), outstanding forthright again and excellent stability；Its specific capacitance stable operation of the stability test of the circle of progress 2000 circulation does not decay under 10A/g high current densities, and specific capacitance value also has increased slightly with circulation and (increases to the 2000th 1220F/g enclosed from the 996F/g of the 1st circle).Preparation process of the present invention is simple and quick, and mild condition can amplify, and the α type NiCo DH overall performances prepared using this method are excellent, have some reference value to the application of super capacitor material.
Description
Technical field
The present invention relates to electrode material field, more particularly to a kind of high stability super capacitor anode material and its system
Preparation Method
Background technology
In recent years, ultracapacitor is due to fast charging and discharging, the advantage such as high power density and security reliability, in energy
Source storage receives much concern with conversion field.At present, conventional super capacitor material be based on electrode surface quick adsorption/desorption from
The double layer capacitor material of handset reason, occurs in electrode material surface, storage energy is often limited, leads yet with the process
Cause the low big restraining factors as electric double layer Materials of specific capacitance.
It is exactly to use the fake capacitance material based on redox reaction to solve a kind of relatively low approach of specific capacitance.As common
Fake capacitance material, RuO2,MnO2,V2O5,Fe2O3Deng.It is exactly a kind of theoretical than electricity electricity wherein based on Ni-based metal hydroxides
Hold high ideal electrode material.Such as α type nickel cobalt double-hydroxides, as electrode material to possess specific capacitance high, forthright good etc. excellent again
Gesture, however, in alkaline solution, often leading to its structural instability and causing cyclical stability poor.In addition, in materials synthesis side
Face, the synthesis of nickel cobalt double-hydroxide is often limited to the hydro-thermal method of HTHP, the method such as chemical precipitation or electro-deposition.Although adopting
The characteristics of material prepared with these methods has high specific capacitance, but there is synthesis condition harshness, generated time is long, synthesis side
The shortcomings of method is cumbersome or synthetic quantity is few.2 points based on more than, it is badly in need of the double hydrogen-oxygens of nickel cobalt of the synthesis with high circulation stability at present
The preparation method of compound electrode material and its simple and effective.
The content of the invention
It is an object of the invention to the nickel cobalt double-hydroxide of the synthesizing high-stability of high-efficient simple energy, to solve to deposit at present
Nickel cobalt double-hydroxide stability it is poor, the shortcomings of synthetic method is complicated cumbersome.
To reach above-mentioned purpose, the invention provides a kind of nickel of the preparation high stability α phase structures of nickel cobalt high-efficiency and economic
Cobalt double-hydroxide, specific technical scheme：
Super capacitor anode material nickel cobalt double-hydroxide, be a kind of ultrathin nanometer piece assembling by no more than 10nm and
Into 3D flower-like microsphere structures, belong to α phase lamellar compounds, interlamellar spacing is
The step Fast back-projection algorithm high stability α type nickel cobalt double-hydroxides of microwave one comprise the following steps：
(1) metal precursor salt is dissolved in deionized water, obtains mixed liquor, stirred
(2) a certain amount of urea of addition stirs as precipitating reagent in above-mentioned mixed liquor
(3) above-mentioned mixed liquor is placed in microwave synthesizer, carries out precipitation reaction.
(4) aging of product after reaction terminates, is washed, and is filtered, and is dried, is obtained the α phase nickel cobalts with high circulation stability
Double-hydroxide microballoon.
It is preferred that, the metal precursor is the one or more in Ni and Co water soluble salt；It is furthermore preferred that the gold
Category presoma is NiCl2·6H2O,CoCl2·6H2O one or two
It is preferred that, the metal precursor solution concentration is 0.01-0.1mol/L；It is furthermore preferred that the metal precursor
Concentration is 0.04-0.06mol/L.
It is preferred that, the urea precipitation agent is 4-20 with metal precursor mol ratio；It is furthermore preferred that the urea precipitation agent
It is 10-20. with metal precursor mol ratio
It is preferred that, the microwave generated time is 8-120min, and reaction temperature is 70-100 DEG C；It is furthermore preferred that described micro-
Ripple generated time is 15-60min, and reaction temperature is 90-100 DEG C.
The α type nickel cobalt double-hydroxides Forming Mechanism can as described below, in microwave synthesizer, urea heated portion
Hydrolysis produces OH-And CNO-, specific reaction equation is as follows：
NH2CONH2→NH4 ++CNO-
CNO-+3H2O→HCO3 -+NH4 ++OH-
NH2CONH2+H2O→2NH3+CO2
NH3+H2O→NH4 ++2OH-
During hydrolysis of urea, metal cation and OH-Reaction forms α type layered metal hydroxides, intercalating ions
For OH-And CNO-。
Brief description of the drawings
Fig. 1 (a) is the XRD of three-dimensional flower-shaped nickel hydroxide microballoon among embodiment 1, and products therefrom is the hydrogen-oxygen of pure α phases
Change nickel.
Fig. 1 (b) is the XRD of three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon among embodiment 2, and products therefrom is pure α phases
Nickel cobalt double-hydroxide.
Fig. 1 (c) is the XRD of three-dimensional flower-shaped cobalt hydroxide microballoon among embodiment 3, and products therefrom is the hydrogen-oxygen of pure α phases
Change cobalt.
Fig. 2 (a), (d) scheme for the SEM of the three-dimensional flower-shaped nickel hydroxide microballoon of embodiment 1.
Fig. 2 (b), (e) scheme for the SEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2.
Fig. 2 (c), (f) scheme for the SEM of the three-dimensional flower-shaped cobalt hydroxide microballoon of embodiment 3.
Fig. 3 (a), (d) scheme for the SEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 4.
Fig. 3 (b), (e) scheme for the SEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2.
Fig. 3 (c), (f) scheme for the SEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 5.
Fig. 4 (a), (b) scheme for the TEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2.
Fig. 4 (c), (d) scheme for the HRTEM of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2.
Fig. 5 is cyclic voltammetric of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2 under 10mV/s sweep speed
Curve.
Fig. 6 is that charge-discharge test of the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2 under different current densities is bent
Line.
Fig. 7 be the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2 under 10A/g current densities it is continuous 2000 circle fill
Discharge stability test result.
Fig. 8 is the three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of embodiment 2 the 1st circle and the 2000th under 10A/g current densities
The charge-discharge test curve of circle.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to limit only to explain the present invention
The fixed present invention.
Embodiment 1
(1) take 714mg NiCl26HO and 3.6g urea to be dissolved in 60ml deionized waters, stir 20min, disperse it
Uniformly.
(2) mixed liquor is transferred to 100mL there-necked flasks, and be placed in microwave synthesizer, it is indirectly cold in there-necked flask
Solidifying pipe, a side joint condenser pipe, opposite side rubber stopper seal.Agitator built in microwave synthesizer.
(3) microwave synthesizer power 300W is set, the reaction time is 30min, 100 DEG C of reaction temperature.Set after parameter,
Microwave synthesizer is opened to be reacted.
(4) reaction is precipitated after terminating, and is washed with deionized after cool aging 1h for several times, product is obtained after drying.
Products therefrom is the nickel hydroxide of pure α phases, in such as Fig. 1 shown in curve (a)；Fig. 2 (a) and (d) are three-dimensional flower-shaped hydrogen
The SEM figures of nickel oxide micro-sphere structure
Embodiment 2
The flower-shaped nickel cobalt double-hydroxide microballoon of microwave one-step synthesis 3-dimensional
(1) take 357mg CoCl26HO, 357mg NiCl26HO and 3.6g urea to be dissolved in 60ml deionized waters, stir
20min is mixed, it is uniformly dispersed.
(2) mixed liquor is transferred to 100mL there-necked flasks, and be placed in microwave synthesizer, it is indirectly cold in there-necked flask
Solidifying pipe, a side joint condenser pipe, opposite side rubber stopper seal.Agitator built in microwave synthesizer
(3) microwave synthesizer power 300W is set, the reaction time is 30min, 100 DEG C of reaction temperature.Set after parameter,
Microwave synthesizer is opened to be reacted.
Reaction is precipitated after terminating, and is washed with deionized after cool aging 1h for several times, product is obtained after drying.
Products therefrom is the nickel cobalt double-hydroxide of pure α phases, in such as Fig. 1 shown in curve (b)；Fig. 2 (b) and (e), Fig. 3 (b)
For the SEM of three-dimensional flower-shaped nickel cobalt double-hydroxide micro-sphere structure scheme (e).Fig. 3 (b) and (e).Fig. 4 (a) and (b) are three-dimensional flower
The TEM figures of shape nickel cobalt double-hydroxide micro-sphere structure, the nanometer sheet thickness of composition micro-sphere structure is less than 10nm.Fig. 4 (c) and (d)
Scheme for the HRTEM of three-dimensional flower-shaped nickel cobalt double-hydroxide micro-sphere structure.
Embodiment 3
The flower-shaped cobalt hydroxide microballoon of microwave one-step synthesis 3-dimensional
(1) take 714mg CoCl26HO and 3.6g urea to be dissolved in 60ml deionized waters, stir 20min, disperse it
Uniformly.
(2) mixed liquor is transferred to 100mL there-necked flasks, and be placed in microwave synthesizer, it is indirectly cold in there-necked flask
Solidifying pipe, a side joint condenser pipe, opposite side rubber stopper seal.Agitator built in microwave synthesizer
(3) microwave synthesizer power 300W is set, the reaction time is 30min, 100 DEG C of reaction temperature.Set after parameter,
Microwave synthesizer is opened to be reacted.
Reaction is precipitated after terminating, and is washed with deionized after cool aging 1h for several times, product is obtained after drying.
Products therefrom is the cobalt hydroxide of pure α phases, in such as Fig. 1 shown in curve (c)；Fig. 2 (c) and (f) are three-dimensional flower-shaped hydroxide
The SEM figures of cobalt micro-sphere structure
Embodiment 4
The flower-shaped nickel cobalt double-hydroxide microballoon of microwave one-step synthesis 3-dimensional
(1) take 357mg CoCl26HO, 357mg NiCl26HO and 3.6g urea to be dissolved in 60ml deionized waters, stir
20min is mixed, it is uniformly dispersed.
(2) mixed liquor is transferred to 100mL there-necked flasks, and be placed in microwave synthesizer, it is indirectly cold in there-necked flask
Solidifying pipe, a side joint condenser pipe, opposite side rubber stopper seal.Agitator built in microwave synthesizer
(3) microwave synthesizer power 300W is set, the reaction time is 8min, 100 DEG C of reaction temperature.Set after parameter,
Microwave synthesizer is opened to be reacted.
Reaction is precipitated after terminating, and is washed with deionized after cool aging 1h for several times, product is obtained after drying.
Fig. 3 (a) and the SEM figures that (d) is the three-dimensional flower-shaped nickel cobalt double-hydroxide micro-sphere structure that 8min microwaves are synthesized.
Embodiment 5
The flower-shaped nickel cobalt double-hydroxide microballoon of microwave one-step synthesis 3-dimensional.
357mg CoCl26HO are taken, 357mg NiCl26HO and 3.6g urea is dissolved in 60ml deionized waters, stirred
20min, makes it be uniformly dispersed.
Mixed liquor is transferred to 100mL there-necked flasks, and is placed in microwave synthesizer, indirect condensing in there-necked flask
Pipe, a side joint condenser pipe, opposite side rubber stopper seal.Agitator built in microwave synthesizer
Microwave synthesizer power 300W is set, the reaction time is 120min, 100 DEG C of reaction temperature.Set after parameter, open
Microwave synthesizer is opened to be reacted.
Reaction is precipitated after terminating, and is washed with deionized after cool aging 1h for several times, product is obtained after drying.
Fig. 3 (c) and the SEM figures that (f) is the three-dimensional flower-shaped nickel cobalt double-hydroxide micro-sphere structure that 120min microwaves are synthesized.
Using the nickel cobalt double-hydroxide prepared as positive electrode, following electrochemistry is carried out to it by following experimental procedure
Performance test.
Working electrode preparation method：By nickel cobalt double-hydroxide powder and acetylene black and PVDF according to 8：1：1 mixing, with
NMP is solvent, and grinding forms slurry, and slurry is coated in 1cm × 1cm foamed nickel current collector, and sample is dried at 60 DEG C
After 24h, in 10MPa lower sheetings.
Test system uses three electrode test systems, and reference electrode is Hg/HgO, is graphite flake to electrode, and electrolyte is 6M's
KOH, is tested using CHI660E type electrochemical workstations.
Cyclic voltammetry is carried out under 0-0.6V, and sweep speed is 10m V/s, and test result is as shown in Figure 5.
Constant current charge-discharge test is tested under different current densities respectively, and test result is as shown in Figure 6.Calculating is obtained
Specific capacitance under 1,2,5,10,15,20A/g current densities be respectively 1120,1117,1075,996,948,892F/g.Electric current
Density increases to 10A/g from 1A/g, and specific capacitance keeps 88.9%, increases to 20A/g, keeps 79.6%, illustrates that the material has
Excellent high rate performance.
Stability test uses continuous constant current charge-discharge test method, and carrying out 2000 to material in 10A/g encloses charge and discharge electrical measurement
Examination, test result is as shown in Figure 7.Test result shows that specific capacitance does not decay in test process, but gradually increases,
After terminating to 2000 circle tests, specific capacitance increases to the 1220F/g of the 2000th circle from the 996F/g of the 1st circle.Illustrate that microwave is synthesized
α type nickel cobalt double-hydroxides there is outstanding stable circulation performance.
Fig. 8 be shown the 1st circle and the 2000th circle charge-discharge test curve ratio compared with.After illustrating stability test, than electricity
Appearance does not decay to be increased on the contrary.
Result above shows, the α type nickel cobalts with high stability energy can be prepared by easy microwave synthesis method
Double-hydroxide, for super capacitor anode material, shows good overall performance.Our method can also be applied to
The synthesis of other inorganic nano materials, so as to apply in catalysis, the field such as electrochemistry.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent and improvement made within refreshing and principle etc., should be included within the scope of the present invention.
Claims (6)
1. a kind of super capacitor anode material, it is characterised in that：The three-dimensional flower-shaped nickel cobalt double-hydroxide microballoon of α phases belongs to cyanogen
The lamellar compound of acid radical anion intercalation, interlamellar spacing isMicroballoon is made up of a large amount of ultrathin nanometer pieces, nanoscale twins thickness
Less than 10nm；Its specific capacitance stable operation of the stability test of the circle of progress 2000 circulation does not decay under 10A/g high current densities,
Specific capacitance value is also had increased slightly with circulation, and the 1220F/g of the 2000th circle is increased to from the 996F/g of the 1st circle.
2. super capacitor anode material according to claim 1, it is characterised in that：By the following microwave reinforced system synthesized
Preparation Method is prepared, a certain amount of cobalt salt, and a certain amount of nickel salt and excessive urea are dissolved in deionized water, and stirring is equal
It is even, solution is placed in microwave synthesizer, synthetic reaction is carried out at 50-150 DEG C, the product after terminating is reacted through aging, filters,
Washing, is dried to obtain the nickel cobalt double-hydroxide of three-dimensional flower-shaped micro-sphere structure.
3. the super capacitor anode material according to claim 1, nickel salt is nickel chloride, nickel nitrate, nickel sulfate, acetic acid
One kind or mixture in the nickel salts such as nickel；Cobalt salt is one kind or mixed in the cobalt salts such as cobalt chloride, cobalt nitrate, cobaltous sulfate, cobalt acetate
Compound.
4. the super capacitor anode material according to claim 1, urea is (20 with metal ion ratio：1) arrive
(60：1).
5. the super capacitor anode material according to claim 1, reaction temperature is 50 DEG C -150 DEG C.
6. the super capacitor anode material prepared according to claim 1, it is characterised in that：Kept in electro-chemical test excellent
Different stability, 2000 are carried out under 10A/g current densities and encloses cyclical stabilities test, specific capacitance do not decay, and specific capacitance is from the 1st
The 996F/g of circle increases to the 1220F/g of the 2000th circle.
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Cited By (4)
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| CN108987121A (en) * | 2018-07-26 | 2018-12-11 | 电子科技大学 | A kind of quick method for preparing NiCo-LDH electrode material for super capacitor |
| CN109650465A (en) * | 2018-12-25 | 2019-04-19 | 四川大学 | Flower and preparation method thereof in a kind of nickel cobalt duplex metal hydroxide nanometer piece |
| CN109772336A (en) * | 2019-03-05 | 2019-05-21 | 浙江工业大学 | A kind of porous double-metal hydroxide catalyst and its preparation method and application for the oxidation of electro-catalysis alcohols selectivity |
| CN112279308A (en) * | 2020-10-15 | 2021-01-29 | 南昌大学 | Method for preparing high-energy-storage nickel-cobalt hydroxide electrode material in large batch |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987121A (en) * | 2018-07-26 | 2018-12-11 | 电子科技大学 | A kind of quick method for preparing NiCo-LDH electrode material for super capacitor |
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| CN109772336A (en) * | 2019-03-05 | 2019-05-21 | 浙江工业大学 | A kind of porous double-metal hydroxide catalyst and its preparation method and application for the oxidation of electro-catalysis alcohols selectivity |
| CN112279308A (en) * | 2020-10-15 | 2021-01-29 | 南昌大学 | Method for preparing high-energy-storage nickel-cobalt hydroxide electrode material in large batch |
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