CN107492452A - The preparation method of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor - Google Patents
The preparation method of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor Download PDFInfo
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- CN107492452A CN107492452A CN201710651371.XA CN201710651371A CN107492452A CN 107492452 A CN107492452 A CN 107492452A CN 201710651371 A CN201710651371 A CN 201710651371A CN 107492452 A CN107492452 A CN 107492452A
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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
- H01G11/22—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
- H01G11/26—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
-
- 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 kind of preparation method of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor, belong to the preparing technical field of electrode of super capacitor.Technical scheme main points are：Using nickel foam, cobalt nitrate and urea as raw material, in 100 180 DEG C of 12h of hydro-thermal reaction 5, deposition growing is crosslinked the cellular multilevel hierarchy cobalt nickel double-hydroxide presoma assembled by ultra-thin lamella in foam nickel base in hydrothermal reaction kettle, it is then immersed into sodium sulfide solution and carries out the secondary 36h of hydro-thermal reaction 3 in 100 180 DEG C, cobalt nickel double-hydroxide presoma is converted into sulfide is finally made by array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor of ultra-thin lamella crosslinking assembling.Active electrode obtained by the present invention can provide excellent electrode specific volume in the alkaline electrolyte, be provided simultaneously with significant high rate performance, show application potential of the active electrode in terms of electrochemical energy storage.
Description
Technical field
The invention belongs to the preparing technical field of electrode of super capacitor, and in particular to a kind of array-like multilevel hierarchy vulcanization
The preparation method of cobalt nickel/nickel foam electrode of super capacitor.
Background technology
Ultracapacitor is a kind of green, efficient electrochemical energy storing device.Compared to traditional secondary battery, ultracapacitor
There is higher power density and charge-discharge velocity, good circulation performance and safety, low stain, in portable electronic products and
The fields such as hybrid vehicle are used as supply unit, have a extensive future.According to energy storage principle, ultracapacitor mainly wraps
Double layer capacitor and pseudocapacitors are included, the former mainly stores electricity by physical absorption of the electrolyte ion on porous electrode surface
Lotus, there is the advantages of multiplying power and higher power density, but specific volume is relatively low；The latter mainly by active electrode material superficial layer and
The Reversible redox reaction of sub-surface layer（Fake capacitance）To store electric charge, its specific volume and energy density are higher, close to tradition two
Primary cell.By optimizing the architectural characteristic of electrode material, improving the electrochemical surface area of fake capacitance material can further optimize
The stored energy capacitance of capacitor.
Transient metal sulfide is a kind of important fake capacitance active material, has the oxidation higher than oxide material also
Former active and higher theoretical specific volume.The binary metal sulfide being made up of different transition metals can be by two kinds of metals not
Comparatively ideal specific volume is obtained with the synergy between the redox reaction between oxidation number and metallic element.This kind of two
In first metal sulfide, cobalt sulfide nickel receives much attention, and both elements are respectively provided with higher oxygen reducing activity, can provide significant
Specific volume.And then the accessible surface of active material can be effectively improved by Rational Path, structure low-dimensional unit mounting structure framework
Product, charge ion diffusion transport speed and fracture toughness, so as to obtain superior and balanced capacitive property.In addition, by this kind of group
Assembling structure binary metal sulfide is grown directly upon metal collector surface and is avoided that insulation adhesive in traditional electrode manufacturing process
The use of agent, the surface utilisation of active electrode can not only be improved to greatest extent, and can effectively reduce electric transmission impedance, from
And obtain optimal specific volume and high rate performance.
The content of the invention
Present invention solves the technical problem that it there is provided a kind of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam super capacitor
The preparation method of device electrode, this method pass through deposit cobalt nickel double-hydroxide forerunner using foamed nickel current collector as substrate and nickel source
Body and precipitation convert, and array-like multilevel hierarchy cobalt sulfide nickel/nickel foam ultracapacitor that assembling is crosslinked by ultra-thin lamella is made
Electrode, obtained active electrode can provide excellent electrode specific volume, be provided simultaneously with significant multiplying power in the alkaline electrolyte
Performance, show application potential of the active electrode in terms of electrochemical energy storage.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, array-like multilevel hierarchy cobalt sulfide nickel/foam
The preparation method of nickel electrode of super capacitor, it is characterised in that concretely comprise the following steps：Using nickel foam, cobalt nitrate and urea as raw material,
In 100-180 DEG C of hydro-thermal reaction 5-12h in hydrothermal reaction kettle, deposition growing is by ultra-thin lamella crosslinking group in foam nickel base
The cellular multilevel hierarchy cobalt nickel double-hydroxide presoma of dress, is then immersed into sodium sulfide solution in 100-180 DEG C
Secondary hydro-thermal reaction 3-36h is carried out, cobalt nickel double-hydroxide presoma is converted into sulfide, final be made is handed over by ultra-thin lamella
Join array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor of assembling.
Further preferably, the molar ratio of the integral molar quantity of the cobalt nitrate and urea and vulcanized sodium is 7:2-40, nitre
The molar ratio of sour cobalt and urea is 1:6-2:5, the size of foam nickel base is 10mm × 10mm × 1mm.
Further preferably, the preparation method of the array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor
Specific building-up process be：1-2mmol cobalt nitrates and 5-6mmol urea are dissolved in shape in 60mL deionized waters under agitation
Into mixed solution, then the mixed solution is transferred in hydrothermal reaction kettle, by the nickel foam that size is 10mm × 10mm × 1mm
Substrate 0.1mol/L dilute nitric acid solution etching processing 5min, washing are immersed in the mixed solution in hydrothermal reaction kettle after drying
In, in 150 DEG C of hydro-thermal reaction 12h, deposition growing is crosslinked the cellular multilevel hierarchy assembled by ultra-thin lamella in foam nickel base
Cobalt nickel double-hydroxide presoma, it is then immersed into 40mL 0.5mol/L sodium polysulfide solution and carries out two in 150 DEG C
Secondary hydro-thermal reaction 6h, cobalt nickel double-hydroxide presoma is converted into sulfide, final be made is crosslinked assembling by ultra-thin lamella
Array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor.
Being crosslinked by ultra-thin lamella in the array-like multilevel hierarchy cobalt sulfide nickel active material of assembling obtained by the present invention, its
Multilevel hierarchy can not only provide higher specific surface area, and its wider aperture is also beneficial to electrolyte ion to deep layer electrode table
The quick scattering and permeating in face and absorption, the relatively high electrochemical activity area and ionic conductivity of electrode are advantageous to obtain compared with Fabrication of High Specific Capacitance
And high rate performance.In addition, the crosslinking between primary piece layer unit can guarantee that it is good be conductively connected, while active material and foam
The good contact of Ni substrate also can effectively reduce electric charge transmission resistance, ensure the Quick Oxidation reduction reaction of electrode surface, these
Factor both contributes to improve electrode high rate performance, is relatively adapted to high current charge-discharge.In addition, the present invention utilizes two step hydro-thermal reaction systems
The technique for making array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor is simple, it is expected to makes height with fairly large
Performance ultracapacitor.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of active electrode obtained by the embodiment of the present invention 3；
Fig. 2 is charging and discharging curve of the active electrode under different current densities obtained by the embodiment of the present invention 2；
Fig. 3 is curve of double curvature of the active electrode under different current densities obtained by the embodiment of the present invention 3.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
5mmol urea is dissolved in 60mL deionized waters under the conditions of magnetic agitation and forms solution, is then transferred to the solution
In hydrothermal reaction kettle, the dust technology etching processing by size for 10mm × 10mm × 1mm foam nickel base 0.1mol/L
5min, and be immersed in after washing drying in the reaction solution in hydrothermal reaction kettle, in 180 DEG C of hydro-thermal reaction 5h in foam nickel base
Surface depositing nickel hydroxide, it is then immersed into 40mL 0.05mol/L sodium polysulfide solution in 150 DEG C of hydro-thermal reactions
6h, deposit nickel sulfide active material on foam nickel base surface through precipitation conversion and form active electrode.By prepared activity electricity
Pole is used as working electrode, makees auxiliary electrode with platinum foil, and HgO/Hg electrodes are reference electrode, immerses group in 2mol/L KOH electrolyte
Into three-electrode system, charge-discharge performance test is carried out in 0-0.5 potential windows（Fig. 2）, the specific volume under 1A/g current densities is
2357F/g。
Embodiment 2
1mmol cobalt nitrates and 6mmol urea are dissolved in 60mL deionized waters under the conditions of magnetic agitation and form mixed solution, so
The mixed solution is transferred in hydrothermal reaction kettle afterwards, by the foam nickel base 0.1mol/ that size is 10mm × 10mm × 1mm
L dust technology etching processing 5min, and be immersed in after washing drying in the mixed solution in hydrothermal reaction kettle, in 120 DEG C of hydro-thermals
React 5h and the cellular multilevel hierarchy cobalt nickel double-hydroxide presoma that assembling is crosslinked by ultra-thin lamella deposited in foam nickel surface,
Then put it into 40mL 1mol/L sodium sulfide solution, in 150 DEG C of hydro-thermal reaction 6h, by vulcanizing treatment in nickel foam
Substrate surface is formed forms active electrode by the array-like multilevel hierarchy cobalt sulfide nickel active material of ultra-thin lamella crosslinking assembling.Will
Prepared active electrode assembles three-electrode system test charge-discharge performance, electrode exists as working electrode according to embodiment 1
Specific volume under 1A/g current densities is up to 3730F/g（Fig. 2）.
Embodiment 3
1mmol cobalt nitrates and 6mmol urea are dissolved in 60mL deionized waters under the conditions of magnetic agitation and form mixed solution, so
The mixed solution is transferred in hydrothermal reaction kettle afterwards, by the foam nickel base 0.1mol/ that size is 10mm × 10mm × 1mm
L dust technology etching processing 5min, and be immersed in after washing drying in the mixed solution in hydrothermal reaction kettle, in 150 DEG C of hydro-thermals
React 12h and the cellular multilevel hierarchy cobalt nickel double-hydroxide forerunner that assembling is crosslinked by ultra-thin lamella is deposited in foam nickel surface
Body, then put it into 40mL 0.5mol/L sodium sulfide solution, in 150 DEG C of hydro-thermal reaction 6h, steeped by vulcanizing treatment
The Ni-based basal surface of foam is formed forms active electricity by the array-like multilevel hierarchy cobalt sulfide nickel active material of ultra-thin lamella crosslinking assembling
Pole（Fig. 1）.This kind of array-like multilevel hierarchy framework can be provided compared with high electrochemical activity area, while is also beneficial to the fast of electrolyte
Speed diffusion, can be provided compared with Fabrication of High Specific Capacitance and high rate performance simultaneously.Using prepared active electrode as working electrode, according to embodiment
1 assembling three-electrode system tests its chemical property, and the specific volume under 1A/g current densities is up to 4500F/g（Fig. 3）；In 1-
In 30A/g current density ranges, its specific volume conservation rate（Multiplying power）For 56%.
Embodiment 4
2mmol cobalt nitrates and 5mmol urea are dissolved in 60mL deionized waters under the conditions of magnetic agitation and form mixed solution, so
The mixed solution is transferred in hydrothermal reaction kettle afterwards, by the foam nickel base 0.1mol/ that size is 10mm × 10mm × 1mm
L dust technology etching processing 5min, and be immersed in after washing drying in the mixed solution in hydrothermal reaction kettle, in 180 DEG C of hydro-thermals
React 5h and the cellular multilevel hierarchy cobalt nickel double-hydroxide presoma that assembling is crosslinked by ultra-thin lamella deposited in foam nickel surface,
Then put it into 40mL 0.05mol/L sodium sulfide solution, in 150 DEG C of hydro-thermal reaction 6h, by vulcanizing treatment in foam
Ni-based basal surface is formed forms active electrode by the array-like multilevel hierarchy cobalt sulfide nickel active material of ultra-thin lamella crosslinking assembling.
Using prepared active electrode as working electrode, three-electrode system test chemical property is assembled according to embodiment 1, electrode exists
Specific volume under 1A/g current densities reaches 3125F/g.
By embodiment as can be seen that by regulate and control cobalt salt, urea and vulcanized sodium dosage and hydrothermal temperature,
The preparation conditions such as time, can Effective Regulation electrode specific volume and high rate performance.
Embodiment above describes the general principle of the present invention, main features and advantages, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (3)
1. the preparation method of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor, it is characterised in that specific step
Suddenly it is：Using nickel foam, cobalt nitrate and urea as raw material, in 100-180 DEG C of hydro-thermal reaction 5-12h in foam in hydrothermal reaction kettle
Deposition growing is crosslinked the double hydroxide presomas of cellular multilevel hierarchy cobalt nickel of assembling by ultra-thin lamella in nickel substrate, then by it
It is immersed in sodium sulfide solution and carries out secondary hydro-thermal reaction 3-36h in 100-180 DEG C, the double hydroxide presomas of cobalt nickel is converted into
Array-like multilevel hierarchy cobalt sulfide nickel/nickel foam super capacitor electrode that assembling is crosslinked by ultra-thin lamella is finally made in sulfide
Pole.
2. the preparation side of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor according to claim 1
Method, it is characterised in that：The integral molar quantity of the cobalt nitrate and urea and the molar ratio of vulcanized sodium are 7:2-40, cobalt nitrate with
The molar ratio of urea is 1:6-2:5, the size of foam nickel base is 10mm × 10mm × 1mm.
3. the preparation side of array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor according to claim 1
Method, it is characterised in that specifically building-up process is：1-2mmol cobalt nitrates and 5-6mmol urea are dissolved in 60mL under agitation
Mixed solution is formed in deionized water, then the mixed solution is transferred in hydrothermal reaction kettle, is 10mm × 10mm by size
× 1mm foam nickel base 0.1mol/L dilute nitric acid solution etching processing 5min, washing are immersed in hydro-thermal reaction after drying
In mixed solution in kettle, in 150 DEG C of hydro-thermal reaction 12h, deposition growing is crosslinked assembling by ultra-thin lamella in foam nickel base
The double hydroxide presomas of cellular multilevel hierarchy cobalt nickel, be then immersed into 40mL 0.5mol/L sodium sulfide solution in
150 DEG C carry out secondary hydro-thermal reaction 6h, and the double hydroxide presomas of cobalt nickel are converted into final be made of sulfide is handed over by ultra-thin lamella
Join array-like multilevel hierarchy cobalt sulfide nickel/nickel foam electrode of super capacitor of assembling.
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| CN108097270A (en) * | 2017-12-20 | 2018-06-01 | 青岛大学 | A kind of elctro-catalyst for being catalyzed water decomposition production hydrogen and its preparation method and application |
| CN108281292A (en) * | 2018-01-18 | 2018-07-13 | 济南大学 | A kind of preparation method and applications of Ni-Co-S nano needle arrays |
| CN108677191A (en) * | 2018-05-30 | 2018-10-19 | 大连交通大学 | A kind of nano wire skeleton three-dimensional porous foams nickel and preparation method thereof |
| CN108899214A (en) * | 2018-07-09 | 2018-11-27 | 吉林大学 | A kind of preparation method of sulfur modification metal hydroxides electrode material |
| CN109161925A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of preparation and Hydrogen Evolution Performance research of 3D structure Zn-Co-S nanocomposite |
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| CN114649150A (en) * | 2022-03-02 | 2022-06-21 | 江苏大学 | Three-dimensional silicon substrate/transition metal compound based composite electrode material, preparation method and application |
| CN114582636A (en) * | 2022-04-12 | 2022-06-03 | 桂林电子科技大学 | Sea urchin-shaped microsphere cobalt-nickel-based electrode material and preparation method and application thereof |
| CN114582636B (en) * | 2022-04-12 | 2023-12-12 | 桂林电子科技大学 | Sea urchin-shaped microsphere cobalt-nickel-based electrode material and preparation method and application thereof |
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Application publication date: 20171219 |