CN106847541A - A kind of CoAl LDH@NF combination electrode materials of carbon coating and preparation method thereof - Google Patents
A kind of CoAl LDH@NF combination electrode materials of carbon coating and preparation method thereof Download PDFInfo
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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
- H01G11/32—Carbon-based
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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
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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
- H01G11/84—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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
CoAl LDH@NF combination electrode materials the invention discloses a kind of carbon coating and preparation method thereof.First respectively with cobalt nitrate and aluminum nitrate as cobalt source and silicon source, nickel foam is substrate to the inventive method, and Co Al LDH@NF are obtained after a step hydro-thermal；Then with glucose or sucrose as carbon source, Co Al LDH@NF are coated, then carry out hydro-thermal process and obtain Co Al LDH@NF@C.The present invention uses substep hydro-thermal seasoning, and preparation technology and required equipment are simple, and raw material sources are abundant and reaction temperature is relatively low, it is not necessary to high temperature cabonization, it is easy to accomplish large-scale production；Not only heat endurance is good, crystallization degree is high for the Co Al LDH@NF@C composites that the inventive method is obtained, and specific surface area is big, and morphology controllable is strong, is one of preferable energy and material.
Description
Technical field
The invention belongs to materialogy technical field, it is related to a kind of three-dimensional hierarchical structure combination electrode material, specifically
A kind of CoAl-LDH@NF combination electrode materials of carbon coating and preparation method thereof.
Background technology
The development of human survival and society all be unable to do without the energy, and the energy is one of important foundation of Economic Development.It is long
Since phase, the mankind use the fossil fuel with oil, coal, the big energy of natural gas three as representative so that greenhouse effects and environment are dirty
Dye is progressively aggravated.Continuing to develop for society, the mankind continue to increase to the demand of the energy, and traditional non-renewable energy resources such as stone
Oil, coal etc., cannot meet human wants.Therefore, new renewable and clean energy resource is developed extremely urgent.At present,
Develop or the novel energy developed is including wind energy, solar energy, Hydrogen Energy etc..In the utilization of new energy, the green of energy
Storage is also indispensable important step.New first throwing of the power vehicle (super capacity public transport car) during Shanghai World's Fair
Enter to use, then indicate reaching its maturity for super capacitor technology.
Current most commercialized electrode material is mainly the carbon material of Large ratio surface, but its energy density compared with
Low, limitation is used on a large scale.And double-metal hydroxide be a kind of structure height in order and with the material of various excellent properties
Material, the space structure of its uniqueness not only determines itself excellent chemical and physical features, meanwhile, variable valency in laminate it is cloudy from
Son more produces pseudo capacitance high to provide substantial amounts of electro-chemical activity site, close with the energy higher than carbon material
Degree, and its layer structure can provide well-proportioned dispersion liquid for transition metal ion so that have in electrochemistry well
Application prospect.But existing bimetallic layered hydroxide technology of preparing easily causes the reunion of particle, the ratio of material is reduced
Surface area, causes electrolyte to be maximized with electroactive component and contacts, and mass transfer rate and electron transfer rate are affected.Cause
This, builds three-dimensional cavity structural material, so can not only make material be difficult to reunite, and good dispersion, specific surface area is big, Er Qiegeng
Be conducive to improving its mass transfer rate and electron transfer rate.So as to significantly affect its super capacitor performance.
The content of the invention
For above-mentioned technical problem, it is an object of the invention to provide a kind of CoAl-LDH@NF combination electrodes of carbon coating
Material and preparation method thereof.The inventive method can solve that double-metal hydroxide electric conductivity of the prior art is bad, use glue
The shortcoming of glutinous agent etc., while environment will not be caused harm, with good cyclical stability.
In the present invention, first with nickel foam as substrate, CoAl-LDH@NF will be obtained after cobalt source and the step hydro-thermal of silicon source one；
Then CoAl-LDH@NF are coated with carbon source, then carries out the CoAl-LDH@NF combination electrode materials that hydro-thermal process obtains carbon coating
(CoAl-LDH@NF@C).The present invention uses substep hydro-thermal-seasoning, by controlling CoAl mass ratioes, the hydro-thermal reaction time and temperature
Degree, the concentration of carbon source, prepare the CoA-LDH@NF@C of three-dimensional hierarchical structure.
Technical solution of the present invention is specifically described as follows.
The present invention provides a kind of preparation method of the CoAl-LDH@NF combination electrode materials of carbon coating, comprises the following steps that：
(1) nickel foam is pre-processed
(2) CoAl-LDH@NF are prepared
First, at room temperature, cobalt source, silicon source, ammonium fluoride, urea and deionized water are mixed, obtains mixed solution；So
Afterwards, in above-mentioned mixed solution being moved into autoclave, and step (1) nickel foam that obtains of pretreatment is added thereto to, is carried out
Hydro-thermal reaction；After reaction terminates, room temperature, washing foam nickel, drying are naturally cooled to；
(3) CoAl-LDH@NF@C are prepared
First, carbon source and deionized water stirring and dissolving are made solution under room temperature condition；Then above-mentioned solution is moved into
In autoclave, and the nickel foam that step (2) is obtained is added thereto to, carries out hydro-thermal reaction；After reaction terminates, natural cooling
To room temperature, washing foam nickel, vacuum drying obtain the CoAl-LDH@NF combination electrode materials of carbon coating.
In above-mentioned steps (1), the method pre-processed to nickel foam is as follows：First cut nickel foam in flakes, then successively
With deionized water, acetone, ethanol, deionized water supersound washing, finally it is vacuum dried.
In above-mentioned steps (2), cobalt source is cobalt nitrate；Silicon source is aluminum nitrate.
In above-mentioned steps (2), the mass ratio of cobalt source and silicon source is 5:1-1:Between 1, the mass body of cobalt source and deionized water
Product is than being 1:30~2:3mg/ml.
In above-mentioned steps (2), the mass ratio of cobalt source and urea is 1:1-1:Between 5, the mass ratio of cobalt source and ammonium fluoride exists
6:1-15:Between 1, mixing time is 5-15min；Ammonium fluoride prepares the pattern of material for control, and urea is alkali source.
In above-mentioned steps (2), hydrothermal temperature is 90-120 DEG C, and the hydro-thermal reaction time is 12-24h；Drying temperature is 60-90
DEG C, drying time is 6-24h.
In above-mentioned steps (3), carbon source is sucrose or glucose.
In above-mentioned steps (3), the mass ratio of cobalt source and carbon source is 1:20-1:150；The quality volume of deionized water and carbon source
Than=1：1-1：10ml/mg；Mixing time is 15-30min.
In above-mentioned steps (3), hydrothermal temperature is 160-180 DEG C, and the hydro-thermal reaction time is 12-18h, vacuum drying temperature
It is 40-60 DEG C to spend, and drying time is 6-24h.
The present invention also provides a kind of CoAl-LDH@NF combination electrode materials of carbon coating that above-mentioned preparation method is obtained.
Compared to the prior art, the beneficial effects of the present invention are：
The present invention is using substep hydro-thermal-seasoning, and preparation technology and required equipment are simple, and raw material sources are abundant and react temperature
Degree is relatively low, it is not necessary to high temperature cabonization, it is easy to accomplish large-scale production；The CoAl-LDH@NF@C obtained by the method for the present invention
Composite takes full advantage of the synergy of layered metal double-hydroxide, nickel foam and carbon, overcomes leading for simple LDH
Shortcoming electrical and that cycle performance is poor, independent carbon material energy density is low, not only heat endurance is good, crystallization degree is high, and circulation is steady
Qualitative and good rate capability, is one of preferable energy and material with specific capacitance higher.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the CoAl-LDH@NF combination electrode materials of the gained of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the CoAl-LDH@NF of the gained of embodiment 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of the CoAl-LDH@NF@C of the gained of embodiment 2.
Fig. 4 is the CoAl-LDH@NF@C electrochemical property test figures of the gained of embodiment 2.
Fig. 5 is the XRD of the CoAl-LDH@NF@C powder of the gained of embodiment 2.
Fig. 6 is the scanning electron microscope (SEM) photograph of the CoAl-LDH@NF of the gained of embodiment 3.
Fig. 7 is the scanning electron microscope (SEM) photograph of the CoAl-LDH@NF@C of the gained of embodiment 4.
Specific embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not intended to limit the present invention.
Embodiment 1
A kind of method of the CoAl-LDH@NF combination electrode materials and its preparation of carbon coating, comprises the following steps：
(1) pretreatment of nickel foam
A., nickel foam is cut into the shape of 1cm × 3cm × 1cm, is surpassed with deionized water, acetone, ethanol, deionized water successively
Sound washs each 15min, then (mass percent concentration of described acetone is 60~98%, and ethanol is to be washed with deionized 2 times
Absolute ethyl alcohol)；
B. and then it is vacuum dried 12h under the conditions of 60 DEG C.
(2) CoAl-LDH@NF are prepared
A. first at room temperature, according to mass ratio, by 2mg cobalt nitrates, 2mg aluminum nitrates, 10mg urea, 0.33mg ammonium fluorides
It is added in beaker with 30ml deionized waters, magnetic agitation 5min is to mixing substantially uniformity；
B. in immigration polytetrafluoroethyllining lining stainless steel autoclave；Then by step 1) pre-process the nickel foam for obtaining
Tiltedly put in a kettle., 90 DEG C of baking box reaction 12h are put into after tightening；
C. room temperature is naturally cooled to after, with deionized water and ethanol successively washing foam nickel 3-4 times；
D. 6h is finally dried at 60 DEG C, that is, obtains CoAl-LDH NF composites.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, to the CoAl- of above-mentioned gained
LDH@NF combination electrode material powder is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in figure 1, as can be seen from Figure 1 CoAl-
LDH is packed together, but still can be seen to be the CoAl double-metal hydroxides of sheet, has been indicated above successfully preparing
CoAl-LDH@NF three-dimensional hierarchical structure materials.
(3) CoAl-LDH@NF@C are prepared
A. the glucose of 300mg and 30ml deionized waters are added in beaker container at ambient temperature, magnetic agitation
15min is to being completely dissolved；
B. in moving it into polytetrafluoroethylene (PTFE) autoclave again, by step 2) nickel foam that obtains tiltedly is placed on reactor
In, 12h in 160 DEG C of baking boxs is placed on after tightening, room temperature is naturally cooled to afterwards, successively with deionized water and ethanol washing foam nickel
3-4 times；
C. 6h is vacuum dried under the conditions of 40 DEG C, that is, obtains the CoAl-LDH NF combination electrode materials of carbon coating.
Electrochemical property test：
Under 1mol/L KOH electrolyte conditions, normal electrode is inertia Pt electrodes, and reference electrode is Ag/AgCl electrodes,
Working electrode is the Pt nets of carrying active substance, with three-electrode system in electrochemical workstation and the electricity of blue electric system test material
Chemical property.The result of material of the present invention is represented, is 1Ag in electric current-1In sweeping the stable circulation linearity curve under speed, the specific volume of material
Amount is changed greatly, but can also be protruded it and had good cyclical stability, and in 1Ag-1There is 1210.3F during constant current charge-discharge
g-1Specific capacity, circulation 2000 times after still maintain nearly 83% specific capacity.
Embodiment 2
A kind of method of the CoAl-LDH@NF combination electrode materials and its preparation of carbon coating, comprises the following steps：
(1) pretreatment of nickel foam
A., nickel foam is cut into the shape of 1cm × 3cm × 1cm, is surpassed with deionized water, acetone, ethanol, deionized water successively
Sound washs each 15min, then (mass percent concentration of described acetone is 60~98%, and ethanol is to be washed with deionized 2 times
Absolute ethyl alcohol)；
B. and then it is vacuum dried 12h under the conditions of 60 DEG C.
(2) CoAl-LDH@NF are prepared
A. first at room temperature, according to mass ratio, by 10mg cobalt nitrates, 5mg aluminum nitrates, 20mg urea, 1.25mg fluorinations
Ammonium and 40ml deionized waters are added in beaker, and magnetic agitation 10min is to mixing substantially uniformity；
B. in immigration polytetrafluoroethyllining lining stainless steel autoclave；Then by step 1) pre-process the nickel foam for obtaining
Tiltedly put in a kettle., 100 DEG C of baking box reaction 18h are put into after tightening；
C. room temperature is naturally cooled to after, with deionized water and ethanol successively washing foam nickel 3-4 times；
D. 12h is finally dried at 70 DEG C, that is, obtains CoAl-LDH NF composites.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, to above-mentioned CoAl-LDH@NF materials
Feed powder end is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in Figure 2.As can be seen from Figure 2 the CoAl-LDH of sheet is more equal
Grow on the surface of nickel foam evenly.
(3) CoAl-LDH@NF@C are prepared
A. the glucose of 360mg and 40ml deionized waters are added in beaker container at ambient temperature, magnetic agitation
20min is to being completely dissolved；
B. in moving it into polytetrafluoroethylene (PTFE) autoclave again, by step 2) nickel foam that obtains tiltedly is placed on reactor
In, 14h in 170 DEG C of baking boxs is placed on after tightening, room temperature is naturally cooled to afterwards, successively with deionized water and ethanol washing foam nickel
3-4 times；
C. 12h is vacuum dried under the conditions of 50 DEG C, that is, obtains the CoAl-LDH NF combination electrode materials of carbon coating.
Fig. 3 is the surface sweeping electron microscope of CoAl-LDH@NF@C powder.As can be seen from Figure 3 carbon more equably CoAl- long
The surface of LDH.Fig. 5 is the XRD of CoAl-LDH@NF@C, the as can be seen from Figure 5 successful preparation of the composite, and
There is good crystallinity.
With embodiment 1, Fig. 4 is the stable circulation performance figure of CoAl-LDH@NF@C powder to electrochemical property test method.Knot
Fruit shows that in the charging and discharging curve of different current densities, composite can be in 1Ag-1The cyclical stability tested under electric current, it is bent
Line finds that what change is smaller, and prominent its has good cyclical stability, and in 1Ag-1Have during constant current charge-discharge
1305.3F g-1Specific capacity, circulation 2000 times after maintain nearly 87% specific capacity.
Embodiment 3
A kind of method of the CoAl-LDH@NF combination electrode materials and its preparation of carbon coating, comprises the following steps：
(1) pretreatment of nickel foam
A., nickel foam is cut into the shape of 1cm × 3cm × 1cm, is surpassed with deionized water, acetone, ethanol, deionized water successively
Sound washs each 15min, then (mass percent concentration of described acetone is 60~98%, and ethanol is to be washed with deionized 2 times
Absolute ethyl alcohol)；
B. and then it is vacuum dried 12h under the conditions of 60 DEG C.
(2) CoAl-LDH@NF are prepared
A. first at room temperature, according to mass ratio, by 15mg cobalt nitrates, 8mg aluminum nitrates, 45mg urea, 1.5mg ammonium fluorides
It is added in beaker with 50ml deionized waters, magnetic agitation 10min is to mixing substantially uniformity；
B. in immigration polytetrafluoroethyllining lining stainless steel autoclave；Then by step 1) pre-process the nickel foam for obtaining
Tiltedly put in a kettle., 110 DEG C of baking box reaction 18h are put into after tightening；
C. room temperature is naturally cooled to after, with deionized water and ethanol successively washing foam nickel 3-4 times；
D. 18h is finally dried at 80 DEG C, that is, obtains CoAl-LDH NF composites.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, Fig. 6 is sweeping for CoAl-LDH@NF
Electron microscope is retouched, by can be seen that the CoAl-LDH of sheet in Fig. 6, laminated structure has a certain degree of damage, but successfully makes
It is standby go out CoAl-LDH@NF three-dimensional composite materials.
(3) CoAl-LDH@NF@C are prepared
A. the glucose of 400mg and 50ml deionized waters are added in beaker container at ambient temperature, magnetic agitation
25min is to being completely dissolved；
B. in moving it into polytetrafluoroethylene (PTFE) autoclave again, by step 2) nickel foam that obtains tiltedly is placed on reactor
In, 16h in 170 DEG C of baking boxs is placed on after tightening, room temperature is naturally cooled to afterwards, successively with deionized water and ethanol washing foam nickel
3-4 times；
C. 18h is vacuum dried under the conditions of 50 DEG C, that is, obtains the combination electrode material of carbon coating.
As a result electrochemical property test method shows with embodiment 1, in the charging and discharging curve of different current densities, tool
There is specific capacity and its stability higher, and in 1Ag-1There is 935.4F g during constant current charge-discharge-1Specific capacity, circulation
Nearly 82% specific capacity is still maintained after 2000 times.
Embodiment 4
A kind of method of the CoAl-LDH@NF combination electrode materials and its preparation of carbon coating, comprises the following steps：
(1) pretreatment of nickel foam
A., nickel foam is cut into the shape of 1cm × 3cm × 1cm, is surpassed with deionized water, acetone, ethanol, deionized water successively
Sound washs each 15min, then (mass percent concentration of described acetone is 60~98%, and ethanol is to be washed with deionized 2 times
Absolute ethyl alcohol)；
B. and then it is vacuum dried 12h under the conditions of 60 DEG C.
(2) CoAl-LDH@NF are prepared
A. first at room temperature, according to mass ratio, by 20mg cobalt nitrates, 10mg aluminum nitrates, 80mg urea, 3.5mg fluorinations
Ammonium and 60ml deionized waters are added in beaker, and magnetic agitation 15min is to mixing substantially uniformity；
B. in immigration polytetrafluoroethyllining lining stainless steel autoclave；Then by step 1) pre-process the nickel foam for obtaining
Tiltedly put in a kettle., 120 DEG C of baking box reaction 24h are put into after tightening；
C. room temperature is naturally cooled to after, with deionized water and ethanol successively washing foam nickel 3-4 times；
D. 24h is finally dried at 90 DEG C, that is, obtains CoAl-LDH NF composites.
(3) CoAl-LDH@NF@C are prepared
A. the glucose of 480mg and 60ml deionized waters are added in beaker container at ambient temperature, magnetic agitation
30min is to being completely dissolved；
B. in moving it into polytetrafluoroethylene (PTFE) autoclave again, by step 2) nickel foam that obtains tiltedly is placed on reactor
In, 18h in 180 DEG C of baking boxs is placed on after tightening, room temperature is naturally cooled to afterwards, successively with deionized water and ethanol washing foam nickel
3-4 times；
C. 24h is vacuum dried under the conditions of 60 DEG C, that is, obtains the CoAl-LDH NF combination electrode materials of carbon coating.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, Fig. 7 is CoAl-LDH@NF@C
Scanning electron microscope (SEM) photograph, by can be seen that carbon is successfully coated on above CoAl-LDH@NF in Fig. 7, but carbon is completely by CoAl-
LDH is covered；
As a result electrochemical property test method shows with embodiment 1, in the charging and discharging curve of different current densities, tool
There is specific capacity and its stability higher, and in 1Ag-1There is 930F g during constant current charge-discharge-1Specific capacity, circulation
Nearly 81% specific capacity is still maintained after 2000 times.
In sum, the method institute of a kind of CoAl-LDH@NF combination electrode materials of carbon coating of the invention and its preparation
The CoAl-LDH@NF@C of the different-shape for obtaining, so as to influence their chemical property different.In 1mol/L KOH electrolyte bars
Under part, with three-electrode system in electrochemical workstation and the chemical property of blue electric system test material, prepared electrochemistry
The best composite of performance can be in 1Ag-1The cyclical stability tested under electric current, curve finds that what change is smaller, prominent
It has good cyclical stability, and in 1Ag-1There is 1305.3F g during constant current charge-discharge-1Specific capacity, circulation
Nearly 87% specific capacity is maintained after 2000 times, with good cyclical stability, in 10Ag-1High current density under, still
Nearly 67% electric capacity is so maintained, with good high rate performance, is taken full advantage of with the netted high surface area of 3 D stereo
Nickel foam, carbon material and transition metal layered double-hydroxide synergy, while the homogenous material for overcoming is used as electrode
Defect.
The above is only specifically enumerating for embodiments of the present invention, and according to appointing that technical scheme is made
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (10)
1. the preparation method of the CoAl-LDH@NF combination electrode materials of a kind of carbon coating, it is characterised in that comprise the following steps that：
(1) nickel foam is pre-processed
(2) CoAl-LDH@NF are prepared
First, at room temperature, cobalt source, silicon source, ammonium fluoride, urea and deionized water are mixed, obtains mixed solution；
Then, in above-mentioned mixed solution being moved into autoclave, and it is added thereto to step (1) foam that obtains of pretreatment
Nickel, carries out hydro-thermal reaction；After reaction terminates, room temperature, washing foam nickel, drying are naturally cooled to；
(3) CoAl-LDH@NF@C are prepared
First, carbon source and deionized water stirring and dissolving are made solution under room temperature condition；Then above-mentioned solution is moved into high pressure
In reactor, and the nickel foam that step (2) is obtained is added thereto to, carries out hydro-thermal reaction；After reaction terminates, room is naturally cooled to
Temperature, washing foam nickel, vacuum drying, obtains the CoAl-LDH@NF combination electrode materials of carbon coating.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), the method pre-processed to nickel foam
It is as follows：First cut nickel foam in flakes, deionized water, acetone, ethanol, deionized water supersound washing, last vacuum are then used successively
Dry.
3. preparation method as claimed in claim 1, it is characterised in that in step (2), cobalt source is cobalt nitrate；Silicon source is nitric acid
Aluminium.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), the mass ratio of cobalt source and silicon source is 5:1-
1:Between 1, the mass volume ratio of cobalt source and deionized water is 1:30~2:3mg/ml.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), the mass ratio of cobalt source and urea is 1:1-
1:Between 5, the mass ratio of cobalt source and ammonium fluoride is 6:1-15:Between 1, mixing time is 5-15min.
6. preparation method as claimed in claim 1, it is characterised in that in step (2), hydrothermal temperature is 90-120 DEG C, hydro-thermal
Reaction time is 12-24h；Drying temperature is 60-90 DEG C, and drying time is 6-24h.
7. preparation method as claimed in claim 1, it is characterised in that in step (3), carbon source is sucrose or glucose.
8. preparation method as claimed in claim 1, it is characterised in that in step (3), the mass ratio of cobalt source and carbon source is 1:
20-1:150；Volume mass ratio=1 of deionized water and carbon source：1-1：10ml/mg；Mixing time is 15-30min.
9. preparation method as claimed in claim 1, it is characterised in that in step (3), hydrothermal temperature is 160-180 DEG C,
The hydro-thermal reaction time is 12-18h, and vacuum drying temperature is 40-60 DEG C, and drying time is 6-24h.
10. a kind of CoAl-LDH@NF combination electrode materials of the carbon coating that preparation method as described in one of claim 1-9 is obtained
Material.
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| CN107265572A (en) * | 2017-06-23 | 2017-10-20 | 中国科学院生态环境研究中心 | A kind of ternary metal oxide membrane electrode and its production and use |
| CN108615610A (en) * | 2018-04-23 | 2018-10-02 | 上海应用技术大学 | A method of using nickel foam as substrate growth in situ cobalt manganese double-metal hydroxide composite material |
| CN109767924A (en) * | 2019-02-16 | 2019-05-17 | 江苏大学 | A kind of LDH based super capacitor combination electrode material and preparation method and purposes |
| CN110257858A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Ag/CoAl-LDH/ nickel foam NF multilevel structure combination electrode material and preparation method thereof |
| CN110257859A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Co2P/Ni2P/Al2O3/ NF multilevel structure combination electrode and preparation method thereof |
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| 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 |
| CN107244700B (en) * | 2017-06-16 | 2020-03-06 | 合肥工业大学 | Fluorinated hydroxyl nickel cobalt nano material for super capacitor and preparation method thereof |
| CN107265572A (en) * | 2017-06-23 | 2017-10-20 | 中国科学院生态环境研究中心 | A kind of ternary metal oxide membrane electrode and its production and use |
| CN107265572B (en) * | 2017-06-23 | 2021-01-12 | 中国科学院生态环境研究中心 | Ternary metal oxide membrane electrode and preparation method and application thereof |
| CN108615610A (en) * | 2018-04-23 | 2018-10-02 | 上海应用技术大学 | A method of using nickel foam as substrate growth in situ cobalt manganese double-metal hydroxide composite material |
| CN110846679A (en) * | 2018-08-20 | 2020-02-28 | 南京理工大学 | Preparation method of flower-ball-shaped cobalt-aluminum sulfide |
| CN109767924A (en) * | 2019-02-16 | 2019-05-17 | 江苏大学 | A kind of LDH based super capacitor combination electrode material and preparation method and purposes |
| CN110257858A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Ag/CoAl-LDH/ nickel foam NF multilevel structure combination electrode material and preparation method thereof |
| CN110257859A (en) * | 2019-06-28 | 2019-09-20 | 青岛科技大学 | A kind of Co2P/Ni2P/Al2O3/ NF multilevel structure combination electrode and preparation method thereof |
| CN110257858B (en) * | 2019-06-28 | 2021-02-26 | 青岛科技大学 | Ag/CoAl-LDH/foamed nickel NF multi-level structure composite electrode material and preparation method thereof |
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