CN109243852A - A kind of cobalt nickel bimetal selenides/graphene complex electrode material - Google Patents
A kind of cobalt nickel bimetal selenides/graphene complex electrode material Download PDFInfo
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- CN109243852A CN109243852A CN201811352935.0A CN201811352935A CN109243852A CN 109243852 A CN109243852 A CN 109243852A CN 201811352935 A CN201811352935 A CN 201811352935A CN 109243852 A CN109243852 A CN 109243852A
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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
- H01G11/30—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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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 discloses a kind of cobalt nickel bimetal selenides/graphene complex electrode materials, belong to the preparation field of electrode for super capacitor material.Preparation method includes following procedure: graphene oxide (GO) being added in ethylene glycol solution, ultrasonic disperse keeps GO evenly dispersed in ethylene glycol solution；Polyvinylpyrrolidone (PVP), four hydration cobalt acetates, four hydration nickel acetates are added in the GO dispersion liquid of above-mentioned configuration, round-bottomed flask progress oil bath reaction is transferred to after ultrasonic disperse dissolution and centrifuge washing is dry；The dry product of centrifuge washing after oil bath and sodium selenite, hydrazine hydrate are carried out hydro-thermal selenization and obtain cobalt nickel bimetal selenides/graphene complex electrode material.The cobalt nickel selenides nano flake of a large amount of size uniformities is uniformly supported on graphene-based bottom on the electrode material microscopic appearance of preparation, while specific capacitance with higher, excellent high rate performance.
Description
Technical field
The invention belongs to the preparation fields of electrode for super capacitor material, and in particular to a kind of cobalt nickel bimetal selenizing
Object/graphene complex electrode material and preparation method thereof.
Background technique
Supercapacitor due to its power density with higher, excellent high rate performance, fast charge/discharge rate,
The excellent features such as the cycle life of overlength, quick charge transport rate and low-maintenance cost, can be applicable to energy storage device,
On dynamic power system and many electronic equipments, the extensive concern from industry and academia is attracted.Super electricity
The performance of container with its used in electrode material it is closely related, currently used three kinds of electrode materials (carbon material, metal oxidation
Object/hydroxide, conducting polymer) respectively there are advantage and disadvantage: carbon material simple production process, cheap, good cycle, but compare
Capacity is lower；Metal oxide/hydroxide and conducting polymer specific capacity are high but at high cost, cyclical stability is bad.Research
Show to carry out above-mentioned different types of electrode material compound the shortcomings that can not only making up homogenous material, while can also be real
The mutual supplement with each other's advantages of existing material property, obtains the super capacitor for having high capacity, excellent cycling and high rate performance concurrently.
Transient metal sulfide has very high theoretical specific capacity and good high rate performance, while electric conductivity is oxidation
Hundred times of object are a kind of electrode material for super capacitor with bright prospects.But exist simultaneously the disadvantage of cyclical stability difference.
Metal selenide is similar with the testing sulphide of the metal in structure and in nature, but has better metallic character and electronegativity,
To have better electric conductivity, there is superior super capacitor performance.Carbon material (active carbon, graphene, carbon fiber etc.)
With excellent electric conductivity and cyclical stability, but specific capacitance is low.It is compound as transition metal selenides using graphene
Base material can use the synergistic effect of the two, prepare the electrode material of high performance supercapacitor.
Summary of the invention
The purpose of the present invention is to provide a kind of cobalt nickel bimetal selenides/graphene complex electrode material and its preparations
Method.To further increase cobalt nickel bimetal selenides/graphene complex super capacitor performance, in hydro-thermal selenization mistake
Cheng Zhong promotes electrode material electric conductivity, to improve super capacitor performance by cobalt-nickel oxide selenizing at cobalt nickel selenides.System
The cobalt nickel selenides nano flake of a large amount of size uniformities is uniformly supported on graphene-based bottom on standby electrode material microscopic appearance
On, while specific capacitance with higher, excellent high rate performance.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of cobalt nickel bimetal selenides/graphene complex electrode material, includes the following steps:
(1) quantitative graphene oxide (GO) is added in ethylene glycol solution, ultrasonic disperse, so that graphene oxide (GO) exists
It is evenly dispersed in ethylene glycol solution；
(2) by quantitative polyvinylpyrrolidone (PVP), four hydration cobalt acetate (Co (CH3COO)2·4H2O), four hydration acetic acid
Nickel (Ni (CH3COO)2·4H2O it) is added in step (1) solution, the above mixed liquor is transferred to round bottom after completely dissolution by ultrasound
The reaction of oil bath pan finish application bath is placed in flask, it is multiple with dehydrated alcohol centrifuge washing then after it naturally cools to room temperature,
The product after washing is finally placed in drying；
(3) product of step (2) centrifugal drying and sodium selenite, hydrazine hydrate are subjected to hydro-thermal selenization, then to its nature
It is multiple with dehydrated alcohol centrifuge washing after being cooled to room temperature, the double gold of cobalt nickel are finally prepared in the product drying after washing
Belong to selenides/graphene complex electrode material.
A kind of cobalt nickel bimetal selenides/graphene complex electrode material, preparation method comprise the following specific steps that:
(1) 5 ~ 30 mg graphene oxides are weighed to be added in 30 ~ 100 mL ethylene glycol solutions, ultrasonic disperse 30 minutes, make to aoxidize
Graphene is uniformly dispersed in ethylene glycol solution；
(2) polyvinylpyrrolidone of 0.1 ~ 0.5 g, four water of four the hydration cobalt acetates and 60 ~ 250 mg of 60 ~ 250 mg are weighed
It closes nickel acetate to be added in step (1) solution, is transferred in round-bottomed flask and is placed in 100 ~ 300 on oil bath pan after ultrasonic dissolution
DEG C oil bath is reacted 1 ~ 5 hour, finally, after it naturally cools to room temperature, with dehydrated alcohol centrifuge washing 4-5 times, after washing
Product drying；
(3) product and 30 ~ 300 mg sodium selenites of 10 ~ 80 mg step (2) centrifugal dryings, 2 ~ 20 mL hydrazine hydrates, magnetic are weighed
Power stirs to form uniform mixed liquor, be placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle carry out selenylation reaction, hydro-thermal selenizing temperature be 100 ~
180 DEG C, 6 ~ 24 hours are kept the temperature, finally naturally cools to room temperature to it, with dehydrated alcohol centrifuge washing, it is double to obtain cobalt nickel for drying
Metal selenide/graphene complex electrode material.
The cobalt nickel selenides nano flake of electrode material obtained by the present invention, a large amount of size uniformities is uniformly supported on stone
On mertenyl bottom.Hydro-thermal selenization simultaneously, improves the super capacitor performance of electrode material.
Remarkable advantage of the invention is:
(1) present invention carries out selenizing using hydro-thermal method, avoids other selenization process bring selenium powders residual using sodium selenite as selenium source
It stays, promotes the purity of selenides.Selenizing simultaneously improves the electric conductivity of electrode material, promotes the supercapacitive of electrode material
Energy.
(2) cobalt nickel selenides nano flake prepared by the present invention is uniformly supported on graphene-based bottom, realizes counterfeit electricity
The combination of appearance and electric double layer, can use its synergistic effect and constructs high-performance super capacitor electrode material.
(3) electrode material prepared by the present invention specific capacitance under 1 A/g current density charge and discharge is 916.7 F/g, 10 A/
It is 84.6% that specific capacitance conservation rate is (forthright again) under g current density charge and discharge, shows prepared electrode material ratio with higher
Capacitor, excellent high rate performance.
Detailed description of the invention
Fig. 1 is cobalt nickel bimetal selenides/graphene complex electrode material XRD diffracting spectrum made from embodiment 1.
Fig. 2 is cobalt nickel bimetal selenides/graphene complex electrode material scanning electron microscope (SEM) photograph made from embodiment 1；
As can be seen from the figure cobalt nickel selenides nano flake is uniformly supported on graphene-based bottom.
Fig. 3 is the figure of cobalt nickel bimetal selenides/graphene complex electrode material EDS made from embodiment 1；From figure
It can be seen that prepared electrode material mainly contains the elements such as Co, Ni, Se, C, show through the method successfully by electrode material selenium
Change.
Fig. 4 is the figure of cobalt nickel bimetal selenides/graphene complex electrode material GCD made from embodiment 1；From figure
It can be seen that the charge and discharge under different current densities of prepared electrode material all show higher coulombic efficiency.
Specific embodiment
The present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to following reality
Apply example.
Embodiment 1
A kind of preparation method of cobalt nickel bimetal selenides/graphene complex electrode material, specific steps are as follows:
(1) 10 mg graphene oxides (GO, self-control) are weighed to be added in 50 mL ethylene glycol, ultrasonic disperse 30 minutes, GO are made to exist
It is uniformly dispersed in ethylene glycol；
(2) polyvinylpyrrolidone (PVP) of 0.3 g, the four hydration cobalt acetate (Co (CH of 125 mg are weighed3COO)2·4H2O)
Nickel acetate (Ni (CH is hydrated with the four of 124 mg3COO)2·4H2O it) is added in step (1) solution, ultrasound sufficiently dissolution, then
The above mixed liquor is transferred in round-bottomed flask and is placed in 150 DEG C oil baths reaction 5 hours on oil bath pan.Finally, naturally cold to it
But to after room temperature, with dehydrated alcohol centrifuge washing 4 times, the product after washing is placed in electric drying oven with forced convection and is dried；
(3) product and 100 mg sodium selenites of 15 mg step (2) centrifugal dryings, 5 mL hydrazine hydrates are weighed, magnetic agitation is formed
Uniform mixed liquor is placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and carries out selenylation reaction, and hydro-thermal selenizing temperature is 150 DEG C, and heat preservation 12 is small
When, room temperature finally is naturally cooled to it, cobalt nickel bimetal selenides/graphene complex electrode material is prepared.
Embodiment 2
A kind of preparation method of cobalt nickel bimetal selenides/graphene complex electrode material, specific steps are as follows:
(1) 5 mg graphene oxides (GO, self-control) are weighed to be added in 30 mL ethylene glycol, ultrasonic disperse 30 minutes, make GO in second
It is uniformly dispersed in glycol；
(2) polyvinylpyrrolidone (PVP) of 0.5 g, the four hydration cobalt acetate (Co (CH of 250 mg are weighed3COO)2·4H2O)
Nickel acetate (Ni (CH is hydrated with the four of 250 mg3COO)2·4H2O it) is added in step (1) solution, ultrasound sufficiently dissolution, then
The above mixed liquor is transferred in round-bottomed flask and is placed in 250 DEG C oil baths reaction 1 hour on oil bath pan.Finally, naturally cold to it
But to after room temperature, with dehydrated alcohol centrifuge washing 5 times, the product after washing is placed in electric drying oven with forced convection and is dried；
(3) product and 250 mg sodium selenites of 30 mg step (2) centrifugal dryings, 20 mL hydrazine hydrates, magnetic agitation shape are weighed
At uniform mixed liquor, it is placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and carries out selenylation reaction, hydro-thermal selenizing temperature is 120 DEG C, heat preservation 24
Hour, room temperature finally is naturally cooled to it, cobalt nickel bimetal selenides/graphene complex electrode material is prepared.
Embodiment 3
A kind of preparation method of cobalt nickel bimetal selenides/graphene complex electrode material, specific steps are as follows:
(1) 20 mg graphene oxides (GO, self-control) are weighed to be added in 100 mL ethylene glycol, ultrasonic disperse 30 minutes, GO are made to exist
It is uniformly dispersed in ethylene glycol；
(2) polyvinylpyrrolidone (PVP) of 0.1 g, the four hydration cobalt acetate (Co (CH of 60 mg are weighed3COO)2·4H2O) and
The four hydration nickel acetate (Ni (CH of 70 mg3COO)2·4H2O it) is added in step (1) solution, ultrasound sufficiently dissolution then will
The above mixed liquor, which is transferred in round-bottomed flask, is placed in 200 DEG C oil baths reaction 1 hour on oil bath pan.Finally, to its natural cooling
To after room temperature, with dehydrated alcohol centrifuge washing 5 times, the product after washing is placed in electric drying oven with forced convection and is dried；
(3) product and 300 mg sodium selenites of 50 mg step (2) centrifugal dryings, 20 mL hydrazine hydrates, magnetic agitation shape are weighed
At uniform mixed liquor, it is placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and carries out selenylation reaction, hydro-thermal selenizing temperature is 180 DEG C, heat preservation 18
Hour, room temperature finally is naturally cooled to it, cobalt nickel bimetal selenides/graphene complex electrode material is prepared.
The test of super capacitor performance
By cobalt nickel bimetal selenides/graphene complex electrode material of above method preparation, acetylene black (conductive agent) and gather
Vinylidene (PVDF, binder) is in 8:1:1(mass ratio) ratio addition mixing after be evenly coated in nickel foam as work
Electrode, using platinum filament as to electrode, using mercury oxidation mercury electrode as reference electrode, using 3 mol/L KOH solutions as electrolyte,
Measure under electrode material three-electrode system made from embodiment 1,2,3 specific capacitance under 1 A/g current density be respectively 916.7,
907.4,910.7 F/g, specific capacitance conservation rate (forthright again) is respectively 84.6,83.8,84.2% under 10 A/g current densities.
The electrode material chemical property for showing prepared by embodiment 1 is best.
Comparative example 1
The method for preparing cobalt nickel selenides electrode material:
2.8 g sodium hydroxides, 0.3 g selenium powder are weighed, are added in 25 mL deionized waters, magnetic agitation 1 hour, are transferred to water
In hot kettle, it is placed in 200 DEG C hydro-thermal reaction 20 hours in baking oven；Then step (2) centrifugal drying in 15 mg embodiments 1 is weighed again
Product be added in the above water heating kettle, the above mixture is placed in 140 DEG C hydro-thermal reaction 12 hours in baking oven, finally to it
After naturally cooling to room temperature, with dehydrated alcohol centrifuge washing 4 times, the product after washing is placed in electric drying oven with forced convection and is dried
It is dry.
The cobalt nickel selenides electrode material of above method preparation is subjected to super capacitor performance according to above-mentioned same method
Test, measuring under electrode material three-electrode system made from comparative example 1 specific capacitance under 1 A/g current density is 616 F/g, 10
Specific capacitance conservation rate (forthright again) is only 78.1% under A/g current density.
Since preparation method of the invention carries out hydro-thermal selenizing using sodium selenite, selenium powder is avoided to remain, obtained selenizing
Object purity is higher, while the introducing of carbon material (graphene), improves the electric conductivity of electrode material.Compared to comparative example 1, the present invention
Cobalt nickel bimetal selenides/graphene complex electrode material of preparation is forthright with higher specific capacitance and more good times
Energy.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (2)
1. a kind of cobalt nickel bimetal selenides/graphene complex electrode material, which is characterized in that preparation method includes following
Step:
(1) it adds graphene oxide into ethylene glycol solution, ultrasonic disperse, so that graphene oxide is equal in ethylene glycol solution
Even dispersion；
(2) polyvinylpyrrolidone, four hydration cobalt acetates, four hydration nickel acetates are added in step (1) solution, ultrasound is sufficiently
It is transferred to after dissolution in round-bottomed flask and is placed in the reaction of oil bath pan finish application bath, then after it naturally cools to room temperature, use is anhydrous
Ethyl alcohol centrifuge washing is multiple, finally dries the product after washing；
(3) product of step (2) centrifugal drying and sodium selenite, hydrazine hydrate are subjected to hydro-thermal selenization, then to its nature
It is multiple with dehydrated alcohol centrifuge washing after being cooled to room temperature, the double gold of cobalt nickel are finally prepared in the product drying after washing
Belong to selenides/graphene complex electrode material.
2. cobalt nickel bimetal selenides/graphene complex electrode material according to claim 1, it is characterised in that: its
Preparation method comprises the following specific steps that:
(1) 5 ~ 30 mg graphene oxides are weighed to be added in 30 ~ 100 mL ethylene glycol solutions, ultrasonic disperse 30 minutes, make to aoxidize
Graphene is uniformly dispersed in ethylene glycol solution；
(2) polyvinylpyrrolidone of 0.1 ~ 0.5 g, four water of four the hydration cobalt acetates and 60 ~ 250 mg of 60 ~ 250 mg are weighed
It closes nickel acetate to be added in step (1) solution, is transferred in round-bottomed flask and is placed in 100 ~ 300 on oil bath pan after ultrasonic dissolution
DEG C oil bath is reacted 1 ~ 5 hour, finally, after it naturally cools to room temperature, with dehydrated alcohol centrifuge washing 4-5 times, after washing
Product drying；
(3) product and 30 ~ 300 mg sodium selenites of 10 ~ 80 mg step (2) centrifugal dryings, 2 ~ 20 mL hydrazine hydrates, magnetic are weighed
Power stirs to form uniform mixed liquor, be placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle carry out selenylation reaction, hydro-thermal selenizing temperature be 100 ~
180 DEG C, 6 ~ 24 hours are kept the temperature, finally naturally cools to room temperature to it, with dehydrated alcohol centrifuge washing, it is double to obtain cobalt nickel for drying
Metal selenide/graphene complex electrode material.
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| CN110354876A (en) * | 2019-07-19 | 2019-10-22 | 南京理工大学 | A kind of hollow Ni2P/Co2P/Fe2The preparation method of the nano combined elctro-catalyst of P |
| CN110400926A (en) * | 2019-08-07 | 2019-11-01 | 福州大学 | A kind of nitrogen-doped carbon cladding two-phase is interspersed type nickel cobalt bimetallic selenides electrode material and preparation method thereof |
| CN110581026A (en) * | 2019-09-03 | 2019-12-17 | 滨州学院 | Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof |
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Application publication date: 20190118 |