CN109243858A - A kind of preparation method of electrode material for super capacitor - Google Patents
A kind of preparation method of electrode material for super capacitor 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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- 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
- H01G11/84—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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Abstract
The invention discloses a kind of preparation methods of electrode material for super capacitor, comprising: by nickel sulfate NiSO4·6H2O, which is dissolved in deionized water, obtains the first solution；GO aqueous solution is added into the first solution under continuous agitation and obtains the second solution；Ammonia spirit is added into the second solution under continuous agitation and obtains third solution；Third solution is successively centrifuged, is washed, dry after obtain presoma Ni (OH)2/GO；By Ni (OH)2/ GO and glucose, which are dissolved in deionized water, obtains the 4th solution；The 4th uniformly mixed solution is successively dried, is heated, is calcined, cool down after obtain electrode material for super capacitor carbon coating NiO/ graphene NiO/rGO@C.NiO nano particle is uniformly distributed in electrode material for super capacitor NiO/rGO@C prepared by the present invention, GO provides active site for the preparation of NiO nano particle, reduce the reunion of NiO, glucose carbonization and rGO collaboration improve the electric conductivity of electrode material, therefore NiO/rGO C electrode material specific capacitance has obtained effective raising.
Description
Technical field
The present invention relates to the preparation field of capacitor electrode material more particularly to a kind of systems of electrode material for super capacitor
Preparation Method.
Background technique
With the rapid development of economy, the whole world needs to increase further to the energy, the increasingly consumption of non-renewable energy resources makes
A kind of economic, efficient, high performance energy-storage system, which must be studied, to be particularly important.Supercapacitor because of its high-energy density, fill
The electric time is short, long service life and get more and more people's extensive concerning.Based on energy storage mechanism, supercapacitor can be divided into two
Kind-electrochemical capacitor in double electrode layer and Faraday pseudo-capacitance device.Relative to the former, Faraday pseudo-capacitance device has higher ratio
Capacitor and energy density, are more suitable for practical application and commercialization.In Faraday pseudo-capacitance device electrode material, oxo transition metal
Compound, especially NiO have excellent redox and charge storage ability (theory specific capacitance 2584F/g under 0.5V voltage),
And earth reserves are big, low cost and studied extensively by researchers.But Faraday pseudo-capacitance device charge and discharge process one
As surface in electrode material or near surface occurs so that electrode body phase material is asked there are electro-chemical activity site utilization rate is low
Topic, NiO are no exception.In addition, NiO the problem of there is also poorly conductives.Therefore in majority research, NiO is not often expressed
High specific capacitance.
Currently, having certain methods to solve these problems.One is the NiO for constructing the nano-scale of different-shape, such as NiO
Nanometer sheet (S.Wu, et.al, J.Mater.Chem.A, 2016,4,9113), NiO nano particle (J.Lin, et.al,
Adv.Sci., 2018,5,1700687), NiO nanowire (V.Kannan, et.al, ACS Appl.Mater.Interfaces,
2016,8,17220) etc., to increase the specific surface area of NiO, the more electro-chemical activity sites of exposure.Another be with centainly
The conductive carbon of amount, such as redox graphene (rGO) (F.Luan, et.al, Nanoscale, 2013,5,7984), hollow carbon sphere
(S.Y.Kim, et.al, Energy Environm.Sci., 2015,8,188), carbon nanotube (Y.Bai, et.al,
J.Mater.Chem.A, 2014,2,3834) mixing such as improve its electric conductivity.In these conductive carbons, rGO is excellent because of its
Surface Physical Chemistry property and the specific capacitance for effectively improving combination electrode are considered as optimal conductive additive.However, in reality
In the research of border, the reduction process of the oxidation of precursor graphene (GO) of rGO needs accurate control, to reduce the stacking or increase of GO
The rGO of NiO is uniformly coated, and realizes the increase of combination electrode electric conductivity.Therefore, develop a kind of simple and easy, economical and effective mention
The method of high NiO/rGO electric conductivity and its specific capacitance is particularly important.
Summary of the invention
It is simple, economical super that the purpose of the present invention is to provide a kind of electric conductivity to improve, specific capacitance also effectively improves
Capacitor electrode material carbon coating NiO/ graphene NiO/rGO@C preparation method.
In order to achieve the above objectives, a kind of preparation method of electrode material for super capacitor, comprising steps of
By nickel sulfate NiSO4·6H2O, which is dissolved in deionized water, obtains the first solution；Under continuous agitation to
GO aqueous solution is added in one solution and obtains the second solution；Second solution is persistently stirred into 5-120min at room temperature.
Ammonia spirit is added into the second solution under continuous agitation and obtains third solution；By third solution in room
0.5-24h is persistently stirred under the conditions of temperature.
Third solution is successively centrifuged, is washed, dry after obtain presoma Ni (OH)2/ GO, wherein centrifugation turns
Speed is 3000-8000r/min；Washing is repeatedly to be washed with deionized water and ethyl alcohol；Drying is in air dry oven or vacuum drying
It is carried out in case, drying temperature is 40-80 DEG C.
By Ni (OH)2/ GO and glucose, which are dissolved in deionized water, obtains the 4th solution；By the 4th uniformly mixed solution
Successively be dried, heat, calcining, cool down after obtain electrode material for super capacitor carbon coating NiO/ graphene NiO/rGO@C,
Wherein, drying carries out in air dry oven or vacuum oven, and drying temperature is 40-80 DEG C；Being heated to be in temperature is 150-
6-24h is heated in 200 DEG C of polytetrafluoroethylene (PTFE) water heating kettle or in tube furnace；Calcining is the tube furnace for being 250-300 DEG C in temperature
Middle calcining 3-12h, the heating rate of tube furnace are 0.1-10 DEG C/min.
Preferably, lasting stirring carries out on magnetic stirring apparatus, mixing speed 300-1000r/min.
Preferably, NiSO in the second solution4·6H2O is 5-50mmol；Deionized water is 10-100mL；GO aqueous solution is
10-100mL, concentration 1-10mg/mL.
Preferably, ammonia spirit is 0.5-50mL in third solution；Second solution is 5-500mL, concentration 24-30%.
Preferably, the 4th glucose in solutions and Ni (OH)2/ GO mass ratio is 1:10-2:1.
Preferably, the adding manner of ammonia spirit is to be added dropwise, rate of addition 0.1-50mL/min.
Preferably, the environment for heating and calcining is inert atmosphere, and inert atmosphere is selected from nitrogen or argon gas.
The present invention has the advantages that prepared electrode material for super capacitor carbon coating NiO/ graphene NiO/rGO@C
Middle NiO nano particle is uniformly distributed, and GO provides active site for the preparation of NiO nano particle, reduces the reunion of NiO, grape
Sugar charcoal and rGO collaboration improve the electric conductivity of electrode material, therefore NiO/rGO@C electrode material specific capacitance has obtained effectively mentioning
It is high；NiO is uniformly distributed with the form of nanoparticles of~5nm or so in electrode material simultaneously.
Detailed description of the invention
In order to become apparent from the technical solution for illustrating the embodiment of the present invention, embodiment will be described below in it is required use it is attached
Figure is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this field
For those of ordinary skill, without creative efforts, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is a kind of preparation method flow chart of electrode material for super capacitor；
Fig. 2 is the TEM figure of the carbon coating NiO/ graphene NiO/rGO@C electrode material prepared in the embodiment of the present invention one；
Fig. 3 is the high-resolution of the carbon coating NiO/ graphene NiO/rGO@C electrode material prepared in the embodiment of the present invention one
TEM figure；
Fig. 4 is the carbon coating NiO/ graphene NiO/rGO@C electrode material difference electric current prepared in the embodiment of the present invention one
Specific capacitance figure under density.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Fig. 1 is a kind of preparation method flow chart of electrode material for super capacitor.As shown in Figure 1, a kind of supercapacitor
The preparation method of electrode material, comprising steps of
Step S101, by nickel sulfate NiSO4·6H2O, which is dissolved in deionized water, obtains the first solution；In lasting stirring
Under the conditions of into the first solution be added GO aqueous solution obtain the second solution.
Specifically, the second solution is persistently stirred into 5-120min at room temperature.
Ammonia spirit is added into the second solution under continuous agitation and obtains third solution by step S102.
Specifically, third solution is persistently stirred into 0.5-24h at room temperature.
Third solution is successively centrifuged, washed by step S103, dry after obtain presoma Ni (OH)2/GO。
Specifically, the revolving speed of centrifugation is 3000-8000r/min；Washing is repeatedly to be washed with deionized water and ethyl alcohol；It is dry
It is carried out in air dry oven or vacuum oven, drying temperature is 40-80 DEG C.
Step S104, by Ni (OH)2/ GO and glucose, which are dissolved in deionized water, obtains the 4th solution；It will be uniformly mixed
The 4th solution be successively dried, heat, calcining, cool down after obtain electrode material for super capacitor carbon coating NiO/ graphene
NiO/rGO@C。
Specifically, drying carries out in air dry oven or vacuum oven, and drying temperature is 40-80 DEG C；It is heated to be
6-24h is heated in the polytetrafluoroethylene (PTFE) water heating kettle that temperature is 150-200 DEG C or in tube furnace；It is 250-300 that calcining, which is in temperature,
DEG C tube furnace in calcine 3-12h, the heating rate of tube furnace is 0.1-10 DEG C/min.
Preferably, lasting stirring carries out on magnetic stirring apparatus, mixing speed 300-1000r/min.
Preferably, NiSO in the second solution4·6H2O is 5-50mmol；Deionized water is 10-100mL；GO aqueous solution is
10-100mL, concentration 1-10mg/mL.
Preferably, ammonia spirit is 0.5-50mL in third solution；Second solution is 5-500mL, concentration 24-30%.
Preferably, the 4th glucose in solutions and Ni (OH)2/ GO mass ratio is 1:10-2:1.
Preferably, the adding manner of ammonia spirit is to be added dropwise, rate of addition 0.1-50mL/min.
Preferably, the environment for heating and calcining is inert atmosphere, and inert atmosphere is selected from nitrogen or argon gas.
Embodiment one
Take 15mmol nickel sulfate NiSO4·6H2O is dissolved in 30mL deionized water, prepares the first solution of 0.5mol/L,
That is 1mg/mL GO aqueous solution 20mL is added under revolving speed 1000r/min stirring condition, continues to stir for nickel sulfate solution
30min。
Under revolving speed 1000r/min stirring condition, the ammonia spirit of 5mL26% is added dropwise in above-mentioned mixed solution,
3min is dripped, and continues to stir 60min.
After reaction, it is centrifuged, deionized water and ethyl alcohol wash three times respectively, are dried to obtain celadon Ni (OH)2/GO。
Take 400mg Ni (OH)2/ GO and 400mg glucose is placed in tube furnace in 2mL deionized water after mixing,
First 150 DEG C of heating 6h in a nitrogen atmosphere, then 300 DEG C of calcining 3h, heating rate are 1 DEG C/min, and cooling obtains carbon coating
NiO/ graphene NiO/rGO@C electrode material, equivalent series resistance are 0.63 Ω, the specific capacitance under different current densities
As shown in table 1 and Fig. 4, the carbonization and rGO for embodying glucose are effectively improved its specific capacitance.
Under the carbon coating NiO/ graphene NiO/rGO@C electrode material difference current density prepared in 1 embodiment one of table
Specific capacitance
The NiO/rGO@C electrode material prepared using projection electron microscope (model: JEM-2100F) shooting embodiment one
Its TEM figure is obtained, as shown in Fig. 2, embodying the thin layer pattern that NiO/rGO@C electrode material maintains rGO.
Further, the NiO/rGO@C prepared using projection electron microscope (model: JEM-2100F) shooting embodiment one
Electrode material obtains its high-resolution TEM figure, as shown in figure 3, the spacing of lattice of nano particle is~0.22nm and~0.24nm, it is right
(200) and (111) face for answering NiO illustrates the generation of NiO nano particle, NiO nanoparticle size~5nm, and is evenly distributed on
In NiO/rGO@C electrode material.
Embodiment two
Take 20mmol nickel sulfate NiSO4·6H2O is dissolved in 40mL deionized water, and the nickel sulfate for preparing 0.5mol/L is water-soluble
1mg/mL GO aqueous solution 20mL is added in liquid under revolving speed 1000r/min stirring condition, continues to stir 30min.
Under the conditions of revolving speed 1000r/min, the ammonia spirit of 10mL 26%, 5min drop are added dropwise in the above solution
It adds, continues to stir 120min.
After reaction, it is centrifuged, deionized water and ethyl alcohol wash three times respectively, are dried to obtain celadon Ni (OH)2/GO。
Take 400mg Ni (OH)2/ GO and 200mg glucose is placed in tube furnace in 2mL deionized water after mixing,
First 150 DEG C of heating 6h in a nitrogen atmosphere, then 300 DEG C of calcining 6h, heating rate are 0.5 DEG C/min, and cooling obtains carbon coating
NiO/ graphene NiO/rGO@C electrode material, equivalent series resistance are 0.65 Ω, the specific capacitance under different current densities
As shown in table 2.
Under the carbon coating NiO/ graphene NiO/rGO@C electrode material difference current density prepared in 2 embodiment two of table
Specific capacitance
The present invention provides a kind of preparation method of electrode material for super capacitor, prepared electrode of super capacitor material
NiO nano particle is uniformly distributed in material carbon coating NiO/ graphene NiO/rGO@C, and GO provides work for the preparation of NiO nano particle
Property site, reduce the reunion of NiO, glucose carbonization and rGO collaboration improve the electric conductivity of electrode material, therefore NiO/rGO C
Electrode material specific capacitance has obtained effective raising；NiO is uniform with the form of nanoparticles of~5nm or so in electrode material simultaneously
Distribution.
Above specific embodiment has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Illustrate, it should be understood that the above is only a specific embodiment of the invention, the protection model that is not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (10)
1. a kind of preparation method of electrode material for super capacitor, which is characterized in that comprising steps of
By nickel sulfate NiSO4·6H2O, which is dissolved in deionized water, obtains the first solution；It is molten to first under continuous agitation
GO aqueous solution is added in liquid and obtains the second solution；
Ammonia spirit is added into the second solution under continuous agitation and obtains third solution；
Third solution is successively centrifuged, is washed, dry after obtain presoma Ni (OH)2/GO；
By Ni (OH)2/ GO and glucose, which are dissolved in deionized water, obtains the 4th solution；Successively by the 4th uniformly mixed solution
Be dried, heat, calcining, cool down after obtain electrode material for super capacitor carbon coating NiO/ graphene NiO/rGO@C.
2. the method according to claim 1, wherein further comprising the steps of:
Second solution is persistently stirred into 5-120min at room temperature；
The third solution is persistently stirred into 0.5-24h at room temperature.
3. method according to claim 1 or 2, which is characterized in that the lasting stirring carries out on magnetic stirring apparatus, stirs
Mixing speed is 300-1000r/min.
4. the method according to claim 1, wherein NiSO in second solution4·6H2O is 5-50mmol；
Deionized water is 10-100mL；GO aqueous solution is 10-100mL, concentration 1-10mg/mL.
5. the method according to claim 1, wherein ammonia spirit is 0.5-50mL in the third solution；The
Two solution are 5-500mL, concentration 24-30%.
6. the method according to claim 1, wherein the adding manner of the ammonia spirit is dropwise addition, the drop
Acceleration is 0.1-50mL/min.
7. the method according to claim 1, wherein after the third solution is successively centrifuged, is washed, being dried
Obtain presoma Ni (OH)2The step of/GO, wherein
The revolving speed of the centrifugation is 3000-8000r/min；
The washing is repeatedly to be washed with deionized water and ethyl alcohol；
The drying carries out in air dry oven or vacuum oven, and drying temperature is 40-80 DEG C.
8. the method according to claim 1, wherein the 4th glucose in solutions and Ni (OH)2/ GO mass
Than for 1:10-2:1.
9. the method according to claim 1, wherein the 4th uniformly mixed solution be successively dried,
The step of obtaining electrode material for super capacitor carbon coating NiO/ graphene NiO/rGO@C after heating, calcining, cooling, wherein
The drying carries out in air dry oven or vacuum oven, and drying temperature is 40-80 DEG C；
It is described to be heated to be in the polytetrafluoroethylene (PTFE) water heating kettle that temperature is 150-200 DEG C or heat 6-24h in tube furnace；
To calcine 3-12h in the tube furnace that temperature is 250-300 DEG C, the heating rate of the tube furnace is 0.1- for the calcining
10℃/min。
10. according to the method described in claim 9, it is characterized in that, it is described heating and calcining environment be inert atmosphere, it is described
Inert atmosphere is selected from nitrogen or argon gas.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
| CN103219169A (en) * | 2013-03-29 | 2013-07-24 | 东华大学 | Preparation method for carbon-coated nickel oxide NiO/C as supercapacitor electrode material |
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- 2018-10-26 CN CN201811258340.9A patent/CN109243858B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
| CN103219169A (en) * | 2013-03-29 | 2013-07-24 | 东华大学 | Preparation method for carbon-coated nickel oxide NiO/C as supercapacitor electrode material |
Non-Patent Citations (2)
| Title |
|---|
| LEI YU等: "Fabrication of carbon-coated NiO supported on graphene for high performance supercapacitors", 《RSC ADVANCES》 * |
| MEILING ZHOU等: "The glucose-assisted synthesis of a grapheme nanosheet–NiO composite for high-performance supercapacitors", 《NEW J. CHEM.》 * |
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