CN103824705A - Preparation method of asymmetric supercapacitor of water system - Google Patents
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- CN103824705A CN103824705A CN201410086050.6A CN201410086050A CN103824705A CN 103824705 A CN103824705 A CN 103824705A CN 201410086050 A CN201410086050 A CN 201410086050A CN 103824705 A CN103824705 A CN 103824705A
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparation method of an asymmetric supercapacitor of a water system. The preparation method comprises the steps of (1) growing a NiCo2O4@CoxNi(1-x)(OH)2 core-shell nanosheet array on foamed nickel as a cathode material of a supercapacitor; (2) coating the foamed nickel with activated carbon CMK-3 as an anode material; (3) with a potassium hydroxide solution as an electrolyte solution, assembling the NiCo2O4@CoxNi(1-x)(OH)2 cathode material and the CMK-3 anode material to form the asymmetric supercapacitor. The NiCo2O4@CoxNi(1-x)(OH)2 electrode material prepared by the method has relatively high area specific capacitance up to 5.71F/cm<2>, and the obtained NiCo2O4@CoxNi(1-x)(OH)2//CMK-3 asymmetric supercapacitor of the water system has the voltage window of 1.6V and is high in energy density, good in stability and simple in preparation process.
Description
Technical field
The invention belongs to NiCo
2o
4ultracapacitor field, particularly a kind of preparation method of water system Asymmetric Supercapacitor.
Background technology
Ultracapacitor has great application prospect in mobile electronic device, mixed power electric car and a large amount of micro element etc., owing to thering is high power density, and long cycle life, safety, advantages of environment protection.NiCo
2o
4electrode material is subject to numerous researchers' extensive concern at present, is mainly because NiCo
2o
4have than NiO and Co
3o
4higher conductivity and electrochemical reaction activity.Therefore can be with NiCo
2o
4electrode material is used for as skeleton the other materials of growing, thereby can improve the conductivity of electrode material, and NiCo
2o
4based composites has cooperative effect and can improve the chemical property of combination electrode material.Recently, the verified NiCo that directly grows on the collectors such as nickel foam of relevant report
2o
4based combined electrode material can be avoided " extremely " volume occurring in traditional electrode material preparation process and cause declining than electric capacity.But up to the present the Area Ratio electric capacity of prepared electrode material still can not reach desirable requirement.
In order to improve the energy density of ultracapacitor of future generation, report at present and certified effective means is to carry high specific capacitance and voltage window.Although organic electrolyte can effectively improve voltage window, there is the weak ionic conductivity of an electrolyte, price is poisonous and limited its large-area business application.According to nearest report, a kind of effectively way is the asymmetric super capacitor of exploitation, and electrode two parts of its faraday's electrode by battery types and capacity type form.Asymmetric Supercapacitor can utilize the electrode material of two different voltage windows and increase voltage window to 2V, thereby can improve energy density.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of water system Asymmetric Supercapacitor, and the present invention has improved voltage window, further improves energy density, has overcome the defects such as traditional capacitor energy density is low.
The preparation method of a kind of water system Asymmetric Supercapacitor of the present invention, comprising:
(1) NiCo
2o
4@Co
xni
1-x(OH)
2preparation:
A ultrasonic cleaning nickel foam, to remove surperficial nickel oxide, obtains the nickel foam after cleaning;
B is by Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2o), cabaltous nitrate hexahydrate (Co (NO
3)
26H
2and ammonium nitrate (NH O)
4nO
3) be dissolved in the water, make mixed solution, wherein Ni (NO
3)
26H
2o and Co (NO
3)
26H
2the ratio of O mole is 1:2;
The nickel foam after above-mentioned cleaning is placed in the mixed solution that B obtains by C, is heated to 60-75 ℃, then utilizes electrochemical deposition method, under constant voltage condition, deposits 4-10min, obtains the nickel foam that contains sample;
D takes out the nickel foam that contains sample, washs and is dried respectively with deionized water and alcohol solvent, then puts into Muffle furnace and calcines, and calcination time is 60-240 minute, and calcining heat is 250-350 ℃, obtains NiCo
2o
4nano-chip arrays;
E is by above-mentioned NiCo
2o
4nano-chip arrays is placed in Ni (NO
3)
26H
2o and Co (NO
3)
26H
2in the mixed solution of O, then utilize electrochemical deposition method to deposit under constant voltage condition; After having reacted, product is used respectively to ethanol, deionized water rinsing for several times, finally, in 60 ℃ of dry 8-20 hour, obtain NiCo
2o
4@Co
xni
1-x(OH)
2positive electrode;
(2) preparation of active carbon CMK-3 negative material:
By CMK-3(Nanjing Xian Feng Nono-material Science & Technology Ltd.), acetylene black, binding agent mixes, then add ethanol and be stirred to and be mixed to get mixture completely, then said mixture is evenly coated in the nickel foam after cleaning, compressing tablet processing again after vacuumize, obtains CMK-3 negative material;
(3) NiCo
2o
4@Co
xni
1-x(OH)
2the assembling of //CMK-3 water system Asymmetric Supercapacitor:
Using potassium hydroxide solution as electrolyte, by above-mentioned NiCo
2o
4@Co
xni
1-x(OH)
2positive electrode and CMK-3 negative material are assembled into sandwich structure, and centre adds one deck barrier film.
The washing lotion adopting in ultrasonic cleaning described in step (1) A is 1M hydrochloric acid solution.
Ni (NO described in step (1) B
3)
26H
2the amount ratio of O and ammonium nitrate is 0.29g:0.08g.
Voltage described in step (1) C in electrochemical deposition method is-1V.
Ni (NO in step (1) E
3)
26H
2o and Co (NO
3)
26H
2the ratio of O is 1:10-10:1.
Voltage described in step (1) E in electrochemical deposition method is-1V.
The NiCo obtaining in step (1) D
2o
4nano-chip arrays is ultra-thin porous structure, sheet is thick~and 6nm, bore dia~5-20nm.
The NiCo obtaining in step (1) E
2o
4@Co
xni
1-x(OH)
2positive electrode is nucleocapsid structure.
The mass ratio of CMK-3, acetylene black and the binding agent described in step (2) is 85:15:5.
Described in step (3), the concentration of potassium hydroxide solution is 1mol/L, and vacuum drying temperature is 120 ℃, and the pressure in described compressing tablet processing is 10Mpa.
Beneficial effect:
The NiCo preparing by method of the present invention
2o
4@Co
xni
1-x(OH)
2electrode material has higher Area Ratio electric capacity (5.71F/cm
2), NiCo
2o
4@Co
xni
1-x(OH)
2//CMK-3 water system Asymmetric Supercapacitor voltage window can reach 1.6V, and energy density is high, good stability, and preparation technology is simple.
The reason that the present invention obtains above-mentioned beneficial effect can be summed up as following some: 1, the ultra-thin NiCo of porous
2o
4nanometer sheet has excellent conductivity, is not only conducive to electric transmission and storage, and can increase the specific activity surface area of electrode material, improves the utilance of material; 2, NiCo
2o
4and Co
xni
1-x(OH)
2are all electrode materials of chemical property excellence, the combination of the two has very strong cooperative effect, thereby can improve chemical property 3, the NiCo of overall electrode
2o
4@Co
xni
1-x(OH)
2electrode material is grown directly upon can avoid " dead volume " that in traditional electrode material preparation process, produce in nickel foam.
Accompanying drawing explanation
Fig. 1 is the NiCo that in the present invention prepared by embodiment 1
2o
4scanning electron microscope (SEM) photograph (a, b), transmission electron microscope picture (c, d), electron diffraction diagram (e), XRD schemes (f);
Fig. 2 is the NiCo that in the present invention prepared by embodiment 1
2o
4@Co
xni
1-x(OH)
2//CMK-3 water system Asymmetric Supercapacitor stability diagram;
Fig. 3 is two NiCo that in the present invention prepared by embodiment 1
2o
4@Co
xni
1-x(OH)
2the optical photograph of LED is lighted in the series connection of //CMK-3 water system Asymmetric Supercapacitor.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
A kind of NiCo
2o
4@Co
xni
1-x(OH)
2the preparation of //CMK-3 water system Asymmetric Supercapacitor, its characterization step is: 1) NiCo
2o
4@Co
xni
1-x(OH)
2preparation:
A puts into the nickel foam of suitable size to contain the ultrasonic cleaning of 1M hydrochloric acid solution, and object is to remove the nickel oxide on nickel foam surface.
B takes raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2o) 0.29g, cabaltous nitrate hexahydrate (Co (NO
3)
26H
2o) 0.58g and ammonium nitrate (NH
4nO
3) be dissolved in the water, and stir, make mixed solution, wherein Ni (NO
3)
26H
2o and Co (NO
3)
26H
2the ratio of O mole is 1:2, and ammonium nitrate is 0.08g.
C is placed in the nickel foam after above-mentioned cleaning the mixed solution of process B, is heated to 70 ℃, then utilizes electrochemical deposition method, under-1V constant voltage condition, deposits 5min.
D takes out the nickel foam that contains sample, washs and is dried respectively with deionized water and alcohol solvent.
E puts into Muffle furnace by dried nickel foam and calcines, and calcination time is 80 minutes, and calcining heat is 350 ℃.
F is by above-mentioned porous NiCo
2o
4nano-chip arrays is placed in Ni (NO
3)
26H
2o and Co (NO
3)
26H
2in O mixed solution, then utilize electrochemical deposition method by NiCo
2o
4under be placed in-1V of nano-chip arrays constant voltage condition, deposit certain hour.
After G has reacted, product is used respectively to ethanol, deionized water rinsing for several times, 60 ℃ are dried 12 hours, obtain product.
2) preparation of active carbon (CMK-3) negative material: by CMK-3, acetylene black, binding agent according to a certain percentage (85:15:5) mixes, then add appropriate ethanol and be stirred to completely and mix, then said mixture is evenly coated in nickel foam, 120 ℃ of vacuumizes, finally by the nickel foam that scribbles sample in the processing of 10MPa lower sheeting, as the negative material of Asymmetric Supercapacitor.
3) NiCo
2o
4@Co
xni
1-x(OH)
2the assembling of //CMK-3 water system Asymmetric Supercapacitor: using the potassium hydroxide of 1M as electrolyte, by above-mentioned steps 1) NiCo that obtains
2o
4@Co
xni
1-x(OH)
2positive electrode and 2) the CMK-3 negative material prepared is assembled into sandwich structure, and centre adds one deck barrier film.
A kind of NiCo
2o
4@Co
xni
1-x(OH)
2the preparation of //CMK-3 water system Asymmetric Supercapacitor, its characterization step is: 3) NiCo
2o
4@Co
xni
1-x(OH)
2preparation:
A puts into the nickel foam of suitable size to contain the ultrasonic cleaning of 1M hydrochloric acid solution, and object is to remove the nickel oxide on nickel foam surface.
B takes raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2o) 0.29g, cabaltous nitrate hexahydrate (Co (NO
3)
26H
2o) 0.58g and ammonium nitrate (NH
4nO
3) be dissolved in the water, and stir, make mixed solution, wherein Ni (NO
3)
26H
2o and Co (NO
3)
26H
2the ratio of O mole is 1:2, and ammonium nitrate is 0.08g.
C is placed in the nickel foam after above-mentioned cleaning the mixed solution of process B, is heated to 70 ℃, then utilizes electrochemical deposition method, under-1V constant voltage condition, deposits 8min.
D takes out the nickel foam that contains sample, washs and is dried respectively with deionized water and alcohol solvent.
E puts into Muffle furnace by dried nickel foam and calcines, and calcination time is 150 minutes, and calcining heat is 300 ℃.
F is by above-mentioned porous NiCo
2o
4nano-chip arrays is placed in Ni (NO
3)
26H
2o and Co (NO
3)
26H
2in O mixed solution, then utilize electrochemical deposition method by NiCo
2o
4under be placed in-1V of nano-chip arrays constant voltage condition, deposit certain hour.
After G has reacted, product is used respectively to ethanol, deionized water rinsing for several times, 60 ℃ are dried 12 hours, obtain product.
2) preparation of active carbon (CMK-3) negative material: by CMK-3, acetylene black, binding agent according to a certain percentage (85:15:5) mixes, then add appropriate ethanol and be stirred to completely and mix, then said mixture is evenly coated in nickel foam, 120 ℃ of vacuumizes, finally by the nickel foam that scribbles sample in the processing of 10Mpa lower sheeting, as the negative material of Asymmetric Supercapacitor.
3) NiCo
2o
4@Co
xni
1-x(OH)
2the assembling of //CMK-3 water system Asymmetric Supercapacitor: using the potassium hydroxide of 1M as electrolyte, by above-mentioned steps 1) NiCo that obtains
2o
4@Co
xni
1-x(OH)
2positive electrode and 2) the CMK-3 negative material prepared is assembled into sandwich structure, and centre adds one deck barrier film.
Embodiment 3
A kind of NiCo
2o
4@Co
xni
1-x(OH)
2the preparation of //CMK-3 water system Asymmetric Supercapacitor, its characterization step is: 1) NiCo
2o
4@Co
xni
1-x(OH)
2preparation:
A puts into the nickel foam of suitable size to contain the ultrasonic cleaning of 1M hydrochloric acid solution, and object is to remove the nickel oxide on nickel foam surface.
B takes raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2o) 0.29g, cabaltous nitrate hexahydrate (Co (NO
3)
26H
2o) 0.58g and ammonium nitrate (NH
4nO
3) be dissolved in the water, and stir, make mixed solution, wherein Ni (NO
3)
26H
2o and Co (NO
3)
26H
2the ratio of O mole is 1:2, and ammonium nitrate is 0.08g.
C is placed in the nickel foam after above-mentioned cleaning the mixed solution of process B, is heated to 70 ℃, then utilizes electrochemical deposition method, under-1V constant voltage condition, deposits 10min.
D takes out the nickel foam that contains sample, washs and is dried respectively with deionized water and alcohol solvent.
E puts into Muffle furnace by dried nickel foam and calcines, and calcination time is 200 minutes, and calcining heat is 250 ℃.
F is by above-mentioned porous NiCo
2o
4nano-chip arrays is placed in Ni (NO
3)
26H
2o and Co (NO
3)
26H
2in O mixed solution, then utilize electrochemical deposition method by NiCo
2o
4under be placed in-1V of nano-chip arrays constant voltage condition, deposit certain hour.
After G has reacted, product is used respectively to ethanol, deionized water rinsing for several times, 60 ℃ are dried 12 hours, obtain product.
2) preparation of active carbon (CMK-3) negative material: by CMK-3, acetylene black, binding agent according to a certain percentage (85:15:5) mixes, then add appropriate ethanol and be stirred to completely and mix, then said mixture is evenly coated in nickel foam, 120 ℃ of vacuumizes, finally by the nickel foam that scribbles sample in the processing of 10MPa lower sheeting, as the negative material of Asymmetric Supercapacitor.
3) NiCo
2o
4@Co
xni
1-x(OH)
2the assembling of //CMK-3 water system Asymmetric Supercapacitor: using the potassium hydroxide of 1M as electrolyte, by above-mentioned steps 1) NiCo that obtains
2o
4@Co
xni
1-x(OH)
2positive electrode and 2) the CMK-3 negative material prepared is assembled into sandwich structure, and centre adds one deck barrier film.
Claims (10)
1. a preparation method for water system Asymmetric Supercapacitor, comprising:
(1) NiCo
2o
4@Co
xni
1-x(OH)
2preparation:
A ultrasonic cleaning nickel foam, to remove surperficial nickel oxide, obtains the nickel foam after cleaning;
B is by Nickelous nitrate hexahydrate Ni (NO
3)
26H
2o, cabaltous nitrate hexahydrate Co (NO
3)
26H
2o and ammonium nitrate NH
4nO
3be dissolved in the water, make mixed solution, wherein Ni (NO
3)
26H
2o and Co (NO
3)
26H
2the ratio of O mole is 1:2;
The nickel foam after above-mentioned cleaning is placed in the mixed solution that B obtains by C, is heated to 60-75 ℃, then utilizes electrochemical deposition method, under constant voltage condition, deposits 4-10min, obtains the nickel foam that contains sample;
D takes out the nickel foam that contains sample, washs and is dried respectively with deionized water and alcohol solvent, then puts into Muffle furnace and calcines, and calcination time is 60-240 minute, and calcining heat is 250-350 ℃, obtains NiCo
2o
4nano-chip arrays;
E is by above-mentioned NiCo
2o
4nano-chip arrays is placed in Ni (NO
3)
26H
2o and Co (NO
3)
26H
2in the mixed solution of O, then utilize electrochemical deposition method to deposit under constant voltage condition; After having reacted, product is used respectively to ethanol, deionized water rinsing for several times, finally, in 60 ℃ of dry 8-20 hour, obtain NiCo
2o
4@Co
xni
1-x(OH)
2positive electrode;
(2) preparation of active carbon CMK-3 negative material:
CMK-3, acetylene black, binding agent are mixed, then add ethanol and be stirred to be mixed to get mixture completely, then said mixture is evenly coated in the nickel foam after cleaning, compressing tablet processing again after vacuumize, obtains CMK-3 negative material;
(3) NiCo
2o
4@Co
xni
1-x(OH)
2the assembling of //CMK-3 water system Asymmetric Supercapacitor:
Using potassium hydroxide solution as electrolyte, by above-mentioned NiCo
2o
4@Co
xni
1-x(OH)
2positive electrode and CMK-3 negative material are assembled into sandwich structure, and centre adds one deck barrier film.
2. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the washing lotion adopting in the ultrasonic cleaning described in step (1) A is 1M hydrochloric acid solution.
3. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the Ni (NO described in step (1) B
3)
26H
2the amount ratio of O and ammonium nitrate is 0.29g:0.08g.
4. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the voltage described in step (1) C in electrochemical deposition method is-1V.
5. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: Ni (NO in step (1) E
3)
26H
2o and Co (NO
3)
26H
2the ratio of O is 1:10-10:1.
6. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the voltage described in step (1) E in electrochemical deposition method is-1V.
7. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the NiCo obtaining in step (1) D
2o
4nano-chip arrays is ultra-thin porous structure, sheet is thick~and 6nm, bore dia~5-20nm.
8. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the NiCo obtaining in step (1) E
2o
4@Co
xni
1-x(OH)
2positive electrode is nucleocapsid structure.
9. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, is characterized in that: the mass ratio of CMK-3, acetylene black and the binding agent described in step (2) is 85:15:5.
10. the preparation method of a kind of water system Asymmetric Supercapacitor according to claim 1, it is characterized in that: described in step (3), the concentration of potassium hydroxide solution is 1mol/L, vacuum drying temperature is 120 ℃, and the pressure in described compressing tablet processing is 10Mpa.
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Cited By (13)
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CN104211128A (en) * | 2014-09-05 | 2014-12-17 | 南开大学 | Preparation method of one-dimensional NiCo2O4 nanorod as supercapacitor material |
CN104795243A (en) * | 2015-02-04 | 2015-07-22 | 三峡大学 | Asymmetric supercapacitor and preparation method thereof |
CN105990044A (en) * | 2016-01-20 | 2016-10-05 | 安徽大学 | Preparation method for flexible solid supercapacitor Cu(OH)2@Ni2(OH)2CO3 multistage nanoarray electrodes |
CN106129401A (en) * | 2016-06-29 | 2016-11-16 | 北京化工大学 | A kind of foamed nickel supported high surface roughness cobalt acid nickel nm wall and preparation method thereof |
CN106449136A (en) * | 2016-09-05 | 2017-02-22 | 郑州大学 | Alpha-nickel hydroxide cobalt electrode material and preparation method and application thereof |
CN106486297A (en) * | 2017-01-06 | 2017-03-08 | 徐靖才 | A kind of electrode material for super capacitor NiCo2O4The preparation method of/activated carbon |
CN106504900A (en) * | 2015-09-04 | 2017-03-15 | 罗伯特·博世有限公司 | Asymmetrical hybrid super capacitor |
CN106504904A (en) * | 2016-11-15 | 2017-03-15 | 三峡大学 | A kind of preparation method of the water system Asymmetric Supercapacitor based on cobaltosic oxide |
CN106710891A (en) * | 2017-02-04 | 2017-05-24 | 徐靖才 | NiCo2O4/active carbon composite material preparation method |
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CN107833757A (en) * | 2017-08-25 | 2018-03-23 | 青岛科技大学 | A kind of high-performance SiC@NiCo2O4/Ni(OH)2Hybrid supercapacitor positive electrode |
CN108630451A (en) * | 2018-04-26 | 2018-10-09 | 吉林大学 | A kind of preparation method of electrode material and ultracapacitor |
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CN106504900A (en) * | 2015-09-04 | 2017-03-15 | 罗伯特·博世有限公司 | Asymmetrical hybrid super capacitor |
CN105990044A (en) * | 2016-01-20 | 2016-10-05 | 安徽大学 | Preparation method for flexible solid supercapacitor Cu(OH)2@Ni2(OH)2CO3 multistage nanoarray electrodes |
CN106129401A (en) * | 2016-06-29 | 2016-11-16 | 北京化工大学 | A kind of foamed nickel supported high surface roughness cobalt acid nickel nm wall and preparation method thereof |
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