CN105460983B - A kind of ultracapacitor preparation method of cobalt acid nickel nano material - Google Patents
A kind of ultracapacitor preparation method of cobalt acid nickel nano material Download PDFInfo
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- CN105460983B CN105460983B CN201510829410.1A CN201510829410A CN105460983B CN 105460983 B CN105460983 B CN 105460983B CN 201510829410 A CN201510829410 A CN 201510829410A CN 105460983 B CN105460983 B CN 105460983B
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- 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 present invention provides a kind of preparation method of ultracapacitor cobalt acid nickel nano material, and step is as follows：(1) nickel nitrate, cobalt nitrate and urea are added in deionized water, are stirred under normal temperature, be well mixed solution, obtain solution A；(2) sodium cetanesulfonate and micro KNO are added in solution A3, ultrasound is allowed to well mixed, obtains solution B；(3) solution B is transferred in reactor, carries out incubating solvent thermal response, washed, drying obtains presoma；(4) after presoma is heat-treated through 360 390 DEG C of constant temperature in atmosphere, cobalt acid nickel nano material is obtained.Cobalt acid nickel nano material purity of the invention is high, the big (68m of specific surface area2/g)；In charge-discharge test, when current density is 1A/g, specific capacity value has reached value 2080F/g relatively higher, and more than 93% is still maintained by specific capacity after 3500 charge-discharge tests, can be used as electrode material for super capacitor.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of ultracapacitor system of cobalt acid nickel nano material
Preparation Method.
Background technology
Cobalt acid nickel (NiCo2O4) it is a kind of AB of Spinel structure2O4Type composite oxides, its in crystal structure, nickel
Ion occupies octahedral site, and cobalt ions had not only occupied octahedral site but also occupied tetrahedral site.Compared to single nickel oxide
And cobaltosic oxide, cobalt acid nickel is in itself with preferable electric conductivity.In addition, cobalt acid nickel has chemical property higher,
Low production cost, raw material abundance and advantages of environment protection, have attracted the common concern of researcher, in Germany《Germany should
With chemistry》Magazine (2015, volume 54 page 1868) has been reported.At present, existing document report prepares the method for cobalt acid nickel and has：It is high
Warm solid phase method, sol-gel process, mechanochemical synthesis, liquid chemical precipitation method etc., but cobalt acid nickel prepared by such method
Grain skewness, poor dispersion yields poorly, and the relatively complicated complexity of preparation method.At present, prepare using commonplace
Method be water (solvent) hot method, because it has simple for process, energy ezpenditure relatively small and product is easily controllable, anti-
The advantages of shorter between seasonable.
The content of the invention
The invention provides a kind of ultracapacitor preparation method of cobalt acid nickel nano material, with excellent performance,
Can be used as electrode of super capacitor.
The invention provides a kind of ultracapacitor preparation method of cobalt acid nickel nano material, step is as follows：
(1) by Ni (NO3)2·6H2O、Co(NO3)2·6H2O and urea are added in deionized water, are stirred under normal temperature, are made
Solution is well mixed, and obtains solution A；
(2) sodium cetanesulfonate and micro KNO are added in solution A3, ultrasound is allowed to well mixed, obtains solution B；
(3) solution B is transferred in reactor, isothermal reaction 20-26 hours at 100-130 DEG C, washing, drying is obtained
To presoma；
(4) after presoma is heat-treated through 360-390 DEG C of constant temperature in atmosphere, cobalt acid nickel nano material is obtained.
Preferably, Ni (NO described in step (1)3)2·6H2O、Co(NO3)2·6H2The mol ratio of O and urea is 1:2:
(10-15), molar concentration of the nickel ion in the solution A is 0.4mol/L.
Preferably, the addition of the sodium cetanesulfonate is the 1/6-1/4 of deionized water volume in step (1),
The KNO3Molar concentration in solution B is 0.003mol/L.
Preferably, washing is washed respectively 3 times with deionized water and absolute ethyl alcohol described in step (2).
The present invention also provides the cobalt acid nickel nano material prepared using any of the above-described method.
The present invention also provides application of the above-mentioned cobalt acid nickel nano material in electrode of super capacitor is prepared.
The present invention using deionized water and sodium cetanesulfonate as solvent, with Ni (NO3)2·6H2O and Co (NO3)2·
6H2O is reaction raw materials, after solvent-thermal method prepares presoma, and then prepares that a kind of purity is high, specific surface area is big
(68m2/ g) cobalt acid nickel nano material, using the contact surface that improve active material and electrolyte in terms of electrode, improve
Reaction rate；In charge-discharge test, when current density is 1A/g, specific capacity value has reached value 2080F/g relatively higher, passes through
Specific capacity still maintains more than 93% after 3500 charge-discharge tests, can be used as electrode material for super capacitor；System
Preparation Method is simple, product cost is low, be adapted to large-scale production.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the ultracapacitor x-ray diffraction pattern of cobalt acid nickel nano material of preparation in embodiment 1, wherein：It is horizontal
Coordinate is angle of diffraction (2 θ), and ordinate is relative diffracted intensity.
Specific embodiment
Following embodiment is only preferred embodiment of the invention, should not be construed as limitation of the invention.Following implementations
Experimental technique in example, unless otherwise specified, is conventional method.It is raw materials used in experiment：Ni(NO3)2·6H2O and Co
(NO3)2·6H2It is pure that O is analysis.
Embodiment 1
A kind of ultracapacitor of the invention is as follows with the preparation method step of cobalt acid nickel nano material：
(1) by 11.6gNi (NO3)2·6H2O (containing nickel ion 0.04mol), 23.3g Co (NO3)2·6H2O (contains cobalt ions
0.08mol) it is added in 100ml deionized waters with 24.0g urea, is stirred under normal temperature, be well mixed solution, obtains solution A；
(2) 16.7ml sodium cetanesulfonates and 0.035gKNO are added in solution A3, ultrasound is allowed to well mixed, obtains
Solution B；
(3) solution B is transferred in reactor, isothermal reaction 22 hours at 110 DEG C, with deionized water and absolute ethyl alcohol
Wash 3 times respectively, the freeze-day with constant temperature at 62 DEG C obtains presoma；
(4) after presoma being heat-treated into 2h (1 DEG C/min of heating rate) through 370 DEG C of constant temperature in atmosphere, cobalt acid nickel is obtained
Nano material.
The applicant has found through experiment, is being surfactant structure with deionized water as solvent, with sodium cetanesulfonate
Into reaction system in, add micro KNO3The specific surface area and ratio of the cobalt acid nickel nano material of preparation can be increased substantially
Capacity, therefore, applicant's conjecture, KNO3The effect of auxiliary agent is served wherein.
The cobalt acid nickel nano material of above-mentioned preparation is carried out into charge-discharge test, when current density is 1A/g, specific capacity value reaches
Value 2080F/g relatively higher is arrived, when current density is 0.5A/g, specific capacity value is 1490F/g；By 3500 charge and discharge electrical measurements
Specific capacity remains at more than 93% after examination.
Embodiment 2
Ultracapacitor of the invention is as follows with the preparation method step of cobalt acid nickel nano material：
(1) by 11.6gNi (NO3)2·6H2O (containing nickel ion 0.04mol), 23.3g Co (NO3)2·6H2O (contains cobalt ions
0.08mol) it is added in 100ml deionized waters with 36.0g urea, is stirred under normal temperature, be well mixed solution, obtains solution A；
(2) 25ml sodium cetanesulfonates and 0.038gKNO are added in solution A3, ultrasound is allowed to well mixed, obtains molten
Liquid B；
(3) solution B is transferred in reactor, isothermal reaction 24 hours at 100 DEG C, with deionized water and absolute ethyl alcohol
Wash 3 times respectively, the freeze-day with constant temperature at 60 DEG C obtains presoma；
(4) after presoma being heat-treated into 3h (2 DEG C/min of heating rate) through 380 DEG C of constant temperature in atmosphere, cobalt acid nickel is obtained
Nano material.
The cobalt acid nickel nano material of above-mentioned preparation is carried out into charge-discharge test, when current density is 1A/g, specific capacity value reaches
Value 2010F/g relatively higher is arrived, when current density is 0.5A/g, specific capacity value is 1430F/g；By 3500 charge and discharge electrical measurements
Specific capacity remains at more than 92% after examination.
Embodiment 3
Ultracapacitor of the invention is as follows with the preparation method step of cobalt acid nickel nano material：
(1) by 11.6gNi (NO3)2·6H2O (containing nickel ion 0.04mol), 23.3g Co (NO3)2·6H2O (contains cobalt ions
0.08mol) it is added in 100ml deionized waters with 31.0g urea, is stirred under normal temperature, be well mixed solution, obtains solution A；
(2) 19ml sodium cetanesulfonates and 0.036gKNO are added in solution A3, ultrasound is allowed to well mixed, obtains molten
Liquid B；
(3) solution B is transferred in reactor, isothermal reaction 26 hours at 130 DEG C, with deionized water and absolute ethyl alcohol
Wash 3 times respectively, the freeze-day with constant temperature at 65 DEG C obtains presoma；
(4) after presoma being heat-treated into 2h (1 DEG C/min of heating rate) through 390 DEG C of constant temperature in atmosphere, cobalt acid nickel is obtained
Nano material.
The cobalt acid nickel nano material of above-mentioned preparation is carried out into charge-discharge test, when current density is 1A/g, specific capacity value reaches
Value 1940F/g relatively higher is arrived, when current density is 0.5A/g, specific capacity value is 1410F/g；By 3500 charge and discharge electrical measurements
Specific capacity remains at more than 90% after examination.
Embodiment 4
Ultracapacitor of the invention is as follows with the preparation method step of cobalt acid nickel nano material：
(1) by 11.6gNi (NO3)2·6H2O (containing nickel ion 0.04mol), 23.3g Co (NO3)2·6H2O (contains cobalt ions
0.08mol) it is added in 100ml deionized waters with 33.0g urea, is stirred under normal temperature, be well mixed solution, obtains solution A；
(2) 21ml sodium cetanesulfonates and 0.037gKNO are added in solution A3, ultrasound is allowed to well mixed, obtains molten
Liquid B；
(3) solution B is transferred in reactor, isothermal reaction 20 hours at 110 DEG C, with deionized water and absolute ethyl alcohol
Wash 3 times respectively, the freeze-day with constant temperature at 63 DEG C obtains presoma；
(4) after presoma being heat-treated into 3h (2 DEG C/min of heating rate) through 370 DEG C of constant temperature in atmosphere, cobalt acid nickel is obtained
Nano material.
The cobalt acid nickel nano material of above-mentioned preparation is carried out into charge-discharge test, when current density is 1A/g, specific capacity value reaches
Value 1980F/g relatively higher is arrived, when current density is 0.5A/g, specific capacity value is 1420F/g；By 3500 charge and discharge electrical measurements
Specific capacity remains at more than 90% after examination.
Embodiment 5
Ultracapacitor of the invention is as follows with the preparation method step of cobalt acid nickel nano material：
(1) by 11.6gNi (NO3)2·6H2O (containing nickel ion 0.04mol), 23.3g Co (NO3)2·6H2O (contains cobalt ions
0.08mol) it is added in 100ml deionized waters with 28.0g urea, is stirred under normal temperature, be well mixed solution, obtains solution A；
(2) 20ml sodium cetanesulfonates and 0.036gKNO are added in solution A3, ultrasound is allowed to well mixed, obtains molten
Liquid B；
(3) solution B is transferred in reactor, isothermal reaction 22 hours at 120 DEG C, with deionized water and absolute ethyl alcohol
Wash 3 times respectively, the freeze-day with constant temperature at 65 DEG C obtains presoma；
(4) after presoma being heat-treated into 3h (1 DEG C/min of heating rate) through 360 DEG C of constant temperature in atmosphere, cobalt acid nickel is obtained
Nano material.
The cobalt acid nickel nano material of above-mentioned preparation is carried out into charge-discharge test, when current density is 1A/g, specific capacity value reaches
Value 2020F/g relatively higher is arrived, when current density is 0.5A/g, specific capacity value is 1460F/g；By 3500 charge and discharge electrical measurements
Specific capacity remains at more than 91% after examination.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (2)
1. a kind of ultracapacitor preparation method of cobalt acid nickel nano material, it is characterised in that：Step is as follows：
(1) by Ni (NO3)2·6H2O、Co(NO3)2·6H2O and urea are added in deionized water, are stirred under normal temperature, make solution
It is well mixed, obtain solution A；Ni (NO described in step (1)3)2·6H2O、Co(NO3)2·6H2The mol ratio of O and urea is 1:2:
(10-15), molar concentration of the nickel ion in the solution A is 0.4mol/L；
(2) sodium cetanesulfonate and KNO are added in solution A3, ultrasound is allowed to well mixed, obtains solution B；The cetyl
The addition of sodium sulfonate is the 1/6-1/4, the KNO of deionized water volume in step (1)3Molar concentration in solution B is
0.003mol/L；
(3) solution B is transferred in reactor, isothermal reaction 20-26 hours at 100-130 DEG C, washing, drying, before obtaining
Drive body；
(4) after presoma is heat-treated through 360-390 DEG C of constant temperature in atmosphere, cobalt acid nickel nano material is obtained.
2. method according to claim 1, it is characterised in that：Washing described in step (3) is with deionized water and anhydrous
Ethanol is washed 3 times respectively.
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| CN106006763A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Method for preparing nickel cobaltate nanocrystalline assembly |
| CN106698527A (en) * | 2016-11-25 | 2017-05-24 | 江苏大学 | Hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as solvent system |
| CN106938859B (en) * | 2017-04-01 | 2018-02-16 | 吉林大学 | One step hydro thermal method prepares cathode of lithium battery tubular material NiCo2O4Method |
| CN109103027A (en) * | 2018-07-09 | 2018-12-28 | 江苏大学 | Solvent-thermal method prepares the method and its application of cobalt acid copper combination electrode material |
| CN111118883B (en) * | 2019-12-31 | 2022-03-01 | 东华大学 | Cellulose-based carbon nanofiber composite material and preparation and application thereof |
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| CN104129818B (en) * | 2014-07-09 | 2017-01-04 | 奇瑞汽车股份有限公司 | A kind of nickel cobalt oxide material and preparation method thereof |
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