CN103979618A - Synthetic method for nickel cobaltate nano-material used for supercapacitor - Google Patents

Synthetic method for nickel cobaltate nano-material used for supercapacitor Download PDF

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CN103979618A
CN103979618A CN201410186605.4A CN201410186605A CN103979618A CN 103979618 A CN103979618 A CN 103979618A CN 201410186605 A CN201410186605 A CN 201410186605A CN 103979618 A CN103979618 A CN 103979618A
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cobalt acid
acid nickel
synthetic method
nano material
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CN103979618B (en
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胡中华
刘纪敏
艾志红
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Tongji University
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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 relates to a synthetic method for a nickel cobaltate nano-material used for a supercapacitor. The method comprises the following steps: adding CoSO4.7H2O, NiSO4.6H2O and urea into deionized water, then adding glycerol and carrying out stirring at a temperature of 60 DEG C until a uniformly mixed solution is obtained; transferring the solution to a reaction vessel, heating the solution to 100 to 140 DEG C and carrying out a hydro-thermal reaction at a constant temperature for 12 h; after completion of the reaction, carrying out filtering so as to prepare a precursor solution and drying a precipitate at a constant temperature so as to obtain a precursor; and placing the prepared precursor in a tubular furnace and carrying out calcining at a constant temperature of 300 to 400 DEG C for 3 h so as to obtain the nickel cobaltate nano-material. The synthetic method has the advantages of simple operation, environment friendliness and high yield; and the prepared nickel cobaltate nano-material is of a three-dimensional structure composed of nanometer flakes, has a high specific surface area and abundant pore channels which are favorable for diffusion of an electrolyte, and can be used as a supercapacitor material.

Description

The synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor
Technical field
The invention belongs to electrochemical energy storage field, relate to the synthetic method of a kind of ultracapacitor cobalt acid nickel nano material.
Background technology
Ultracapacitor, is also called electrochemical capacitor, is a kind of Novel energy storage apparatus between traditional capacitor and rechargeable battery.It had both had very high discharge power the same as ordinary capacitor, had again larger charge storage capacity as battery, can say that ultracapacitor is the combination of these two kinds of element optimals.Wherein, electrode materials is larger on the impact of ultracapacitor performance.According to the difference of its energy storage principle, carbon material, metal oxide and conductive polymers are current conventional electrode material for super capacitor.
Cobalt acid nickel (NiCo 2o 4) be a kind of AB of Spinel structure 2o 4type composite oxides, in its crystalline structure, nickel ion occupies octahedral site, and cobalt ion not only occupies octahedral site but also occupy tetrahedral site.Than single nickel oxide and tricobalt tetroxide, cobalt acid nickel itself has good electroconductibility.In addition, cobalt acid nickel has higher chemical property, and production cost is low, raw material abundance and advantages of environment protection, and these advantages all make it receive much concern in supercapacitor applications field.
At present, the main synthetic method of cobalt acid nickel has: high temperature solid-state method, sol-gel method, mechanochemical synthesis, liquid chemical precipitation method etc.Wherein hydrothermal method has the advantages such as simple for process, energy expenditure is relatively little and hydrothermal product diameter of particle is easy to control, and the reaction times is shorter, is to use at present one of means of preparing comparatively widely cobalt acid nickel nano material.Utilizing hydrothermal method successfully to prepare nano-sheet cobalt acid nickel material taking NaOH as precipitation agent as the people [Rui Ding et a1., J Appl Electrochem, 2013,43,903-910] such as the Ding. of nearest report adopt soft template method, is 591F/g than electric capacity.Chinese patent (CN102745752.A, 2012) utilizes hydrothermal method to synthesize pattern for sea urchin shape, and degree of crystallinity is high, the nano nickel cobalt oxide material of even aperture distribution.
Summary of the invention
Object of the present invention is exactly the synthetic method that a kind of ultracapacitor cobalt acid nickel nano material is provided in order to overcome the defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A synthetic method for cobalt acid nickel nano material for ultracapacitor, the method comprises the following steps:
(1) by CoSO 47H 2o, NiSO 46H 2o and urea add in deionized water, under normal temperature, stir, and solution is mixed;
(2) in the mixing solutions making to step (1), add glycerol, and under 60 DEG C of conditions, be stirred to solution and mix;
(3) solution step (2) gained being mixed is transferred in reactor, is heated to 100～140 DEG C, carries out hydro-thermal reaction, and isothermal reaction 12h, after hydro-thermal reaction finishes, is cooled to room temperature by precursor solution;
(4) the prepared precursor solution of filtration step (3), by the precipitated product of gained respectively with the each washing of deionized water and ethanol at least 3 times, and under 60 DEG C of conditions freeze-day with constant temperature, obtain presoma;
(5) presoma step (4) being made is placed in tube furnace, and calcining at constant temperature 3h under 300～400 DEG C of conditions makes cobalt acid nickel nano material.
The CoSO that step (1) is described 47H 2o, NiSO 46H 2the mol ratio of O and urea is 2: 1: 15, and the volumetric molar concentration of nickel ion in described solution is 0.01mol/L.
The add-on of described glycerol is 1/3 of the middle deionized water volume of step (1).
Described presoma is to calcine in the atmosphere of air.
The inner lining material of described autoclave is tetrafluoroethylene.
The present invention, in simple hydro-thermal preparation process, does not need to add template and tensio-active agent, and the product purity of gained is higher, and specific surface area is larger, is applicable to the application of super capacitor material.
Compared with prior art, the present invention is simple to operate, and the nano nickel cobalt oxide material purity of gained is higher, has larger specific surface area and is beneficial to the macropore of electrolytic solution diffusion, can be used as capacitor electrode material, can reach 960F/g than electric capacity.
Brief description of the drawings
Fig. 1 is the SEM figure that cobalt acid nickel nano material magnification prepared by the present invention is 5.00um;
Fig. 2 is the SEM figure that cobalt acid nickel nano material magnification prepared by the present invention is 1.00um;
Fig. 3 is the SEM figure that cobalt acid nickel nano material magnification prepared by the present invention is 500nm;
Fig. 4 is nitrogen adsorption-desorption isotherm figure of the cobalt acid nickel material prepared of the present invention;
Fig. 5 is the pore size distribution curve figure of the cobalt acid nickel material prepared of the present invention;
Fig. 6 is the cyclic voltammetry curve figure (electrolyte solution be 6M KOH solution) of the cobalt acid nickel nano material prepared of the present invention under different scanning rates;
Fig. 7 is the discharge curve of the cobalt acid nickel material prepared of the present invention under different current densities.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
(1) take 0.34g CoSO 47H 2o, 0.16g NiSO 46H 2o and 0.54g urea are dissolved in 60ml deionized water, under normal temperature, fully stir 30 minutes, and solution is mixed.
(2) measure about 20ml glycerol and add in the mixing solutions of step (1) gained, at 60 DEG C, heated and stirred to solution mixes.
(3) step (2) gained mixing solutions is transferred to in teflon-lined reactor, be heated to 100 DEG C after isothermal reaction 12 hours.After hydro-thermal reaction, precursor solution is cooled to room temperature.
(4) precursor solution obtaining in filtration step (3), uses respectively deionized water and washing with alcohol 5 times by gained precipitation, and dry in 60 DEG C of baking ovens.
(5) above-mentioned gained precursor is placed in to porcelain boat, taking air as atmosphere, is placed in 300 DEG C of calcining at constant temperature of tube furnace 3 hours, prepare cobalt acid nickel nano material.
(6) the cobalt acid nickel nano material of being prepared by step (5) to gained characterizes and electro-chemical test.Result shows that the synthetic cobalt acid nickel nano material of this method has higher specific surface area (121m 2/ g), than electric capacity up to 960F/g.
Cobalt acid nickel Characterization of Nano-materials result prepared by the present embodiment is as shown in Fig. 1～Fig. 7.
Fig. 1 to Fig. 3 is the SEM figure of cobalt acid nickel nano material under different multiples.As seen from the figure, cobalt acid nickel nano material is to be about by thickness the flower-shaped vesicular structure that the nanometer sheet of 60nm assembles.
Nitrogen adsorption-desorption isotherm figure of the cobalt acid nickel material that Fig. 4 is prepared for the present invention, according to IUPC classification, this curve can be attributed to IV type curve.Within the scope of 0.5-1.0P/P0, can be observed hysteresis loop, the mesoporous property of prepared material has been described.
Fig. 5 is the pore size distribution curve figure of the cobalt acid nickel material prepared of the present invention.As seen from the figure, the pore size distribution range of material is wider, illustrates in cobalt acid nickel material and has a large amount of mesoporous and macropores.
Fig. 6 is the cyclic voltammetry curve figure of the cobalt acid nickel nano material prepared of the present invention under different scanning rates, and the redox peak obviously existing in these CV curves shows that it mainly reacts generation electric capacity by faraday.
Fig. 7 is the discharge curve of the cobalt acid nickel material prepared of the present invention under different current densities, the fake capacitance performance of material that had platform validation in discharge curve.By calculating discharge time in the time that current density is 1A/g, the ratio electric capacity of cobalt acid nickel material prepared by the present invention can reach 960F/g.
Embodiment 2
(1) take 0.34g CoSO 47H 2o, 0.16g NiSO 46H 2o and 0.54g urea are dissolved in 60ml deionized water, under normal temperature, fully stir 30 minutes, and solution is mixed.
(2) measure about 20ml glycerol and add in the mixing solutions of step (1) gained, at 60 DEG C, heated and stirred to solution mixes.
(3) step (2) gained mixing solutions is transferred to in teflon-lined reactor, be heated to 120 DEG C after isothermal reaction 12 hours.After hydro-thermal reaction, precursor solution is cooled to room temperature.
(4) precursor solution obtaining in filtration step (3), uses respectively deionized water and washing with alcohol 5 times by gained precipitation, and dry in 60 DEG C of baking ovens.
(5) above-mentioned gained precursor is placed in to porcelain boat, taking air as atmosphere, is placed in 300 DEG C of calcining at constant temperature of tube furnace 3 hours, prepare cobalt acid nickel nano material.
Embodiment 3
(1) take 0.34g CoSO 47H 2o, 0.16g NiSO 46H 2o and 0.54g urea are dissolved in 60ml deionized water, under normal temperature, fully stir 30 minutes, and solution is mixed.
(2) measure about 20ml glycerol and add in the mixing solutions of step (1) gained, at 60 DEG C, heated and stirred to solution mixes.
(3) step (2) gained mixing solutions is transferred to in teflon-lined reactor, be heated to 120 DEG C after isothermal reaction 12 hours.After hydro-thermal reaction, precursor solution is cooled to room temperature.
(4) precursor solution obtaining in filtration step (3), uses respectively deionized water and washing with alcohol 4 times by gained precipitation, and dry in 60 DEG C of baking ovens.
(5) above-mentioned gained precursor is placed in to porcelain boat, taking air as atmosphere, is placed in 400 DEG C of calcining at constant temperature of tube furnace 3 hours, prepare cobalt acid nickel nano material.
Embodiment 4
(1) take 0.34g CoSO 47H 2o, 0.16g NiSO 46H 2o and 0.54g urea are dissolved in 60ml deionized water, under normal temperature, fully stir 30 minutes, and solution is mixed.
(2) measure about 20ml glycerol and add in the mixing solutions of step (1) gained, at 60 DEG C, heated and stirred to solution mixes.
(3) step (2) gained mixing solutions is transferred to in teflon-lined reactor, be heated to 140 DEG C after isothermal reaction 12 hours.After hydro-thermal reaction, precursor solution is cooled to room temperature.
(4) precursor solution obtaining in filtration step (3), uses respectively deionized water and washing with alcohol 6 times by gained precipitation, and dry in 60 DEG C of baking ovens.
(5) above-mentioned gained precursor is placed in to porcelain boat, taking air as atmosphere, is placed in 300 DEG C of calcining at constant temperature of tube furnace 3 hours, prepare cobalt acid nickel nano material.
Embodiment 5
(1) take 0.34g CoSO 47H 2o, 0.16g NiSO 46H 2o and 0.54g urea are dissolved in 60ml deionized water, under normal temperature, fully stir 30 minutes, and solution is mixed.
(2) measure about 20ml glycerol and add in the mixing solutions of step (1) gained, at 60 DEG C, heated and stirred to solution mixes.
(3) step (2) gained mixing solutions is transferred to in teflon-lined reactor, be heated to 140 DEG C after isothermal reaction 12 hours.After hydro-thermal reaction, precursor solution is cooled to room temperature.
(4) precursor solution obtaining in filtration step (3), uses respectively deionized water and washing with alcohol 6 times by gained precipitation, and dry in 60 DEG C of baking ovens.
(5) above-mentioned gained precursor is placed in to porcelain boat, taking air as atmosphere, is placed in 400 DEG C of calcining at constant temperature of tube furnace 3 hours, prepare cobalt acid nickel nano material.

Claims (5)

1. a synthetic method for cobalt acid nickel nano material for ultracapacitor, is characterized in that, the method comprises the following steps:
(1) by CoSO 47H 2o, NiSO 46H 2o and urea add in deionized water, under normal temperature, stir, and solution is mixed;
(2) in the mixing solutions making to step (1), add glycerol, and under 60 DEG C of conditions, be stirred to solution and mix;
(3) solution step (2) gained being mixed is transferred in reactor, is heated to 100～140 DEG C, carries out hydro-thermal reaction, and isothermal reaction 12h, after hydro-thermal reaction finishes, is cooled to room temperature by precursor solution;
(4) the prepared precursor solution of filtration step (3), by the precipitated product of gained respectively with the each washing of deionized water and ethanol at least 3 times, and under 60 DEG C of conditions freeze-day with constant temperature, obtain presoma;
(5) presoma step (4) being made is placed in tube furnace, and calcining at constant temperature 3h under 300～400 DEG C of conditions makes cobalt acid nickel nano material.
2. the synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor according to claim 1, is characterized in that the CoSO that step (1) is described 47H 2o, NiSO 46H 2the mol ratio of O and urea is 3: 1: 15, and the volumetric molar concentration of nickel ion in described solution is 0.01mol/L.
3. the synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor according to claim 1, is characterized in that, the add-on of described glycerol is 1/3 of the middle deionized water volume of step (1).
4. the synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor according to claim 1, is characterized in that, described presoma is to calcine in the atmosphere of air.
5. the synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor according to claim 1, is characterized in that, the inner lining material of described autoclave is tetrafluoroethylene.
CN201410186605.4A 2014-05-05 2014-05-05 The synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor Expired - Fee Related CN103979618B (en)

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Cited By (15)

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CN104766725A (en) * 2015-03-12 2015-07-08 广东工业大学 Preparation method for electrode material used for supercapacitor and application of electrode material
CN105013491A (en) * 2015-07-06 2015-11-04 中山大学 Novel efficient formaldehyde catalyst and preparation method thereof
CN105244177A (en) * 2015-10-28 2016-01-13 扬州大学 3D-nanostructure NiCo2S4 electrode material for super capacitor and preparation method thereof
CN105271438A (en) * 2015-10-27 2016-01-27 渤海大学 Preparation method of magnesium cobaltate porous structure electrode material with double-sea urchin shape
CN105399150A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 NiCo2O4 nano-material as well as preparation method and application thereof
CN105399149A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of supercapacitor electrode material
CN105399151A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of NiCo2O4 nano-material
CN105448527A (en) * 2015-11-24 2016-03-30 青岛能迅新能源科技有限公司 Electrode material for super capacitor and preparation method for the same
CN105460983A (en) * 2015-11-24 2016-04-06 青岛能迅新能源科技有限公司 Method for preparing nickel cobaltate nano material for super capacitor
CN106115805A (en) * 2016-06-24 2016-11-16 扬州大学 The preparation method of nanometer hierarchy cobalt acid nickel/mos2 microsphere
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
CN107473273A (en) * 2017-08-02 2017-12-15 东北大学秦皇岛分校 Three-dimensional structure micron order cobalt acid Ni cluster, preparation method and the usage
CN107658145A (en) * 2017-09-29 2018-02-02 山东大学 A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method and application
CN110342589A (en) * 2019-07-30 2019-10-18 安徽大学 A kind of cobalt acid nickel nano flower-like composite material and preparation method
CN110655120A (en) * 2019-11-13 2020-01-07 东北电力大学 Preparation method of mesoporous spherical nickel cobaltate nano material

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Cited By (20)

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CN104766725B (en) * 2015-03-12 2017-06-20 广东工业大学 A kind of preparation method and applications for electrode material for super capacitor
CN104766725A (en) * 2015-03-12 2015-07-08 广东工业大学 Preparation method for electrode material used for supercapacitor and application of electrode material
CN105013491A (en) * 2015-07-06 2015-11-04 中山大学 Novel efficient formaldehyde catalyst and preparation method thereof
CN105271438A (en) * 2015-10-27 2016-01-27 渤海大学 Preparation method of magnesium cobaltate porous structure electrode material with double-sea urchin shape
CN105244177A (en) * 2015-10-28 2016-01-13 扬州大学 3D-nanostructure NiCo2S4 electrode material for super capacitor and preparation method thereof
CN105448527B (en) * 2015-11-24 2018-02-06 青岛能迅新能源科技有限公司 A kind of electrode material for ultracapacitor and preparation method thereof
CN105399149A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of supercapacitor electrode material
CN105448527A (en) * 2015-11-24 2016-03-30 青岛能迅新能源科技有限公司 Electrode material for super capacitor and preparation method for the same
CN105460983A (en) * 2015-11-24 2016-04-06 青岛能迅新能源科技有限公司 Method for preparing nickel cobaltate nano material for super capacitor
CN105399151A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of NiCo2O4 nano-material
CN105399150A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 NiCo2O4 nano-material as well as preparation method and application thereof
CN106115805A (en) * 2016-06-24 2016-11-16 扬州大学 The preparation method of nanometer hierarchy cobalt acid nickel/mos2 microsphere
CN106115805B (en) * 2016-06-24 2017-10-17 扬州大学 The preparation method of the sour nickel/mos2 microsphere of nanometer hierarchy cobalt
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
CN107473273A (en) * 2017-08-02 2017-12-15 东北大学秦皇岛分校 Three-dimensional structure micron order cobalt acid Ni cluster, preparation method and the usage
CN107658145A (en) * 2017-09-29 2018-02-02 山东大学 A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method and application
CN107658145B (en) * 2017-09-29 2019-01-08 山东大学 A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and the preparation method and application thereof
CN110342589A (en) * 2019-07-30 2019-10-18 安徽大学 A kind of cobalt acid nickel nano flower-like composite material and preparation method
CN110655120A (en) * 2019-11-13 2020-01-07 东北电力大学 Preparation method of mesoporous spherical nickel cobaltate nano material
CN110655120B (en) * 2019-11-13 2022-03-25 东北电力大学 Preparation method of mesoporous spherical nickel cobaltate nano material

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