CN105417591A - Method for preparing nickel cobaltite nano material through solvothermal method - Google Patents
Method for preparing nickel cobaltite nano material through solvothermal method Download PDFInfo
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- CN105417591A CN105417591A CN201510829469.0A CN201510829469A CN105417591A CN 105417591 A CN105417591 A CN 105417591A CN 201510829469 A CN201510829469 A CN 201510829469A CN 105417591 A CN105417591 A CN 105417591A
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Abstract
The invention provides a method for preparing a nickel cobaltite nano material through a solvothermal method. The method comprises the following steps that 1, nickel nitrate, cobalt nitrate and trace KNO3 are added to polyethylene glycol 600 to be fully dissolved, sodium acetate anhydrous is added into the mixture for complete dissolution, and a mixed solution is obtained; 2, a reaction is conducted on the mixed solution in a reaction kettle under the condition of stirring at the constant temperature for a certain period of time, washing and drying are conducted, and a precursor is obtained; 3, isothermal heat treatment is conducted on the precursor in the air for 2-10 h at the temperature ranging from 360 DEG C to 400 DEG C, and the nickel cobaltite nano material is obtained. The specific capacity of the nickel cobaltite nano material reaches up to 1960 F/g, after charge-discharge tests are conducted for 4,000 times, the specific capacity still remains at 90% or above, the preparation method is simple, the product cost is low, and the method is suitable for large-scale production.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of method that solvent-thermal method prepares cobalt acid nickel nano material.
Background technology
Cobalt acid nickel (NiCo
2o
4) be a kind of AB of Spinel structure
2o
4type composite oxides, it is in crystalline structure, and nickel ion occupies octahedral site, and cobalt ion not only occupies octahedral site but also occupy tetrahedral site.Compared to 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, attract the common concern of researcher, have report at " German applied chemistry " magazine (2015,54 volumes 1868 pages) of Germany.At present, the method that existing bibliographical information prepares cobalt acid nickel has: high temperature solid-state method, sol-gel method, mechanochemical synthesis, liquid chemical precipitation method etc., but cobalt acid nickel size distribution prepared by these class methods is uneven, dispersed bad, yield poorly, and making method comparatively very complicated.At present, prepare and use commonplace method to be water (solvent) hot method, because of its have simple for process, energy expenditure is relatively little and product is easy to advantages such as controlling, the reaction times is shorter.Had report at " nanometer bulletin " magazine (2013,13 volumes 3135 pages) of the U.S. and " advanced material " magazine (2013,25 volumes 976 pages) of Germany, patent CN201210222916.2 also discloses the synthetic method of cobalt acid nickel.
Summary of the invention
The invention provides a kind of method that solvent-thermal method prepares cobalt acid nickel nano material, the cobalt acid nickel nano material specific surface area that application the method prepares is large, and specific storage is up to 1960F/g.
The invention provides a kind of method that solvent-thermal method prepares cobalt acid nickel nano material, step is as follows:
(1) by Ni (NO
3)
26H
2o, Co (NO
3)
26H
2o and micro-KNO
3join in Polyethylene Glycol-600 and fully dissolve, add anhydrous sodium acetate wherein and make it to dissolve completely, obtain mixing solutions;
(2) by the mixing solutions that obtains isothermal reaction certain hour under agitation in a kettle., washing, dries, obtains presoma;
(3) by presoma in atmosphere through 360-400 DEG C of constant temp. heating process, temperature rise rate is 1-2 DEG C/min, and soaking time is after 2-10h, obtains cobalt acid nickel nano material.
As preferably, the mol ratio of described nickel ion and cobalt ion is 0.97-1.04:2.
Further, the concentration of described nickel ion in Polyethylene Glycol-600 is 0.17-0.2mol/L.
As preferably, described KNO
3add-on be 0.0017-0.002mol/L.
As preferably, the add-on of described anhydrous sodium acetate is add 10-15g anhydrous sodium acetate in every 50-60mL Polyethylene Glycol-600.
As preferably, described in step (2), isothermal reaction is isothermal reaction 16-24h under the rotating speed of 120-150r/min under agitation.
The present invention also provides the application cobalt acid nickel nano material that above-mentioned arbitrary described method prepares.
The present invention also provides above-mentioned cobalt acid nickel nano material preparing the application in electrode of super capacitor.
The present invention using Polyethylene Glycol-600 as solvent, with Ni (NO
3)
26H
2o and Co (NO
3)
26H
2o is reaction raw materials, using anhydrous sodium acetate as precipitation agent, with KNO
3for auxiliary agent, after preparing presoma by solvent-thermal method, and then prepare the large (63m of a kind of specific surface area
2/ g) cobalt acid nickel nano material, specific storage is up to 1960F/g, and after 4000 charge-discharge tests, specific storage still remains on more than 90%, can use as electrode of super capacitor.Preparation method is simple, product cost is low, be applicable to scale operation.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the x-ray diffraction pattern of the cobalt acid nickel nano material of preparation in embodiment 1, wherein: X-coordinate is angle of diffraction (2 θ), and ordinate zou is relative diffracted intensity.
Embodiment
Following embodiment is only preferred embodiment of the present invention, should not be construed as limitation of the invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.Raw materials used in experiment: Ni (NO
3)
26H
2o and Co (NO
3)
26H
2o is analytical pure.
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 50-60mL Polyethylene Glycol-600, then add 10-15g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 180-200 DEG C, under agitation isothermal reaction 16-24h, stirring velocity is 120-150r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 70-80 DEG C of condition freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 360-400 DEG C of constant temp. heating process 2-10h (temperature rise rate 1-2 DEG C/min), obtains cobalt acid nickel nano material.
The applicant finds through experiment, when taking Polyethylene Glycol-600 as solvent, adds the KNO of trace
3, can increase substantially specific surface area and the specific storage of the cobalt acid nickel nano material of preparation, therefore, applicant guesses, KNO
3serve the effect of auxiliary agent wherein.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1830-1960F/g, and when current density is 2A/g, specific capacity value is 1370-1430F/g; After 4000 charge-discharge tests, specific storage still remains on more than 90%.
Embodiment 1
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 50mL Polyethylene Glycol-600, then add 10g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 200 DEG C, under agitation isothermal reaction 16h, stirring velocity is 150r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 80 DEG C of conditions freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 360 DEG C of constant temp. heating process 2h (temperature rise rate 1 DEG C/min), obtains cobalt acid nickel nano material.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1960F/g, and when current density is 2A/g, specific capacity value is 1430F/g; After 4000 charge-discharge tests, specific storage still remains on more than 92%.
Embodiment 2
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 60mL Polyethylene Glycol-600, then add 12g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 180 DEG C, under agitation isothermal reaction 20h, stirring velocity is 130r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 75 DEG C of conditions freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 370 DEG C of constant temp. heating process 3h (temperature rise rate 1 DEG C/min), obtains cobalt acid nickel nano material.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1860F/g, and when current density is 2A/g, specific capacity value is 1390F/g; After 4000 charge-discharge tests, specific storage still remains on more than 90%.
Embodiment 3
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 55mL Polyethylene Glycol-600, then add 15g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 180 DEG C, under agitation isothermal reaction 24h, stirring velocity is 120r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 70 DEG C of conditions freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 400 DEG C of constant temp. heating process 10h (temperature rise rate 2 DEG C/min), obtains cobalt acid nickel nano material.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1920F/g, and when current density is 2A/g, specific capacity value is 1400F/g; After 4000 charge-discharge tests, specific storage still remains on more than 91%.
Embodiment 4
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 58mL Polyethylene Glycol-600, then add 13g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 190 DEG C, under agitation isothermal reaction 22h, stirring velocity is 140r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 76 DEG C of conditions freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 390 DEG C of constant temp. heating process 8h (temperature rise rate 1 DEG C/min), obtains cobalt acid nickel nano material.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1950F/g, and when current density is 2A/g, specific capacity value is 1390F/g; After 4000 charge-discharge tests, specific storage still remains on more than 90%.
Embodiment 5
The method steps that solvent-thermal method of the present invention prepares cobalt acid nickel nano material is as follows:
(1) 2.9gNi (NO is taken
3)
26H
2o (containing nickel ion 0.01mol), 5.8gCo (NO
3)
26H
2o (containing cobalt ion 0.02mol) and 0.01gKNO
3be scattered in 52mL Polyethylene Glycol-600, then add 11g anhydrous sodium acetate (NaCH
3cOO), ultrasonic to dissolving completely, be then transferred in reactor by the mixing solutions of gained, be heated to 195 DEG C, under agitation isothermal reaction 24h, stirring velocity is 150r/min; After question response terminates, precursor solution is cooled to room temperature, products therefrom is first used deionized water wash 3 times, then use absolute ethanol washing 3 times, and under 76 DEG C of conditions freeze-day with constant temperature, namely obtain presoma.
(2) gained presoma is placed in tube furnace in atmosphere through 370 DEG C of constant temp. heating process 6h (temperature rise rate 1 DEG C/min), obtains cobalt acid nickel nano material.
The cobalt of above-mentioned preparation acid nickel nano material is carried out charge-discharge test, and when current density is 0.5A/g, specific capacity value reaches higher value 1880F/g, and when current density is 2A/g, specific capacity value is 1380F/g; After 4000 charge-discharge tests, specific storage still remains on more than 91%.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. solvent-thermal method prepares a method for cobalt acid nickel nano material, it is characterized in that: step is as follows:
(1) by Ni (NO
3)
26H
2o, Co (NO
3)
26H
2o and micro-KNO
3join in Polyethylene Glycol-600 and fully dissolve, add anhydrous sodium acetate wherein and make it to dissolve completely, obtain mixing solutions;
(2) by the mixing solutions that obtains isothermal reaction certain hour under agitation in a kettle., washing, dries, obtains presoma;
(3) by presoma in atmosphere through 360-400 DEG C of constant temp. heating process, temperature rise rate is 1-2 DEG C/min, and soaking time is after 2-10h, obtains cobalt acid nickel nano material.
2. method according to claim 1, is characterized in that: the mol ratio of described nickel ion and cobalt ion is 0.97-1.04:2.
3. method according to claim 2, is characterized in that: the concentration of described nickel ion in Polyethylene Glycol-600 is 0.17-0.2mol/L.
4. method according to claim 1, is characterized in that: described KNO
3add-on be 0.0017-0.002mol/L.
5. method according to claim 1, is characterized in that: the add-on of described anhydrous sodium acetate is add 10-15g anhydrous sodium acetate in every 50-60mL Polyethylene Glycol-600.
6. method according to claim 1, is characterized in that: described in step (2), isothermal reaction is isothermal reaction 16-24h under the rotating speed of 120-150r/min under agitation.
7. the application rights cobalt acid nickel nano material that requires the arbitrary described method of 1-6 to prepare.
8. cobalt acid nickel nano material according to claim 7 is preparing the application in electrode of super capacitor.
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Cited By (2)
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| CN110395774A (en) * | 2019-07-19 | 2019-11-01 | 五邑大学 | A kind of preparation method and application of cobalt acid nickel porous material |
| CN114105224A (en) * | 2021-11-23 | 2022-03-01 | 黑龙江工程学院 | Preparation method and application of nickel hydroxide/carbon nano tube composite nanosheet |
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