CN105399151B - A kind of preparation method of cobalt acid nickel nano material - Google Patents
A kind of preparation method of cobalt acid nickel nano material Download PDFInfo
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- CN105399151B CN105399151B CN201510829413.5A CN201510829413A CN105399151B CN 105399151 B CN105399151 B CN 105399151B CN 201510829413 A CN201510829413 A CN 201510829413A CN 105399151 B CN105399151 B CN 105399151B
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Abstract
The present invention provides a kind of preparation method of cobalt acid nickel nano material, and step is as follows：(1) nickel nitrate and cobalt nitrate are dissolved in the in the mixed solvent of 1,2 propane diols and water, then adding urea thereto is completely dissolved it, obtains mixed solution；The volume ratio of 1,2 propane diols and water is 1:10‑1:4；(2) by obtained mixed solution, isothermal reaction for a period of time, is washed in a kettle, drying, obtains cobalt acid nickel nano material presoma；(3) presoma is obtained into cobalt acid nickel nano material in atmosphere after 280 320 DEG C of constant temperature are heat-treated.The cobalt acid nickel nano material of the present invention is in charge-discharge test, and when current density is 5A/g, specific capacity value has reached higher value 1850F/g, when current density is 2A/g, specific capacity value 1460F/g；Specific capacity remains at more than 90% after 3000 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 preparation method of cobalt acid nickel nano material.
Background technology
Cobalt acid nickel (NiCo2O4) it is a kind of AB of Spinel structure2O4Type composite oxides, it is 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 have preferable electric conductivity in itself.In addition, cobalt acid nickel has higher chemical property,
Production cost is low, raw material abundance and advantages of environment protection, has attracted the common concern of researcher, in Germany《Germany should
With chemistry》Magazine (2015, volume 54 page 1868) has been reported.At present, the method that existing document report prepares cobalt acid nickel 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 expenditure is relatively small and product is easily controllable, anti-
The advantages that shorter between seasonable.In the U.S.《Nanometer bulletin》Magazine (2013, volume 13 page 3135) and Germany《Advanced material》
Magazine (2013, volume 25 page 976) has been reported, and patent CN201210222916.2 also discloses that the synthetic method of cobalt acid nickel.
The content of the invention
The invention provides a kind of preparation method of cobalt acid nickel nano material, the cobalt acid nickel being prepared using this method is received
Rice material specific surface area is big, specific capacity is high, can be used as ultracapacitor electric capacity.
The present invention provides a kind of preparation method of cobalt acid nickel nano material, and step is as follows：
(1) by Ni (NO3)2·6H2O and Co (NO3)2·6H2O is dissolved in the in the mixed solvent of 1,2-PD and water, then
Adding urea thereto is completely dissolved it, obtains mixed solution；The volume ratio of the 1,2- propane diols and water is 1:10-1:4；
(2) by obtained mixed solution, isothermal reaction for a period of time, is washed in a kettle, drying, is obtained cobalt acid nickel and is received
Rice material precursor；
(3) presoma is obtained into cobalt acid nickel nano material in atmosphere after 280-320 DEG C of constant temperature is heat-treated.
Through experiment, only when the volume ratio of 1,2-PD and water is 1:10-1:When 4, a kind of specific surface area can be just obtained
The cobalt acid nickel nano material big with specific capacity.
Preferably, the amount ratio of the material of nickle atom and cobalt atom is 0.97-1.04 in the mixed solution:2.Nickel ion
Mol ratio with cobalt ions is 1:When 2, cobalt nickle atom is just completely formed NiCo2O4, but be not excluded for process conditions limitation make cobalt nickel
Atom loses, and now can suitably adjust both and match, but need to make it in 0.97-1.04:Between 2.
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 mixed solution are 0.4mol/L.
The size of nickel ion and concentration of cobalt ions can also influence the performance of final products, through experiment, when nickel ion is mixing
When molar concentration in solution is 0.4mol/L, the specific surface area and specific capacity value of obtained product are maximum.
Preferably, the temperature of mixed solution isothermal reaction in a kettle is 120-150 DEG C in step (2), during reaction
Between be 14-20 hours.
Preferably, washing is first to be washed with deionized 3 times described in step (2), then washed 3 times with absolute ethyl alcohol.
Preferably, drying described in step (2) is that vacuum constant temperature dries 10-15h at 60-70 DEG C.
The present invention also provides the application cobalt acid nickel nano material that any of the above-described described method is prepared.
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 is with Ni (NO3)2·6H2O and Co (NO3)2·6H2O is reaction raw materials, using 1,2-PD and water to mix
Solvent, using urea as precipitating reagent, after presoma is prepared by solvent-thermal method, and then a kind of NiCo is prepared2O4Nanometer material
Material, preparation method is simple, product cost is low, is adapted to large-scale production, for NiCo2O4Further exploitation, certain using playing
Impetus.
The cobalt acid nickel nano material of the present invention is in charge-discharge test, and when current density is 5A/g, specific capacity value reaches
Compare high value 1850F/g, when current density is 2A/g, specific capacity value 1460F/g；After 3000 charge-discharge tests
Specific capacity remains at more than 90%, can be used as electrode material for super capacitor.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
Apply example to be used to explain the present invention together, be 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 prepared in embodiment 1, wherein：Abscissa is the angle of diffraction
Spend (2 θ), ordinate is relative diffracted intensity.
Embodiment
Following embodiment is only the preferred embodiment of the present invention, should not be construed as limitation of the invention.Following implementations
Experimental method in example, is conventional method unless otherwise specified.It is raw materials used in experiment：Ni(NO3)2·6H2O and Co
(NO3)2·6H2O is that analysis is pure.
Embodiment 1
The preparation method step of the cobalt acid nickel nano material of the present invention is as follows：
(1) by 2.9gNi (NO3)2·6H2O (containing nickel ion 0.01mol) and 5.8g Co (NO3)2·6H2O (contains cobalt ions
0.02mol) it is dissolved in the in the mixed solvent of 1,2-PD and water, the volume of 1,2-PD is 5ml, the volume of deionized water
For 20ml, then adding 7.2g urea thereto is completely dissolved it, obtains mixed solution；
(2) obtained mixed solution is transferred in reactor, 135 DEG C of isothermal reaction 16h is heated to, after question response terminates
Precursor solution is cooled to room temperature, products therefrom is first washed with deionized 3 times, then is washed 3 times with absolute ethyl alcohol, and
Vacuum constant temperature dries 13h under the conditions of 70 DEG C, obtains cobalt acid nickel nano material presoma；
(3) gained presoma is placed in tube furnace in atmosphere after 300 DEG C of constant temperature are heat-treated 2h, obtains cobalt acid nickel and receive
Rice material.The programming rate of heat treatment is 1 DEG C/min.
The cobalt acid nickel nano material of above-mentioned preparation is subjected to charge-discharge test, when current density is 5A/g, specific capacity value reaches
Higher value 1850F/g has been arrived, when current density is 2A/g, specific capacity value 1460F/g；By 3000 charge-discharge tests
Specific capacity remains at more than 90% afterwards.
Embodiment 2
The preparation method step of the cobalt acid nickel nano material of the present invention is as follows：
(1) by 2.9gNi (NO3)2·6H2O (contains nickel ion 6.0 × 10-4) and 5.8g Co (NO mol3)2·6H2O (contains cobalt
Ion 1.2 × 10-3Mol) be dissolved in the in the mixed solvent of 1,2-PD and water, the volume of 1,2-PD is 2.3ml, go from
The volume of sub- water is 22.7ml, then adding 6.0g urea thereto is completely dissolved it, obtains mixed solution；
(2) obtained mixed solution is transferred in reactor, 150 DEG C of isothermal reaction 14h is heated to, after question response terminates
Precursor solution is cooled to room temperature, products therefrom is first washed with deionized 3 times, then is washed 3 times with absolute ethyl alcohol, and
Vacuum constant temperature dries 15h under the conditions of 60 DEG C, obtains cobalt acid nickel nano material presoma；
(3) gained presoma is placed in tube furnace in atmosphere after 320 DEG C of constant temperature are heat-treated 2h, obtains cobalt acid nickel and receive
Rice material.The programming rate of heat treatment is 2 DEG C/min.
The cobalt acid nickel nano material of above-mentioned preparation is subjected to charge-discharge test, when current density is 5A/g, specific capacity value reaches
Higher value 1830F/g has been arrived, when current density is 2A/g, specific capacity value 1480F/g；By 3000 charge-discharge tests
Specific capacity remains at more than 91% afterwards.
Embodiment 3
The preparation method step of the cobalt acid nickel nano material of the present invention is as follows：
(1) by 2.9gNi (NO3)2·6H2O (containing nickel ion 0.01mol) and 5.8g Co (NO3)2·6H2O (contains cobalt ions
0.02mol) it is dissolved in the in the mixed solvent of 1,2-PD and water, the volume of 1,2-PD is 3.1ml, the body of deionized water
Product is 21.9ml, then adding 9.0g urea thereto is completely dissolved it, obtains mixed solution；
(2) obtained mixed solution is transferred in reactor, 120 DEG C of isothermal reaction 20h is heated to, after question response terminates
Precursor solution is cooled to room temperature, products therefrom is first washed with deionized 3 times, then is washed 3 times with absolute ethyl alcohol, and
Vacuum constant temperature dries 14h under the conditions of 65 DEG C, obtains cobalt acid nickel nano material presoma；
(3) gained presoma is placed in tube furnace in atmosphere after 280 DEG C of constant temperature are heat-treated 2h, obtains cobalt acid nickel and receive
Rice material.The programming rate of heat treatment is 2 DEG C/min.
The cobalt acid nickel nano material of above-mentioned preparation is subjected to charge-discharge test, when current density is 5A/g, specific capacity value reaches
Higher value 1790F/g has been arrived, when current density is 2A/g, specific capacity value 1470F/g；By 3000 charge-discharge tests
Specific capacity remains at more than 87% afterwards.
Embodiment 4
The preparation method step of the cobalt acid nickel nano material of the present invention is as follows：
(1) by 2.9gNi (NO3)2·6H2O (containing nickel ion 0.01mol) and 5.8g Co (NO3)2·6H2O (contains cobalt ions
0.02mol) it is dissolved in the in the mixed solvent of 1,2-PD and water, the volume of 1,2-PD is 4.2ml, the body of deionized water
Product is 20.8ml, then adding 8.0g urea thereto is completely dissolved it, obtains mixed solution；
(2) obtained mixed solution is transferred in reactor, 140 DEG C of isothermal reaction 15h is heated to, after question response terminates
Precursor solution is cooled to room temperature, products therefrom is first washed with deionized 3 times, then is washed 3 times with absolute ethyl alcohol, and
Vacuum constant temperature dries 10h under the conditions of 62 DEG C, obtains cobalt acid nickel nano material presoma；
(3) gained presoma is placed in tube furnace in atmosphere after 290 DEG C of constant temperature are heat-treated 2h, obtains cobalt acid nickel and receive
Rice material.The programming rate of heat treatment is 1 DEG C/min.
The cobalt acid nickel nano material of above-mentioned preparation is subjected to charge-discharge test, when current density is 5A/g, specific capacity value reaches
Higher value 1760F/g has been arrived, when current density is 2A/g, specific capacity value 1510F/g；By 3000 charge-discharge tests
Specific capacity remains at more than 89% afterwards.
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 the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (3)
- A kind of 1. preparation method of cobalt acid nickel nano material, it is characterised in that：Step is as follows：（1）By Ni (NO3)2·6H2O and Co (NO3)2·6H2O is dissolved in the in the mixed solvent of 1,2-PD and water, then to its Middle addition urea is completely dissolved it, obtains mixed solution；The volume ratio of the 1,2- propane diols and water is 1:10-1:4；It is described The amount ratio of the material of nickel ion and cobalt ions is 0.97-1.04 in mixed solution:2；Ni (the NO3)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 mixed solution is 0.4mol/L；（2）By the isothermal reaction in a kettle of obtained mixed solution, the temperature of reaction is 120-150 DEG C, reaction time 14- 20 hours, wash, drying, obtain cobalt acid nickel nano material presoma；（3）By presoma in atmosphere after 280-320 DEG C of constant temperature is heat-treated, cobalt acid nickel nano material is obtained.
- 2. according to the method for claim 1, it is characterised in that：Step（2）Described in washing be first to be washed with deionized 3 It is secondary, then washed 3 times with absolute ethyl alcohol.
- 3. according to the method for claim 1, it is characterised in that：Step（2）Described in drying be that vacuum is permanent at 60-70 DEG C Temperature dries 10-15h.
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| RU2756678C1 (en) * | 2021-04-01 | 2021-10-04 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for obtaining a nanopowder of complex nickel-cobalt oxide with a spinel structure |
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| CN106011911B (en) * | 2016-05-26 | 2018-04-17 | 重庆大学 | A kind of method that partial vulcanization improves metal hydroxides analysis oxygen electrode performance |
| CN106328383B (en) * | 2016-09-12 | 2018-05-11 | 电子科技大学 | A kind of preparation method of microspheroidal hierarchy carbon parcel cobalt acid nanosized nickel rods composite material |
| CN106564968A (en) * | 2016-11-17 | 2017-04-19 | 东华大学 | Preparation method for nickel cobaltite electrode material with high specific surface area |
| 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 |
| CN108680625A (en) * | 2018-05-07 | 2018-10-19 | 杭州电子科技大学 | The preparation method and applications of cuprous oxide/cobalt acid nickel hollow-core construction composite nano-microsphere |
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| CN103771542B (en) * | 2014-01-22 | 2015-02-18 | 广东工业大学 | Preparation method for high-heat stability cobalt oxide with large specific surface |
| CN103979618B (en) * | 2014-05-05 | 2016-05-18 | 同济大学 | The synthetic method of cobalt acid nickel nano material for a kind of ultracapacitor |
| CN104505508A (en) * | 2014-12-17 | 2015-04-08 | 江苏合志锂硫电池技术有限公司 | Preparation method of nickel cobalt oxide electrode material |
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| RU2756678C1 (en) * | 2021-04-01 | 2021-10-04 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for obtaining a nanopowder of complex nickel-cobalt oxide with a spinel structure |
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