CN105800698B - A kind of preparation method of the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade - Google Patents
A kind of preparation method of the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade Download PDFInfo
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Abstract
The invention belongs to energy storage technical field of material, the preparation method of the flower ball-shaped cobaltosic oxide material of specially a kind of three-dimensional nanometer-grade.Cobalt acetate is mixed ultrasonic 15 30min with deionized water first and prepares cobalt acetate dispersion liquid by preparation method of the present invention, and the pH of dispersion liquid is then adjusted with weak acid；Ammonia spirit is subsequently added into, after being well mixed, above-mentioned solution is moved into hydrothermal reaction kettle, is reacted at a temperature of 100 140 DEG C and centrifuges, washs after 12 16h, be dried to obtain cobalt hydroxide powder；Obtained cobalt hydroxide powder is finally calcined into the cobaltosic oxide material that certain time produces the flower ball-shaped of three-dimensional nanometer-grade at a certain temperature.Preparation method of the present invention is simple and reliable, with low cost, environmental protection.There is obtained cobaltosic oxide material hierarchy, specific capacity to be up to 679F/g, circulation and good rate capability.
Description
Technical field
The present invention relates to a kind of preparation method of the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, belong to energy storage
Technical field of material.
Background technology
Fast development and increasingly deficient, the various problem of environmental pollution phases of progressive and traditional fossil energy with science and technology
After appearance, a kind of new clean energy resource of urgent requirement scientists study.Ultracapacitor has fast charging and discharging, power close
Degree is high, have extended cycle life, operating temperature range extensively, Environmental Safety the advantages of, it is adaptable to some common portable systems,
Such as electronic product and power vehicle, as a kind of very promising new energy memory device.And cobaltosic oxide be then it is a kind of very
Important transition metal oxide, its theoretical specific capacity is up to 3560F/g, and powder, which is presented, does not dissolve in salt under (ash) black, normal temperature
The strong acid such as acid, nitric acid, but hot sulfuric acid can be slowly dissolved in, its is cheap, natural resources storage level is big.
Co3O4Belong to cubic system, be a kind of important p-type semiconductor, its lattice parameter is 0.809nm, with sharp brilliant
Stone AB2O4Structure, have higher crystalline field stability.Because of its unique physics and chemical property, in sensor, lithium ion
Had a wide range of applications in terms of battery, ultracapacitor and catalysis.
Co3O4The main preparation methods of material are constantly updated, and mainly have sol-gel process, spray heating decomposition, water now
Thermal synthesis method, chemical precipitation method etc., but cobaltosic oxide nano particle be easy to be agglomerated into preparation process bulky grain and
Structural stability is poor, and its pattern, crystal formation, the stability of specific surface area and structure have important influence to performance.Therefore,
High-performance cobaltosic oxide material is prepared to be particularly important.
The content of the invention
In view of the shortcomings of the prior art, three-dimensional nanometer-grade is prepared easily to operate it is an object of the invention to provide a kind of
The method of flower ball-shaped cobaltosic oxide material.The present invention is prepared using hydro-thermal-method for calcinating, and obtained three-dimensional material pattern can
Control, crystallinity is high, with hierarchy, particle size is uniform and dispersiveness is fine.
Technical scheme is specifically described as follows.
The present invention provides a kind of preparation method of the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, and specific steps are such as
Under：
(1) it is 5 according to mass volume ratio：1-20:1mg/ml, ultrasound 15- in deionized water is added to by cobalt acetate
30min, obtains dispersed cobalt acetate solution, weak acid is then added thereto, and the pH value of solution is adjusted into 6.0-6.5；
(2) 25wt%-28wt% ammonia spirits are added in the solution obtained to step (1), hydro-thermal is moved into after being well mixed
In reactor, reacted at a temperature of 100-140 DEG C, after reaction terminates, naturally cool to room temperature, obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged, collects precipitation；Then precipitation is washed with deionized water and absolute ethyl alcohol
PH value to efflux obtains cobalt hydroxide powder in neutrality；
(4) cobalt hydroxide powder obtained by step (3) is risen to 800-850 DEG C with 5-8 DEG C/min programming rate, in air
Condition calcines 2-3h, and room temperature is naturally cooled to afterwards, that is, obtains the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade.
In above-mentioned steps (1), ultrasonic power is 300-400w.
In above-mentioned steps (1), the weak acid is any in citric acid, acetic acid or hydrofluoric acid.
In above-mentioned steps (2), the mass ratio of the 25wt%-28wt% ammonia spirits and cobalt acetate is 1:3-1:10.
In above-mentioned steps (2), the hydro-thermal time is 12-16h.
In above-mentioned steps (3), drying temperature is 60-80 DEG C, and drying time is 10-12h.
Three-dimensional cobaltosic oxide material of the present invention as obtained by above-mentioned preparation method is in flower ball-shaped pattern, the oxygen of flower ball-shaped four
Change three cobalts a diameter of 8-15 μm, it is made up of particle diameter for 400-600nm nano particle.
Compared with existing preparation method, beneficial effects of the present invention are as described below：
1st, the synthetic method is simple, raw material sources enrich, and with low cost, preparation process is environmentally friendly.
2nd, of the invention to obtain cobaltosic oxide material, in flower ball-shaped, it is made up of nano particle, with hierarchy.
3rd, the obtained cobaltosic oxide material of the present invention, the cavernous structure with three dimensional micron or nanometer, dispersive property is good,
Particle size is uniform, crystallinity height and morphology controllable.
4th, the cobaltosic oxide material that the present invention is obtained has preferable electro-chemical activity, and its specific capacity is reached as high as
679F/g, therefore can be directly used for electrode material for super capacitor.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the gained cobalt hydroxide material of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the gained cobaltosic oxide material of embodiment 1.
Fig. 3 is the X-ray diffractogram of the gained cobaltosic oxide material of embodiment 1.
Fig. 4 is the scanning electron microscope (SEM) photograph of the gained cobalt hydroxide material of embodiment 2.
Fig. 5 is the performance chart of the gained cobaltosic oxide material of embodiment 2.
Fig. 6 is the scanning electron microscope (SEM) photograph of the gained cobaltosic oxide material of embodiment 3.
Embodiment
The present invention is described further below by specific embodiment and with reference to accompanying drawing, it is necessary to which what is illustrated is that this is specific real
Example is applied, the limitation to the claimed scope of the invention is not constituted.
Using charge-discharge performance and stability of the blue electric battery test system to the cobaltosic oxide material obtained by the present invention
Tested, step is as follows：
Calculate in mass ratio, a kind of flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade obtained by the present invention：Conductive charcoal
It is black：Bonding agent (PTFE) is 8:1:1 ratio is mixed, and the mixture of gained is added to ultrasonic agitation 30- in absolute ethyl alcohol
60min, the slurry of the gained film in the nickel foam cut out and handled well in advance, film area is about 1cm2, film will be coated
Nickel foam be placed in 60-80 DEG C of baking oven and dry 10-12h, obtain scribbling the nickel foam of cobaltosic oxide material, weigh and subtract
Nickel foam net weight obtains the quality of applied cobaltosic oxide material；
The nickel foam for scribbling cobaltosic oxide material using above-mentioned gained is working electrode, using blank nickel foam as to electricity
Pole, using saturated calomel electrode as reference electrode, constitutes and the 6M KOH aqueous solution is added in three-electrode system, three electrode glass electrolytic cells
As electrolyte, respectively by working electrode, blank nickel foam is put into electrode and reference electrode in three electrode glass electrolytic cells, is connect
Go out corresponding test mouth, constant current charge-discharge loop test carried out in the case of current density 1A/g using blue electric discharge and recharge instrument,
Discharge and recharge instrument is picked out using alligator clip.
Absolute ethyl alcohol needed for various embodiments of the present invention is pure to analyze, and other reagents are that chemistry is pure, are bought in traditional Chinese medicines
Solution on Chemical Reagents in Shanghai company of group.
Embodiment 1
A kind of flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, method as follows is prepared from：
(1) 150mg cobalt acetates are added in 30ml deionized waters, it is ultrasonic at ambient temperature with 350w power
15min, obtains dispersed cobalt acetate solution, then with 1.0mol/L citric acid solution by salting liquid pH obtained above
Value is adjusted to 6.0-6.5；
(2) 50mg ammonia spirits (25wt%-28wt%) are added in the solution obtained to step (1), is moved after being well mixed
Enter in hydrothermal reaction kettle, reacted in 100 DEG C of baking box after 14h, naturally cool to room temperature and obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged under the conditions of 7000r/min, then with deionized water and absolute ethyl alcohol
Repeatedly washing is 7 to efflux pH, and 10h is finally dried under the conditions of 60 DEG C obtains cobalt hydroxide powder；
(4) cobalt hydroxide powder presoma obtained by step (3) is risen to 800 DEG C with 5 DEG C/min programming rate, in air
Under the conditions of carry out after calcination processing 2.5h, naturally cool to room temperature and can obtain nano level three-dimensional cobaltosic oxide flower ball-shaped
Material；
Using surface texture of the S-3400N electron microscopes (Hitachi) to the cobalt hydroxide material of the gained of above-described embodiment 1
It is scanned, the scanning electron microscope (SEM) photograph of gained is as shown in figure 1, from figure 1 it appears that the cobalt hydroxide material of gained is three wieners
The flower ball-shaped structure of meter level.
The surface of the cobaltosic oxide material of the gained of above-described embodiment 1 is tied using S-3400N electron microscopes (Hitachi)
Structure is scanned, the scanning electron microscope (SEM) photograph of gained as shown in Fig. 2 from figure 2 it can be seen that the cobaltosic oxide material of gained still
Nanoscale structures with flower ball-shaped pattern, a diameter of 8-15 μm of flower ball-shaped cobaltosic oxide, it is 400-600nm by particle diameter
Nano particle constitute.
The cobaltosic oxide material of above-mentioned gained is measured using Rigaku X-ray diffractometers, the X-ray of gained
Diffraction pattern is as shown in figure 3, from figure 3, it can be seen that diffraction maximum has all corresponded to the diffraction maximum of cobaltosic oxide well in figure, show
The diffraction maximum shown is consistent with the standard card of cobaltosic oxide crystal (JCPDS no.43-1003), has been indicated above material
Middle product is single cobaltosic oxide and better crystallinity degree.
Using blue electric battery test system (LAND 2001A system), at ambient temperature, from three-electrode system,
Using the 6M KOH aqueous solution as electrolyte, electrochemical window is set to three-dimensional cobaltosic oxide materials of the 0-0.4V to the gained of above-described embodiment 1
Capacitor chemical property and stability tested, show that specific capacity is about under 1A/g charging and discharging currents density
650F/g, and after the circle of circulation 1000, still with higher specific capacity 612F/g.
Embodiment 2
A kind of flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, method as follows is prepared from：
(1) 300mg cobalt acetates are added in 30ml deionized waters, it is ultrasonic at ambient temperature with 350w power
20min, obtains dispersed cobalt acetate solution, then with 1.0mol/L acetum by salting liquid pH value obtained above
It is adjusted to 6.0-6.5；
(2) 100mg ammonia spirits (25wt%-28wt%) are added in the solution obtained to step (1), is moved after being well mixed
Enter in hydrothermal reaction kettle, reacted in 120 DEG C of baking box after 14h, naturally cool to room temperature and obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged under the conditions of 8000r/min, then with deionized water and absolute ethyl alcohol
Repeatedly washing is 7 to efflux pH, and 10h is finally dried under the conditions of 70 DEG C obtains cobalt hydroxide powder；
(4) cobalt hydroxide powder presoma obtained by step (3) is risen to 850 DEG C with 5 DEG C/min programming rate, in air
Under the conditions of carry out after calcination processing 3h, naturally cool to room temperature and can obtain nano level three-dimensional cobaltosic oxide flower ball-shaped material
Material；
Using surface texture of the S-3400N electron microscopes (Hitachi) to the cobalt hydroxide material of the gained of above-described embodiment 2
It is scanned, the scanning electron microscope (SEM) photograph of gained is as shown in figure 4, figure 4, it is seen that the cobaltosic oxide material of gained is in bouquet
Shape structure, a diameter of 8-15 μm of the flower ball-shaped cobaltosic oxide, it is made up of particle diameter for 400-600nm nano particle,
And be evenly distributed, dispersiveness very well.
Using blue electric battery test system (LAND 2001A system), at ambient temperature, from three-electrode system,
Using the 6M KOH aqueous solution as electrolyte, electrochemical window is set to three-dimensional cobaltosic oxide materials of the 0-0.4V to the gained of above-described embodiment 2
Capacitor chemical property and stability tested, the performance chart of gained is as shown in figure 5, as can be seen from Figure 5
Specific capacity is about 679F/g under 1A/g charging and discharging currents density, and after the circle of circulation 1000, still with higher specific volume
Measure 650F/g.It is indicated above that the three-dimensional flower ball-shaped cobaltosic oxide material obtained by the present invention is with very high specific capacity and very well
Cyclical stability.
Embodiment 3
A kind of flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, method as follows is prepared from：
(1) 450mg cobalt acetates are added in 30ml deionized waters, it is ultrasonic at ambient temperature with 400w power
25min, obtains dispersed cobalt acetate solution, then with 1.0mol/L hydrofluoric acid solution by salting liquid pH obtained above
Value is adjusted to 6.0-6.5；
(2) 75mg ammonia spirits are added in the solution obtained to step (1), are moved into after being well mixed in hydrothermal reaction kettle,
Reacted in 130 DEG C of baking box after 14h, naturally cool to room temperature and obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged under the conditions of 8000r/min, then with deionized water and absolute ethyl alcohol
Repeatedly washing is 7 to efflux pH, and 10h is finally dried under the conditions of 80 DEG C obtains cobalt hydroxide powder；
(4) cobalt hydroxide powder presoma obtained by step (3) is risen to 820 DEG C with 8 DEG C/min programming rate, in air
Under the conditions of carry out after calcination processing 3h, naturally cool to room temperature and can obtain nano level three-dimensional cobaltosic oxide flower ball-shaped material
Material；
The surface of the cobaltosic oxide material of the gained of above-described embodiment 3 is tied using S-3400N electron microscopes (Hitachi)
Structure is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in fig. 6, from fig. 6 it can be seen that the oxidation of three-dimensional flower ball-shaped four three of gained
Cobalt material is made up of many nano-scale particles, and particle diameter is about 400nm.
Using blue electric battery test system (LAND 2001A system), at ambient temperature, from three-electrode system,
Using the 6M KOH aqueous solution as electrolyte, electrochemical window is set to three-dimensional cobaltosic oxide materials of the 0-0.4V to the gained of above-described embodiment 3
Capacitor chemical property and stability tested, must beat the specific capacity under 1A/g charging and discharging currents density is about
627F/g, and after the circle of circulation 1000, still with higher specific capacity 592F/g.
Embodiment 4
A kind of flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, method as follows is prepared from：
(1) 600mg cobalt acetates are added in 30ml deionized waters, it is ultrasonic at ambient temperature with 400w power
30min, obtains dispersed cobalt acetate solution, then with 1.0mol/L citric acid solution by salting liquid pH obtained above
Value is adjusted to 6.0-6.5；
(2) 60mg ammonia spirits (25wt%-28wt%) are added in the solution obtained to step (1), is moved after being well mixed
Enter in hydrothermal reaction kettle, reacted in 140 DEG C of baking box after 16h, naturally cool to room temperature and obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged under the conditions of 8000r/min, then with deionized water and absolute ethyl alcohol
Repeatedly washing is 7 to efflux pH, and 12h is finally dried under the conditions of 80 DEG C obtains cobalt hydroxide powder；
(4) cobalt hydroxide powder presoma obtained by step (3) is risen to 800 DEG C with 8 DEG C/min programming rate, in air
Under the conditions of carry out after calcination processing 3h, naturally cool to room temperature and can obtain nano level three-dimensional cobaltosic oxide flower ball-shaped material
Material；
In summary, the flower ball-shaped cobaltosic oxide material for a kind of three-dimensional nanometer-grade that the present invention is provided, it has three-dimensional
, there is the crystallinity that hierarchy is become reconciled in pattern, and specific capacity is up to 679F/g, can with remarkable circulation and high rate performance
For use as ultracapacitor.
Described above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, some improvement can also be made, these improvement also should be regarded as this
The protection domain of invention.
Claims (6)
1. the preparation method of the flower ball-shaped cobaltosic oxide material of a kind of three-dimensional nanometer-grade, it is characterised in that comprise the following steps that：
(1) it is 5 according to mass volume ratio：1-20:1mg/mL, is added to ultrasound 15-30min in deionized water by cobalt acetate, obtains
To dispersed cobalt acetate solution, weak acid is then added thereto, and the pH value of solution is adjusted to 6.0-6.5；
(2) 25wt%-28wt% ammonia spirits are added in the solution obtained to step (1), hydrothermal reaction kettle is moved into after being well mixed
In, reacted at a temperature of 100-140 DEG C, after reaction terminates, naturally cool to room temperature and obtain reaction solution；
(3) reaction solution obtained by step (2) is centrifuged, collects precipitation；Then washed with deionized water and absolute ethyl alcohol and be precipitated to stream
Go out the pH value of liquid in neutrality, cobalt hydroxide powder is finally dried to obtain under the conditions of 60-80 DEG C；
(4) cobalt hydroxide powder obtained by step (3) is risen to 800-850 DEG C with 5-8 DEG C/min programming rate, in air conditionses
Lower calcining 2-3h, naturally cools to room temperature afterwards, that is, obtains the flower ball-shaped cobaltosic oxide material of three-dimensional nanometer-grade, its is a diameter of
8-15 μm, it is made up of particle diameter for 400-600nm nano particle.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), ultrasonic power is 300-400W.
3. preparation method as claimed in claim 1, it is characterised in that in step (1), the weak acid be citric acid, acetic acid or
It is any in hydrofluoric acid.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), the 25wt%-28wt% ammonia spirits
Mass ratio with cobalt acetate is 1:3-1:10.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), the hydro-thermal time is 12-16h.
6. preparation method as claimed in claim 1, it is characterised in that in step (3), drying temperature is 60-80 DEG C, when drying
Between be 10-12h.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106219615B (en) * | 2016-08-23 | 2017-09-29 | 肖洋 | The preparation method of flower-shaped cobalt hydroxide microballoon |
| CN106542584A (en) * | 2016-10-19 | 2017-03-29 | 常州大学 | A kind of preparation method of rich defect cobalt oxide photocatalyst |
| CN106450254B (en) * | 2016-11-03 | 2018-11-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Ni, Sb- codope cobaltosic oxide nano oxide |
| CN107162066B (en) * | 2017-05-26 | 2019-01-01 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of nickel doped cobaltic-cobaltous oxide nano flower composite material and its preparation method and application |
| CN108666144A (en) * | 2018-05-04 | 2018-10-16 | 上海应用技术大学 | A kind of three-dimensional flower-shaped cobalt hydroxide-graphene composite material and preparation method thereof |
| CN108615612A (en) * | 2018-05-04 | 2018-10-02 | 上海应用技术大学 | A kind of flower-shaped cobaltosic oxide-graphene composite material and preparation method thereof |
| CN110182854B (en) * | 2019-06-10 | 2022-03-22 | 中国科学院青岛生物能源与过程研究所 | Sea urchin-like cobaltosic oxide photothermal conversion film and preparation method and application thereof |
| CN110683589B (en) * | 2019-10-17 | 2022-03-25 | 宁波大学 | Preparation method of cobaltosic oxide nano material |
| CN115974170A (en) * | 2022-12-02 | 2023-04-18 | 惠州学院 | Universal preparation method of cobaltosic oxide porous nano material with special morphology |
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