CN105800698A - Preparation method of three-dimensional nanoscale flower-like structure cobaltosic oxide material - Google Patents
Preparation method of three-dimensional nanoscale flower-like structure cobaltosic oxide material Download PDFInfo
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Abstract
The invention belongs to the technical field of energy storage material preparation, and in particular relates to a preparation method of a three-dimensional nanoscale flower-like structure cobaltosic oxide material. The preparation method comprises the following steps of: firstly, performing ultrasonic mixing on cobalt acetate and deionized water for 15-30 minutes so as to prepare a cobalt acetate dispersion liquid, and adjusting the pH value of the dispersion liquid by using weak acid; adding a ammonia water solution, uniformly mixing, transferring the solution into a hydrothermal reaction kettle, enabling the components to react for 12-16 hours at 100-140 DEG C, centrifuging, washing, and drying so as to obtain cobalt hydroxide powder; and finally, calcining the obtained cobalt hydroxide powder at certain temperature for a certain time, thereby obtaining the three-dimensional nanoscale flower-like structure cobaltosic oxide material. The preparation method provided by the invention is simple and reliable, low in cost and environment-friendly. The prepared t cobaltosic oxide material has a graded structure and is good in circulation and rate capability, and the specific capacity is as high as 679F/g.
Description
Technical field
The present invention relates to the preparation method of the flower ball-shaped Cobalto-cobaltic oxide material of a kind of three-dimensional nanometer-grade, belong to energy storage material
Preparing technical field.
Background technology
Day by day deficient along with the fast development of science and technology and progress and traditional fossil energy, various problem of environmental pollutions go out in succession
Existing, a kind of new clean energy resource of urgent requirement scientists study.Ultracapacitor has fast charging and discharging, power density
High, have extended cycle life, operating temperature range extensively, the advantage such as Environmental Safety, it is adaptable to some common portable systems,
Such as electronic product and power vehicle, become a kind of very promising new forms of energy memory device.Cobalto-cobaltic oxide be then one very
Important transition metal oxide, its theoretical specific capacity is up to 3560F/g, and powder presents (grey) black, insoluble in salt under room temperature
The strong acid such as acid, nitric acid, but can slowly be dissolved in hot sulphuric acid, and it is cheap, natural resources storage level is big.
Co3O4Belonging to cubic system, be a kind of important p-type quasiconductor, its lattice parameter is 0.809nm, has spinelle
AB2O4Structure, have higher crystalline field stability.Because of physics and the chemical property of its uniqueness, sensor, lithium from
The aspects such as sub-battery, ultracapacitor and catalysis have a wide range of applications.
Co3O4The main preparation methods of material is constantly updated, and mainly has sol-gel process, spray heating decomposition, hydro-thermal
Synthetic method, chemical precipitation method etc., but cobaltosic oxide nano granule is easy to be agglomerated into bulky grain and knot in preparation process
Structure less stable, and the stability of its pattern, crystal formation, specific surface area and structure has important impact to performance.Therefore,
Prepare high-performance Cobalto-cobaltic oxide material to be particularly important.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of easy and simple to handle bouquet preparing three-dimensional nanometer-grade
The method of shape Cobalto-cobaltic oxide material.The present invention uses hydro-thermal-method for calcinating to prepare, the three-dimensional material morphology controllable that obtains, knot
Crystalline substance degree is high, have hierarchy, and size is uniform and dispersibility is fine.
Technical scheme is specifically described as follows.
The present invention provides the preparation method of the flower ball-shaped Cobalto-cobaltic oxide material of a kind of three-dimensional nanometer-grade, specifically comprises the following steps that
(1) it is 5:1-20:1mg/ml according to mass volume ratio, cobaltous acetate is joined ultrasonic 15-30min in deionized water,
To homodisperse cobalt acetate solution, then it is added thereto to weak acid, the pH value of solution is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 25wt%-28wt% ammonia spirit, after mix homogeneously, move into hydro-thermal reaction
In still, react at a temperature of 100-140 DEG C, after reaction terminates, naturally cool to room temperature, obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged, collects precipitation；Then it is precipitated to stream with deionized water and absolute ethanol washing
The pH value going out liquid is neutrality, obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder is risen to 800-850 DEG C with the programming rate of 5-8 DEG C/min, at air bar
Part calcining 2-3h, naturally cools to room temperature afterwards, i.e. obtains the flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade.
In above-mentioned steps (1), ultrasonic power is 300-400w.
In above-mentioned steps (1), described weak acid is any one in citric acid, acetic acid or Fluohydric acid..
In above-mentioned steps (2), the mass ratio of described 25wt%-28wt% ammonia spirit and cobaltous acetate is 1:3-1:10.
In above-mentioned steps (2), the hydro-thermal time is 12-16h.
In above-mentioned steps (3), baking temperature is 60-80 DEG C, and drying time is 10-12h.
The present invention is flower ball-shaped pattern by the three-dimensional Cobalto-cobaltic oxide material of above-mentioned preparation method gained, flower ball-shaped four oxygen
Changing a diameter of 8-15 μm of three cobalts, it is made up of the nano-particle that particle diameter is 400-600nm.
Compared with existing preparation method, beneficial effects of the present invention is as described below:
1, this synthetic method is simple, abundant raw material source, with low cost, preparation process environmental protection.
2, the present invention obtain Cobalto-cobaltic oxide material, in flower ball-shaped, it is made up of nano-particle, has hierarchy.
3, the Cobalto-cobaltic oxide material that the present invention obtains, has the cavernous structure of three dimensional micron or nanometer, and dispersive property is good, particle diameter
Size is uniform, degree of crystallinity height and morphology controllable.
4, the Cobalto-cobaltic oxide material that the present invention obtains has preferable electro-chemical activity, and its specific capacity reaches as high as 679F/g, because of
This can be directly used for electrode material for super capacitor.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 gained cobalt hydroxide material.
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained Cobalto-cobaltic oxide material.
Fig. 3 is the X-ray diffractogram of embodiment 1 gained Cobalto-cobaltic oxide material.
Fig. 4 is the scanning electron microscope (SEM) photograph of embodiment 2 gained cobalt hydroxide material.
Fig. 5 is the performance chart of embodiment 2 gained Cobalto-cobaltic oxide material.
Fig. 6 is the scanning electron microscope (SEM) photograph of embodiment 3 gained Cobalto-cobaltic oxide material.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is described further, it should be noted that and be originally embodied as
Example, is not intended that the restriction to claimed scope.
Use blue electricity battery test system that charge-discharge performance and the stability of the Cobalto-cobaltic oxide material of gained of the present invention are carried out
Test, step is as follows:
Calculate in mass ratio, the flower ball-shaped Cobalto-cobaltic oxide material of a kind of three-dimensional nanometer-grade of gained of the present invention: conductive black:
Bonding agent (PTFE) is that the ratio of 8:1:1 mixes, and the mixture of gained joins ultrasonic agitation in dehydrated alcohol
30-60min, the slurry of gained is film in the nickel foam cut out in advance and handle well, and film area is about 1cm2, will be coated with
The nickel foam of good film is placed in 60-80 DEG C of baking oven drying 10-12h, obtains scribbling the nickel foam of Cobalto-cobaltic oxide material, weighs
And deduct nickel foam net weight and obtain the quality of be coated with Cobalto-cobaltic oxide material；
With the nickel foam scribbling Cobalto-cobaltic oxide material of above-mentioned gained as working electrode, using blank nickel foam as to electrode,
With saturated calomel electrode as reference electrode, form three-electrode system, three electrode glass electrolyzers add 6M KOH aqueous solution
As electrolyte, respectively by working electrode, electrode and reference electrode are put in three electrode glass electrolyzers by blank nickel foam,
Pick out corresponding test port, use blue electricity discharge and recharge instrument to carry out constant current charge-discharge circulation in the case of electric current density 1A/g and survey
Examination, discharge and recharge instrument uses alligator clip to pick out.
In various embodiments of the present invention, required dehydrated alcohol is analytical pure, and other reagent are chemical pure, buy in traditional Chinese medicines group
Solution on Chemical Reagents in Shanghai company.
Embodiment 1
A kind of flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade, method as follows is prepared from:
(1) 150mg cobaltous acetate is joined in 30ml deionized water, with the most ultrasonic 15min of the power of 350w,
Obtain homodisperse cobalt acetate solution, then with the citric acid solution of 1.0mol/L by saline solution pH obtained above
Value is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 50mg ammonia spirit (25wt%-28wt%), move into after mix homogeneously
In hydrothermal reaction kettle, after reacting 14h in the baking box of 100 DEG C, naturally cool to room temperature and obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged under the conditions of 7000r/min, then uses deionized water and dehydrated alcohol repeatedly
Washing to effluent pH is 7, is finally dried 10h under the conditions of 60 DEG C and obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder presoma is risen to 800 DEG C with the programming rate of 5 DEG C/min, at air bar
After carrying out calcination processing 2.5h under part, naturally cool to room temperature and i.e. can get the Cobalto-cobaltic oxide flower of nano level three-dimensional
Spheroidal material；
Use S-3400N ultramicroscope (Hitachi) that the surface texture of the cobalt hydroxide material of above-described embodiment 1 gained is entered
Row scanning, the scanning electron microscope (SEM) photograph of gained is as it is shown in figure 1, from figure 1 it appears that the cobalt hydroxide material of gained is three-dimensional
Nano level flower ball-shaped structure.
Use the S-3400N ultramicroscope (Hitachi) surface texture to the Cobalto-cobaltic oxide material of above-described embodiment 1 gained
Be scanned, the scanning electron microscope (SEM) photograph of gained as in figure 2 it is shown, from figure 2 it can be seen that the Cobalto-cobaltic oxide material of gained still
So having the nanoscale structures of flower ball-shaped pattern, a diameter of 8-15 μm of flower ball-shaped Cobalto-cobaltic oxide, it by particle diameter is
The nano-particle of 400-600nm is constituted.
Using Rigaku X-ray diffractometer to be measured the Cobalto-cobaltic oxide material of above-mentioned gained, the X-ray of gained is spread out
Penetrate figure as it is shown on figure 3, from figure 3, it can be seen that all well corresponding diffraction maximum of Cobalto-cobaltic oxide of diffraction maximum in figure,
The diffraction maximum demonstrated is all consistent with the standard card of Cobalto-cobaltic oxide crystal (JCPDS no.43-1003), has been indicated above material
In material, product is single Cobalto-cobaltic oxide and better crystallinity degree.
Use blue electricity battery test system (LAND 2001A system), at ambient temperature, select three-electrode system, with
6M KOH aqueous solution is electrolyte, and electrochemical window is set to the 0-0.4V three-dimensional Cobalto-cobaltic oxide material to above-described embodiment 1 gained
Capacitor chemical property and stability test, show that under the charging and discharging currents density of 1A/g specific capacity is about
650F/g, and after circulation 1000 circle, still there is higher specific capacity 612F/g.
Embodiment 2
A kind of flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade, method as follows is prepared from:
(1) 300mg cobaltous acetate is joined in 30ml deionized water, with the most ultrasonic 20min of the power of 350w,
Obtain homodisperse cobalt acetate solution, then with the acetum of 1.0mol/L by saline solution pH obtained above
Value is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 100mg ammonia spirit (25wt%-28wt%), move into after mix homogeneously
In hydrothermal reaction kettle, after reacting 14h in the baking box of 120 DEG C, naturally cool to room temperature and obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged under the conditions of 8000r/min, then uses deionized water and dehydrated alcohol repeatedly
Washing to effluent pH is 7, is finally dried 10h under the conditions of 70 DEG C and obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder presoma is risen to 850 DEG C with the programming rate of 5 DEG C/min, at air bar
After carrying out calcination processing 3h under part, naturally cool to room temperature and i.e. can get the Cobalto-cobaltic oxide flower of nano level three-dimensional
Spheroidal material；
Use S-3400N ultramicroscope (Hitachi) that the surface texture of the cobalt hydroxide material of above-described embodiment 2 gained is entered
Row scanning, the scanning electron microscope (SEM) photograph of gained as shown in Figure 4, figure 4, it is seen that the Cobalto-cobaltic oxide material of gained is flower
Chondritic, a diameter of 8-15 μm of this flower ball-shaped Cobalto-cobaltic oxide, it is made up of the nano-particle that particle diameter is 400-600nm
, and be evenly distributed, dispersibility fine.
Use blue electricity battery test system (LAND 2001A system), at ambient temperature, select three-electrode system, with
6M KOH aqueous solution is electrolyte, and electrochemical window is set to the 0-0.4V three-dimensional Cobalto-cobaltic oxide material to above-described embodiment 2 gained
Capacitor chemical property and stability test, the performance chart of gained is as it is shown in figure 5, can from Fig. 5
Go out specific capacity under the charging and discharging currents density of 1A/g and be about 679F/g, and after circulation 1000 circle, still have higher
Specific capacity 650F/g.It is indicated above that the three-dimensional flower ball-shaped Cobalto-cobaltic oxide material of gained of the present invention have the highest specific capacity and
Well cyclical stability.
Embodiment 3
A kind of flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade, method as follows is prepared from:
(1) 450mg cobaltous acetate is joined in 30ml deionized water, with the most ultrasonic 25min of the power of 400w,
Obtain homodisperse cobalt acetate solution, then with the hydrofluoric acid solution of 1.0mol/L by saline solution pH obtained above
Value is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 75mg ammonia spirit, move into after mix homogeneously in hydrothermal reaction kettle,
After the baking box of 130 DEG C reacts 14h, naturally cool to room temperature and obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged under the conditions of 8000r/min, then uses deionized water and dehydrated alcohol repeatedly
Washing to effluent pH is 7, is finally dried 10h under the conditions of 80 DEG C and obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder presoma is risen to 820 DEG C with the programming rate of 8 DEG C/min, at air bar
After carrying out calcination processing 3h under part, naturally cool to room temperature and i.e. can get the Cobalto-cobaltic oxide flower of nano level three-dimensional
Spheroidal material；
Use the S-3400N ultramicroscope (Hitachi) surface texture to the Cobalto-cobaltic oxide material of above-described embodiment 3 gained
Be scanned, the scanning electron microscope (SEM) photograph of gained as shown in Figure 6, from fig. 6 it can be seen that the three-dimensional flower ball-shaped four of gained aoxidizes
Three cobalt materials are made up of many nano-scale particles, and particle diameter is about 400nm.
Use blue electricity battery test system (LAND 2001A system), at ambient temperature, select three-electrode system, with
6M KOH aqueous solution is electrolyte, and electrochemical window is set to the 0-0.4V three-dimensional Cobalto-cobaltic oxide material to above-described embodiment 3 gained
Capacitor chemical property and stability test, specific capacity must be beaten under the charging and discharging currents density of 1A/g and be about
627F/g, and after circulation 1000 circle, still there is higher specific capacity 592F/g.
Embodiment 4
A kind of flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade, method as follows is prepared from:
(1) 600mg cobaltous acetate is joined in 30ml deionized water, with the most ultrasonic 30min of the power of 400w,
Obtain homodisperse cobalt acetate solution, then with the citric acid solution of 1.0mol/L by saline solution pH obtained above
Value is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 60mg ammonia spirit (25wt%-28wt%), move into after mix homogeneously
In hydrothermal reaction kettle, after reacting 16h in the baking box of 140 DEG C, naturally cool to room temperature and obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged under the conditions of 8000r/min, then uses deionized water and dehydrated alcohol repeatedly
Washing to effluent pH is 7, is finally dried 12h under the conditions of 80 DEG C and obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder presoma is risen to 800 DEG C with the programming rate of 8 DEG C/min, at air bar
After carrying out calcination processing 3h under part, naturally cool to room temperature and i.e. can get the Cobalto-cobaltic oxide flower of nano level three-dimensional
Spheroidal material；
In sum, the flower ball-shaped Cobalto-cobaltic oxide material of a kind of three-dimensional nanometer-grade that the present invention provides, it has three-dimensional appearance,
There is the degree of crystallinity that hierarchy is become reconciled, and specific capacity is up to 679F/g, there is circulation and high rate performance, the Ke Yiyong of brilliance
Make ultracapacitor.
The above is only the citing of embodiments of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement, these improvement also should be regarded as this
Bright protection domain.
Claims (7)
1. the preparation method of the flower ball-shaped Cobalto-cobaltic oxide material of a three-dimensional nanometer-grade, it is characterised in that specifically comprise the following steps that
(1) it is 5:1-20:1mg/ml according to mass volume ratio, cobaltous acetate is joined ultrasonic 15-30min in deionized water,
To homodisperse cobalt acetate solution, then it is added thereto to weak acid, the pH value of solution is adjusted to 6.0-6.5；
(2) in the solution that step (1) obtains, add 25wt%-28wt% ammonia spirit, after mix homogeneously, move into hydro-thermal reaction
In still, react at a temperature of 100-140 DEG C, after reaction terminates, naturally cool to room temperature and obtain reactant liquor；
(3) step (2) gained reactant liquor is centrifuged, collects precipitation；Then by deionized water and absolute ethanol washing precipitation
PH value to effluent is neutrality, obtains cobalt hydroxide powder；
(4) step (3) gained cobalt hydroxide powder is risen to 800-850 DEG C with the programming rate of 5-8 DEG C/min, at air bar
Calcine 2-3h under part, naturally cool to room temperature afterwards, i.e. obtain the flower ball-shaped Cobalto-cobaltic oxide material of three-dimensional nanometer-grade.
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), described weak acid is citric acid, acetic acid
Or in Fluohydric acid. any one.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), described 25wt%-28wt% ammonia is molten
The mass ratio of liquid and cobaltous 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), baking temperature is 60-80 DEG C, is dried
Time is 10-12h.
7. the preparation method as described in one of claim 1-6, it is characterised in that the three-dimensional Cobalto-cobaltic oxide material of gained is bouquet
Shape pattern, a diameter of 8-15 μm of flower ball-shaped Cobalto-cobaltic oxide, it is made up of the nano-particle that particle diameter is 400-600nm.
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| CN106219615A (en) * | 2016-08-23 | 2016-12-14 | 肖洋 | The preparation method of flower-shaped cobalt hydroxide microsphere |
| 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 |
| CN106450254A (en) * | 2016-11-03 | 2017-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing Ni and Sb co-doped cobaltosic oxide nano oxide |
| CN107162066A (en) * | 2017-05-26 | 2017-09-15 | 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 |
| 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 |
| CN110182854A (en) * | 2019-06-10 | 2019-08-30 | 中国科学院青岛生物能源与过程研究所 | One type sea urchin shape cobalt oxide photothermal conversion film and its preparation method and application |
| 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 |
| CN110683589A (en) * | 2019-10-17 | 2020-01-14 | 宁波大学 | Preparation method of cobaltosic oxide nano material |
| 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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