CN109273727A - A kind of nano flower array flexible air electrode material and preparation method thereof, application - Google Patents
A kind of nano flower array flexible air electrode material and preparation method thereof, application Download PDFInfo
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- CN109273727A CN109273727A CN201810979115.8A CN201810979115A CN109273727A CN 109273727 A CN109273727 A CN 109273727A CN 201810979115 A CN201810979115 A CN 201810979115A CN 109273727 A CN109273727 A CN 109273727A
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8846—Impregnation
- H01M4/885—Impregnation followed by reduction of the catalyst salt precursor
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- H01M4/90—Selection of catalytic material
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Abstract
A kind of nano flower array flexible air electrode material and preparation method thereof, application, are related to electrode material field.A kind of preparation method of nano flower array flexible air electrode material, it include: that nickel acetate, cobalt acetate and vulcanized sodium are add to deionized water stirring to form homogeneous mixture solotion, mixed solution and carbon cloth are subjected to hydro-thermal reaction again, product is taken out after being cooled to room temperature after reaction, obtaining growth has CoNi2S4The CP of nano flower array.The electrode material has the characteristics that flexible and self-supporting, and can improve Li-O2The cycle performance and high rate performance of battery.
Description
Technical field
The present invention relates to electrode material fields, and in particular to a kind of nano flower array flexible air electrode material and its system
Preparation Method, application.
Background technique
In recent years, flexible electronic devices are becoming increasingly popular, because they can be bent to a certain extent, are distorted, rolling
Dynamic or stretching, but still keep its function.Lithium ion battery (English abbreviation LIB) is considered as the head in flexible power supply recently
Choosing, but the low theoretical energy density of commercial lithium-ion batteries substantially limits them in next-generation flexible device at present
Using.Fortunately, chargeable lithium-oxygen (Li-O2) battery is due to high (the about 3600Whkg of its theoretical energy density-1),
As one of most promising electrochemical energy storage technology.Although developing a kind of flexible Li-O2Battery theoretically can satisfy soft
Urgent need of the property device to high energy density cells, but the technology is still in its infancy, also deposits before putting into practical application
In problems.
To solve the above-mentioned problems, developing suitable catalyst is the key link for realizing Li-O2 battery practical application.One
Aspect, high performance catalyst can accelerate to improve the dynamics of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER), reduce simultaneously
Li-O2The overpotential of battery, on the other hand, active catalyst can effectively catalyze formation/decomposition of solid discharge product, this
Li-O will be improved2The cycle performance and high rate performance of battery.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of nano flower array flexible air electrode material, the system
Growth, which can be prepared, in Preparation Method CoNi2S4The carbon cloth of nano flower array.
The second object of the present invention is to provide a kind of nano flower array flexible air electrode material, which has
The characteristics of flexible and self-supporting, and Li-O can be improved2The cycle performance and high rate performance of battery.
The third object of the present invention is to provide a kind of application of nano flower array flexible air electrode material, can apply
In flexible and wearable power supply.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of nano flower array flexible air electrode material, comprising:
Nickel acetate, cobalt acetate and vulcanized sodium are add to deionized water stirring and form homogeneous mixture solotion, then will mixing
Solution and carbon cloth carry out hydro-thermal reaction, and product is taken out after being cooled to room temperature after reaction, and obtaining growth has CoNi2S4Nano flower
The CP of array.
A kind of nano flower array flexible air electrode material, by above-mentioned nano flower array flexible air electrode material
Preparation method is made.
A kind of application such as above-mentioned nano flower array flexible air electrode material in flexible and wearable power supply.
The beneficial effect of the embodiment of the present invention is:
Growth, which can be prepared, in the preparation method of the nano flower array flexible air electrode material of the application CoNi2S4
The carbon cloth of nano flower array, for carbon cloth as collector, its own has flexibility, then the nano flower array flexible air being prepared
Electrode material also has the characteristics that flexibility, porous structure are also storage Li2O2Provide more memory spaces.
Nano flower array flexible air electrode material contains CoNi2S4Nano flower array belongs to binary metal sulfide,
Its catalytic activity is better than unitary metal sulfide.In addition, CoNi2S4Shape characteristic be nano flower array structure, which has
Biggish specific surface area, active site are more, it is thus possible to increase its catalytic activity.In addition, carbon cloth has excellent electrical conductance,
Then growth has CoNi2S4The carbon cloth of nano flower array not only has excellent electro catalytic activity, and can improve the electronics conduction of itself
Property, so as to improve discharge capacity, high rate performance and the cyclical stability of battery.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the SEM figure that the nano flower array flexible air electrode material that the embodiment of the present invention 1 provides amplifies 15000 times；
Fig. 2 is the SEM that the nano flower array flexible air electrode material that the embodiment of the present invention 1 provides amplifies 200000 times
Figure；
Fig. 3 is the BET figure for the nano flower array flexible air electrode material that the embodiment of the present invention 1 provides；
Fig. 4 is the XRD diagram for the nano flower array flexible air electrode material that the embodiment of the present invention 1 provides；
Fig. 5 is the nano flower array flexible air electrode material that provides of the embodiment of the present invention 1 as lithium air electrode material
First charge-discharge test chart；
Fig. 6 is the nano flower array flexible air electrode material that provides of the embodiment of the present invention 1 as lithium air electrode material
High rate performance test chart；
Fig. 7 is the nano flower array flexible air electrode material that provides of the embodiment of the present invention 1 as lithium air electrode material
Cycle performance test chart.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to a kind of preparation method of nano flower array flexible air electrode material of the embodiment of the present invention, using progress
It illustrates.
In recent years, metal sulfide is including evolving hydrogen reaction due to its excellent thermal stability and high electro catalytic activity
(HER), it is explored in the various applications including carbon dioxide conversion and ORR.However, their low electric conductivity limits its electrification
Learn performance.
A kind of preparation method of nano flower array flexible air electrode material, comprising:
Nickel acetate, cobalt acetate and vulcanized sodium and deionized water are mixed to form mixed solution, by mixed solution and carbon cloth into
Row hydro-thermal reaction, obtaining growth has CoNi2S4The carbon cloth of nano flower array.
Wherein, the English abbreviation of carbon cloth is CP, and growth has CoNi2S4The carbon cloth f-CoNi of nano flower array2S4/ CP table
Show.
Nickel acetate, cobalt acetate and vulcanized sodium form mixed solution after mixing with deionized water, in the present embodiment, pass through
The mode of stirring enables to each component in mixed solution evenly dispersed.When carrying out hydro-thermal reaction, nickel acetate, cobalt acetate and sulphur
Change sodium reacts and can generate CoNi2S4Nano flower array, CoNi2S4Nano flower array is as active catalytic material, due to carbon
Cloth has porous structure, reacts the CoNi of generation2S4Then it is attached on carbon cloth.For carbon cloth as collector, its own has flexibility,
The nano flower array flexible air electrode material being then prepared also has the characteristics that flexible and is easy to restore, porous structure
It also is storage Li2O2Provide more memory spaces.
Traditional cathode is to be coated active catalyst on the current collector using polymer, may generate some pairs in this way
Product.The CoNi of present embodiment2S4Nano flower array is grown on carbon cloth, avoids and occurs because using polymer
Lead to the problem of by-product.
The nano flower array flexible air electrode material of present embodiment contains CoNi2S4Nano flower array, belongs to binary
Metal sulfide, catalytic activity are better than unitary metal sulfide.In addition, CoNi2S4Shape characteristic be nano flower array junctions
Structure, the structure have biggish specific surface area, and active site is more, it is thus possible to increase its catalytic activity.In addition, carbon cloth has
Excellent electrical conductance, then f-CoNi2S4/ CP not only has excellent electro catalytic activity, and can improve the electronic conductivity of itself.
In some embodiments, the molar ratio of nickel acetate, cobalt acetate and vulcanized sodium is 2:1:8~12.The second of the ratio
Sour nickel, cobalt acetate and vulcanized sodium reaction, wherein vulcanized sodium is just appropriate or excessive, can react to obtain purer
CoNi2S4, after the completion of reaction, whole system is cooled to room temperature, taking out growth has CoNi2S4The carbon cloth of nano flower array, benefit
It is cleaned by ultrasonic repeatedly with ethyl alcohol and deionized water, the vulcanized sodium for not participating in reaction can be washed away.
In the present embodiment, the temperature of hydro-thermal reaction is 180~200 DEG C, and the time of hydro-thermal reaction is 12~12.5h.
A kind of nano flower array flexible air electrode material, is made by above-mentioned preparation method.Nano flower array flexible
Main group of air electrode material becomes f-CoNi2S4/ CP after tested, has good electrification as a kind of cathode material
Learn performance, including high discharge capacity, good high rate performance and cyclical stability.
f-CoNi2S4/ CP cathode has flexibility, it is shown that its potential application in flexible and wearable power supply.This is received
Popped rice array flexible air electrode material applicable property and wearable power supply.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
1) carbon cloth pre-processes:
Carbon cloth is successively used to acetone, ethyl alcohol and deionized water ultrasonic cleaning 30min, dried for standby.
2)f-CoNi2S4The synthesis of/CP: 2mmol nickel acetate, 1mmol cobalt acetate and 8mmol vulcanized sodium are added to 60ml
1h is stirred in deionized water and forms mixed solution, and mixed solution and carbon cloth (CP) are then transferred to the autoclave of 100ml
In, in 180 DEG C of reaction 12h.After hydro-thermal reaction, it is cooled to room temperature taking-up carbon cloth in temperature, and handed over ethyl alcohol and deionized water
For washing 5 times after be dried, finally obtain growth has CoNi2S4Carbon cloth (the i.e. f-CoNi of nano flower array2S4/CP)。
Embodiment 2
1) carbon cloth pre-processes:
Carbon cloth is successively used to acetone, ethyl alcohol and deionized water ultrasonic cleaning 30min, dried for standby.
2)f-CoNi2S4The synthesis of/CP: 2mmol nickel acetate, 1mmol cobalt acetate and 8mmol vulcanized sodium are added to 60ml
1h is stirred in deionized water and forms mixed solution, and mixed solution and carbon cloth (CP) are then transferred to the autoclave of 100ml
In, in 200 DEG C of reaction 12.5h.After hydro-thermal reaction, taking-up carbon cloth is cooled to room temperature in temperature, and with ethyl alcohol and deionized water
It is dried after alternately washing 4 times, finally obtaining growth has CoNi2S4Carbon cloth (the i.e. f-CoNi of nano flower array2S4/CP)。
Embodiment 3
1) carbon cloth pre-processes:
Carbon cloth is successively used to acetone, ethyl alcohol and deionized water ultrasonic cleaning 30min, dried for standby.
2)f-CoNi2S4The synthesis of/CP: 2mmol nickel acetate, 1mmol cobalt acetate and 10mmol vulcanized sodium are added to 60ml
45min is stirred in deionized water and forms mixed solution, and mixed solution and carbon cloth (CP) are then transferred to the reaction under high pressure of 100ml
In kettle, in 190 DEG C of reaction 12h.After hydro-thermal reaction, taking-up carbon cloth is cooled to room temperature in temperature, and with ethyl alcohol and deionized water
It is dried after alternately washing 4 times, finally obtaining growth has CoNi2S4Carbon cloth (the i.e. f-CoNi of nano flower array2S4/CP)。
Embodiment 4
1) carbon cloth pre-processes:
Carbon cloth is successively used to acetone, ethyl alcohol and deionized water ultrasonic cleaning 30min, dried for standby.
2)f-CoNi2S4The synthesis of/CP: 2mmol nickel acetate, 1mmol cobalt acetate and 12mmol vulcanized sodium are added to 60ml
50min is stirred in deionized water and forms mixed solution, and mixed solution and carbon cloth (CP) are then transferred to the reaction under high pressure of 100ml
In kettle, in 190 DEG C of reaction 12h.After hydro-thermal reaction, taking-up carbon cloth is cooled to room temperature in temperature, and with ethyl alcohol and deionized water
It is dried after alternately washing 5 times, finally obtaining growth has CoNi2S4Carbon cloth (the i.e. f-CoNi of nano flower array2S4/CP)。
Test example
(1) f-CoNi that embodiment 1 is prepared2S4/ CP is observed under electronic scanner microscope, and SEM test chart is such as
Shown in Fig. 1 and Fig. 2.
Interpretation of result: it can be seen that f-CoNi from Fig. 1 and Fig. 22S4CoNi in/CP2S4Pattern be nano flower array junctions
Structure, CoNi2S4It is attached on carbon cloth.
(2) f-CoNi that embodiment 1 is prepared2S4/ CP carries out specific surface area test, BET test chart such as Fig. 3 institute
Show.
Interpretation of result: it can be seen that the f-CoNi that embodiment 1 is prepared from the result of Fig. 32S4/ CP specific surface area reaches
18.418m2/ g has biggish specific surface area.
(3) f-CoNi that embodiment 1 is prepared2S4/ CP carries out X-ray diffraction test, XRD test chart such as Fig. 4 institute
Show.
Interpretation of result: can be seen that the product that hydro-thermal reaction generates from the result of Fig. 4 is CoNi2S4。
(4) by the f-CoNi with embodiment 12S4The Li-O of/CP cathode2Battery carries out charge-discharge test, for the first time charge and discharge
Electrical measurement attempts as shown in Figure 5.
Interpretation of result: it can be seen that the f-CoNi with embodiment 1 from the result of Fig. 52S4The Li-O of/CP cathode2Battery
Under the current density of 200mA/g, it is capable of providing the high discharge capacity of about 7850mAh/g.
(5) to the f-CoNi with embodiment 12S4The Li-O of/CP cathode2Battery is tested under different current densities respectively
Its high rate performance, test results are shown in figure 6.
Interpretation of result: from fig. 6, it can be seen that when current density is restored to initial current density, blanking voltage does not almost have
There is decaying, shows containing f-CoNi2S4The Li-O of/CP cathode2Battery has good times of forthright and restorability.
(6) test has the f-CoNi of embodiment 12S4The Li-O of/CP cathode2The cycle performance of battery, test result is such as
Shown in Fig. 7.
Interpretation of result: the f-CoNi with embodiment 12S4The Li-O2 battery of/CP cathode is under the current density of 500mA/g
Stablize and Reversible Cycle 100 times, and without apparent voltage change, cycle performance is good.
In conclusion the preparation method of the nano flower array flexible air electrode material of the embodiment of the present invention can be prepared
Obtaining growth has CoNi2S4The carbon cloth of nano flower array, f-CoNi2S4/ CP has flexibility, can be storage Li2O2It provides more
More memory spaces.f-CoNi2S4/ CP not only has excellent electro catalytic activity, and can improve the electronic conductivity of itself, from
And it can be improved discharge capacity, high rate performance and the cyclical stability of battery.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nano flower array flexible air electrode material characterized by comprising
Nickel acetate, cobalt acetate and vulcanized sodium are add to deionized water stirring and form homogeneous mixture solotion, then by mixed solution
Hydro-thermal reaction is carried out with carbon cloth, product is taken out after being cooled to room temperature after reaction, obtaining growth has CoNi2S4Nano flower array
CP.
2. the preparation method of nano flower array flexible air electrode material according to claim 1, which is characterized in that described
The temperature of hydro-thermal reaction is 180~200 DEG C.
3. the preparation method of nano flower array flexible air electrode material according to claim 1 or 2, which is characterized in that
The time of the hydro-thermal reaction is 12~12.5h.
4. the preparation method of nano flower array flexible air electrode material according to claim 3, which is characterized in that described
The molar ratio of nickel acetate, cobalt acetate and vulcanized sodium is 2:1:8~12.
5. the preparation method of nano flower array flexible air electrode material according to claim 1, which is characterized in that take out
After product, there is the CoNi to growth2S4The carbon cloth of nano flower array successively uses ethyl alcohol and deionized water to be cleaned by ultrasonic.
6. a kind of preparation method of nano flower array flexible air electrode material characterized by comprising
Nickel acetate, cobalt acetate and vulcanized sodium and deionized water are mixed to form mixed solution, by the mixed solution and carbon cloth into
Row hydro-thermal reaction, obtaining growth has CoNi2S4The carbon cloth of nano flower array.
7. the preparation method of nano flower array flexible air electrode material according to claim 6, which is characterized in that described
The temperature of hydro-thermal reaction is 180~200 DEG C.
8. the preparation method of nano flower array flexible air electrode material according to claim 6, which is characterized in that described
The molar ratio of nickel acetate, cobalt acetate and vulcanized sodium is 2:1:8~12.
9. a kind of nano flower array flexible air electrode material, which is characterized in that it is received by claim 1-8 is described in any item
The preparation method of popped rice array flexible air electrode material is made.
10. a kind of nano flower array flexible air electrode material as claimed in claim 9 is in flexible and wearable power supply
Using.
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| CN110137511A (en) * | 2019-05-10 | 2019-08-16 | 深圳大学 | Y-oxides doping lithium air battery positive electrode and preparation method thereof and lithium-air battery |
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| CN109621981B (en) * | 2018-10-31 | 2022-04-15 | 中山大学 | Metal oxide-sulfide composite oxygen evolution electrocatalyst and preparation method and application thereof |
| CN114371202B (en) * | 2020-10-14 | 2023-05-02 | 东华大学 | Carbon fiber composite material and preparation method and application thereof |
| CN112551585A (en) * | 2020-12-24 | 2021-03-26 | 齐鲁工业大学 | Surfactant-induced MoS2Preparation method and application of nanoflower electrode material |
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| CN106732649A (en) * | 2017-02-20 | 2017-05-31 | 天津理工大学 | A kind of preparation method of alkaline oxygen evolution reaction elctro-catalyst |
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| CN106732649A (en) * | 2017-02-20 | 2017-05-31 | 天津理工大学 | A kind of preparation method of alkaline oxygen evolution reaction elctro-catalyst |
| CN107492657A (en) * | 2017-07-12 | 2017-12-19 | 三峡大学 | A kind of preparation method of cobalt sulfide nickel both positive and negative polarity battery and its application on the recyclable battery of alkalescence |
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| CN110137511A (en) * | 2019-05-10 | 2019-08-16 | 深圳大学 | Y-oxides doping lithium air battery positive electrode and preparation method thereof and lithium-air battery |
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Application publication date: 20190125 |