CN110112391A - Spherical carbon coating cobaltosic oxide composite material and its preparation method and application - Google Patents
Spherical carbon coating cobaltosic oxide composite material and its preparation method and application Download PDFInfo
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- CN110112391A CN110112391A CN201910390186.9A CN201910390186A CN110112391A CN 110112391 A CN110112391 A CN 110112391A CN 201910390186 A CN201910390186 A CN 201910390186A CN 110112391 A CN110112391 A CN 110112391A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a kind of spherical carbon coating cobaltosic oxide composite materials and its preparation method and application, it should be the preparation method comprises the following steps: then solid powder be washed, is dried by being heat-treated under air atmosphere after precursor solution ultrasonic atomizatio to obtain solid powder, is calcined under atmosphere of inert gases spherical carbon coating cobaltosic oxide composite material is made；Wherein, precursor solution contains cobalt source, glucose and solvent；The temperature of heat treatment is 380-480 DEG C, and the temperature of calcining is 350-500 DEG C.The spherical carbon coating cobaltosic oxide composite material has excellent specific capacity and then use can be applied in lithium ion battery, while the preparation method has the characteristics that easy to operate, process is simple and low for equipment requirements.
Description
Technical field
The present invention relates to cobaltosic oxide composite materials, and in particular, to a kind of spherical carbon coating cobaltosic oxide is compound
Material and its preparation method and application.
Background technique
As the device for converting chemical energy to electric energy, battery has been widely used in daily life and production.Wherein, lithium
Ion battery due to its higher operating voltage, have extended cycle life, the highly-safe and advantages such as environmental-friendly have become perhaps
One of the important equipment of energy storage is used in multi-field.Currently, commercial li-ion battery more depends on the research of anode material.
Carbon material is always the emphasis that scientist studies anode material due to cheap, high conductivity and chemical stability.But
Their practical application is due to its low theoretical specific capacity (372mAhg-1) and lower initial coulombic efficiency and be obstructed.
Simultaneously with cobaltosic oxide (890mAhg-1) received more and more for the height ratio capacity 3d transition metal oxide of representative
Concern, however, these transition metal oxides still have inevitable defect: will appear volume effect in charge and discharge process
It answers, circulation stability is poor.
The Chinese patent application of Publication No. CN108695507A discloses a kind of porous cobaltosic oxide nano of carbon coating
The preparation method and applications of particle, product obtained have high-intensitive nanostructure and slow down volume expansion problem, institute
It obtains material and is widely used in lithium ion battery negative material aspect.However, the product charge/discharge capacity that this method obtains is relatively low.
Summary of the invention
The object of the present invention is to provide a kind of spherical carbon coating cobaltosic oxide composite material and its preparation method and application,
The spherical carbon coating cobaltosic oxide composite material has excellent specific capacity and then use can be applied in lithium ion battery,
The preparation method has the characteristics that easy to operate, process is simple and low for equipment requirements simultaneously.
To achieve the goals above, the present invention provides a kind of preparation sides of spherical carbon coating cobaltosic oxide composite material
Method, should be the preparation method comprises the following steps: connect by being heat-treated after precursor solution ultrasonic atomizatio under air atmosphere to obtain solid powder
Solid powder is washed, is dried, is calcined under atmosphere of inert gases spherical carbon coating cobaltosic oxide is made
Composite material；
Wherein, precursor solution contains cobalt source, glucose and solvent；The temperature of heat treatment is 380-480 DEG C, the temperature of calcining
Degree is 350-500 DEG C.
The present invention also provides a kind of spherical carbon coating cobaltosic oxide composite material, the spherical carbon coating cobaltosic oxides
Composite material is prepared by above-mentioned preparation method.
Invention further provides a kind of if above-mentioned spherical carbon coating cobaltosic oxide composite material is in lithium battery
Application.
In the above-mentioned technical solutions, cobaltosic oxide is made by the step of ultrasonic atomizatio, heat treatment and calcining in the present invention
And carbon composite, which has hollow graded porous structure, and (ball wall thickness can be not necessarily between 3-100nm from master regulation
Subsequent screening), not only there is higher mechanical performance, while being conducive to the infiltration and diffusion of electrolyte, convenient for the transmission of lithium ion；
So that material specific capacity with higher, in 0.2Ag-1Lower capacity is up to 1100mAhg-1(it is much higher than Co3O4
(890mAh·g-1) and carbon (372mAhg-1) theoretical capacity).The preparation method reaction time is short, yield is high simultaneously, to setting
It is standby require it is low, production can be met without pre-burning, common high temperature process furnances so that this method is with before being widely popularized
Scape.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 a is the SEM figure of product M1 obtained in embodiment 1；
Fig. 1 b is the SEM figure of product M2 obtained in embodiment 2；
Fig. 1 c is the SEM figure of product M3 obtained in embodiment 3；
Fig. 1 d is the SEM figure of product M4 obtained in embodiment 4；
Fig. 1 e is the SEM figure of product D1 obtained in comparative example 1；
Fig. 1 f is the SEM figure of product D2 obtained in comparative example 2；
Fig. 1 g is the SEM figure of product D3 obtained in comparative example 3；
Fig. 1 h is the SEM figure of product D4 obtained in comparative example 4；
Fig. 2 is the XRD spectrum of product M1 obtained in embodiment 1.
Fig. 3 is the cycle performance figure of product M1 obtained in embodiment 1.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of preparation method of spherical carbon coating cobaltosic oxide composite material, should the preparation method comprises the following steps:
To be heat-treated under air atmosphere after precursor solution ultrasonic atomizatio (in order to be pyrolyzed glucose for small organic molecule) with
Solid powder is obtained, then solid powder is washed, is dried, is calcined under atmosphere of inert gases Spherical Carbon is made
Coat cobaltosic oxide composite material；
Wherein, precursor solution contains cobalt source, glucose and solvent；The temperature of heat treatment is 380-480 DEG C, the temperature of calcining
Degree is 350-500 DEG C.
In the above preparation method, the dosage of each material can select in a wide range, but in order to further control
The ball wall thickness of carbon coating cobaltosic oxide composite material, pattern are to improve the chemical property of material, it is preferable that cobalt source, Portugal
The amount ratio of grape sugar and solvent is 1.5mmol:1.5-2.5mmol:15-30mL.
In the above preparation method, the specific type of cobalt source can select in a wide range, but in order in view of at
This, it is preferable that cobalt source is selected from least one of cobalt nitrate, cobalt acetate, acetylacetone cobalt；Solvent is water.
In the above-described embodiment, the concrete mode of heat treatment can select in a wide range, but in order to further
The stability of the hollow structure of carbon coating cobaltosic oxide composite material obtained and the OK range of specific surface area are controlled, it is excellent
Selection of land, heat treatment are as follows: handle the aerosol after atomization by tube furnace；On the basis of 20mL precursor solution, atomization
The time that aerosol afterwards passes through tube furnace is 5-10s.
In the above-described embodiment, the time of calcining can select in a wide range, but in order to further control system
The stability of the hollow structure of the carbon coating cobaltosic oxide composite material obtained and the OK range of specific surface area, it is preferable that
The time of calcining is 1.5-2.5h.
On the basis of the above embodiment, it is preferable that before being calcined, which further includes heating process: will
Desciccate is warming up to 350-900 DEG C from the 15-35 DEG C of rate with 1.8-2.5 DEG C/min.
In the present invention, the specific steps of washing can select in a wide range, but in order to enable in solid powder
Impurity clean it is more thorough, it is preferable that washing are as follows: water and dehydrated alcohol is successively respectively adopted and washs 2-5 times.
In the present invention, dry condition can select in a wide range, but in order to further increase drying effect,
Preferably, drying meets the following conditions: drying temperature is 50-80 DEG C, drying time 48-72h.
The present invention also provides a kind of spherical carbon coating cobaltosic oxide composite material, the spherical carbon coating cobaltosic oxides
Composite material is prepared by above-mentioned preparation method；
In the present invention, the morphology and size of spherical carbon coating cobaltosic oxide composite material can be selected in a wide range
It selects, but in order to further increase the chemical property of spherical carbon coating cobaltosic oxide composite material, it is preferable that Spherical Carbon packet
The hollow ball that cobaltosic oxide composite material is wall thickness 3-100nm is covered, the diameter of sphere is 0.5-1.0 μm.
Invention further provides a kind of if above-mentioned spherical carbon coating cobaltosic oxide composite material is in lithium battery
Application.
The present invention will be described in detail by way of examples below.The preparation of lithium battery: firstly, by spherical carbon coating four
Co 3 O composite material, conductive black (super-P-Li) and polyvinylidene fluoride (PVDF) are stirred according to mass ratio 7:2:1；
It is subsequently added into solvent NMP at the uniform velocity to stir 6 hours, then be coated in slurry on clean painting carbon copper foil, dry, compacting is made thin
Piece；Finally using thin slice as working electrode, lithium piece is used as to electrode assembling into 2023 type button cells, and assembling process is being full of argon
(H in the glove box of gas2O content is less than 1ppm, O2Content is less than 8ppm).
SEM detection is obtained by the detection of Hitachi's S-4800 scanning electron microscope；XRD detection is to pass through D8AdvanceX
Ray powder diffractometer is detected and is obtained；Lithium battery performance detection is obtained by the detection of Neware CT-3008 lithium electrical testing frame.
Embodiment 1
1) 0.2973g (1.5mmol) glucose is dissolved in 20ml deionized water, stirring forms the solution of homogeneous transparent
A；
2) 0.6615g (2.25mmol) cabaltous nitrate hexahydrate is added in above-mentioned solution A and is stirred to forming uniform forerunner
Liquid solution B；
3) above-mentioned precursor solution B is placed in atomizer and is atomized, coutroi velocity is by tube furnace (air atmosphere, control
Temperature is maintained at 380 DEG C, all by passing through 5-10s) obtain powder；
It is 4) powder being collected into is dry after water and dehydrated alcohol wash 3 times respectively that (drying temperature is 70 DEG C, when dry
Between be 60h) obtain solid powder；
5) solid powder being collected into is warming up to 350 DEG C from 15 DEG C of rates with 2 DEG C/min in nitrogen atmosphere and protected
Temperature calcining 2h obtains product M1.The SEM figure of product M1 is as shown in Figure 1a；The XRD spectrum of product M1 is as shown in Figure 2；Product M1's
Lithium battery performance map is as shown in figure 3, in 0.2Ag-1Lower capacity is up to 1297.074mAhg-1。
Embodiment 2
Product M2 is obtained according to the preparation method of embodiment 1, unlike, the weight of cabaltous nitrate hexahydrate is added in step 2)
Amount is 0.4410g, and the SEM figure of product M2 is as shown in Figure 1 b, in 0.2Ag-1Lower capacity is up to 1100mAhg-1。
Embodiment 3
Product M3 is obtained according to the preparation method of embodiment 1, unlike, the temperature of tube furnace is 480 DEG C in step 3),
The SEM of product M3 schemes as illustrated in figure 1 c, in 0.2Ag-1Lower capacity is up to 950mAhg-1。
Embodiment 4
Product M4 is obtained according to the preparation method of embodiment 1, unlike, final calcination temperature is 500 DEG C in step 4),
The SEM figure of product M4 is as shown in Figure 1 d, in 0.2Ag-1Lower capacity is up to 1000mAhg-1。
Comparative example 1
Product D1 is made according to the preparation method of embodiment 1, unlike, glucose is replaced with etc. to the lemon of weight
Acid, the SEM figure of product D1 is as shown in fig. le.
Comparative example 2
Product D2 is made according to the preparation method of embodiment 1, unlike, glucose is replaced with etc. to the PVP of weight, is produced
The SEM figure of object D2 is as shown in Figure 1 f.
Comparative example 3
Product D3 is made according to the preparation method of embodiment 1, unlike, glucose is replaced with etc. to the P123 of weight
The SEM figure of (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer), product D3 is as shown in Figure 1 g.
Comparative example 4
Product D4 is made according to the preparation method of embodiment 1, unlike, cabaltous nitrate hexahydrate is replaced with into equimolar amounts
Acetylacetone cobalt, product D4 SEM figure as shown in figure 1h.
From SEM figure shown in Fig. 1 a and 1b, it can be seen that add the content of cobalt nitrate to spherical carbon coating Co3O4Electrode
The wall thickness of material produces influence, and by increasing the content of the cobalt nitrate in precursor solution, the ball wall of nanosphere is by the left side 100nm
The right side is reduced into 30nm or so, and thinning trend occurs in ball wall.Ball wall to a certain extent to the mechanical stability of sample and lithium from
It is impacted on sub-transmission path, further influences performance of lithium ion battery.
From Fig. 1 c and 1d figure as can be seen that spray pyrolysis temperature and later period calcination temperature it is different to having on sample topography
Significant impact, the raising of pyrolysis temperature can be greatly promoted the reduction of ball wall wall thickness, form a kind of thick ultra-thin of only 3-5nm
Hollow Nano ball material, the structure will also result in the collapsing of pattern, although early period while reducing the path of lithium ion transport
The promotion of capacity to a certain extent is had, but strong influence can be generated to its cyclical stability.On the contrary, improving later period calcining temperature
The sample of degree, nanometer ball surface macropore ingredient is higher, possesses higher stability compared to product obtained by embodiment 3.
The citric acid, PVP and P123 that equivalent is added from Fig. 1 e, 1f and 1g figure as can be seen that under square one are made
Product keeps the pattern of ball substantially, but for the sample shown in the example 1, the smooth nanosphere pattern in surface is on the whole
It changes, it is not full enough, it shows a degree of " shrivelled ".By changing carbon source kind in precursor solution, Ke Yifen
The recess nanosphere of different-shape is not obtained.
From, as can be seen that adding the acetylacetone cobalt of equivalent under square one, structure is most in SEM figure shown in Fig. 1 h
It changes, and shows the pattern of the shuttle-type of cut, be difficult to maintain chondritic of the presently claimed invention.
As can be seen that 1 products therefrom of embodiment matches with the Cubic cobaltosic oxide of standard from Fig. 2 and Fig. 3,
0.2A·g-1Lower capacity is up to 1297.074mAhg-1(it is much higher than Co3O4(890mAh·g-1) and carbon (372mAhg-1)
Theoretical capacity) and show excellent performance of lithium ion battery higher than cobaltosic oxide and carbon.
The product of other embodiments is detected according to identical XRD and lithium battery method for testing performance, testing result
It is consistent substantially with the product of embodiment 1.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of spherical carbon coating cobaltosic oxide composite material, which is characterized in that the preparation method is that: it will
Be heat-treated under air atmosphere after precursor solution ultrasonic atomizatio to obtain solid powder, then by the solid powder into
Row washing, drying are calcined under atmosphere of inert gases the spherical carbon coating cobaltosic oxide composite material is made；
Wherein, the precursor solution contains cobalt source, glucose and solvent；The temperature of the heat treatment is 380-480 DEG C, described
The temperature of calcining is 350-500 DEG C.
2. preparation method according to claim 1, wherein the amount ratio of the cobalt source, glucose and solvent is
1.5mmol:1.5-2.5mmol:15-30mL.
3. preparation method according to claim 1, wherein the cobalt source is in cobalt nitrate, cobalt acetate, acetylacetone cobalt
At least one；The solvent is water.
4. preparation method according to claim 1, wherein the heat treatment are as follows: the aerosol after atomization is passed through tubular type
Furnace is handled；On the basis of precursor solution described in 20mL, the time that the aerosol after atomization passes through tube furnace is 5-10s.
5. preparation method according to claim 1, wherein the time of the calcining is 1.5-2.5h.
6. preparation method according to claim 1, wherein before the calcining, the preparation method further includes heating
Process: desciccate is warming up to 350-500 DEG C from the 15-35 DEG C of rate with 1.8-2.5 DEG C/min.
7. preparation method according to claim 1, wherein the washing are as follows: water is successively respectively adopted and dehydrated alcohol is washed
It washs 2-5 times.
8. preparation method according to claim 1, wherein the drying meets the following conditions: drying temperature 50-80
DEG C, drying time 48-72h.
9. a kind of spherical carbon coating cobaltosic oxide composite material, which is characterized in that the spherical carbon coating cobaltosic oxide is multiple
Condensation material is prepared by preparation method described in any one of claim 1-8；
Preferably, the spherical carbon coating cobaltosic oxide composite material is the hollow ball of wall thickness 3-100nm, the diameter of sphere
It is 0.5-1.0 μm or so.
10. a kind of application of the spherical carbon coating cobaltosic oxide composite material in lithium battery as claimed in claim 9.
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| CN113201751A (en) * | 2021-03-26 | 2021-08-03 | 广州费舍尔人工智能技术有限公司 | Magnesium-cobalt-copper oxide modified nitrogen-doped carbon sphere electrode catalyst |
| CN114899382A (en) * | 2022-06-02 | 2022-08-12 | 安徽师范大学 | N-doped porous carbon double-shell microsphere structure coated Co 3 O 4 Material, preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111740083A (en) * | 2020-06-12 | 2020-10-02 | 新昌县华发机械股份有限公司 | Carbon-coated porous Co3O4Microsphere lithium ion battery cathode material and preparation method thereof |
| CN113201751A (en) * | 2021-03-26 | 2021-08-03 | 广州费舍尔人工智能技术有限公司 | Magnesium-cobalt-copper oxide modified nitrogen-doped carbon sphere electrode catalyst |
| CN114899382A (en) * | 2022-06-02 | 2022-08-12 | 安徽师范大学 | N-doped porous carbon double-shell microsphere structure coated Co 3 O 4 Material, preparation method and application thereof |
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