CN111342038A - High-voltage lithium cobalt oxide composite positive electrode material, preparation method thereof and application of lithium battery - Google Patents
High-voltage lithium cobalt oxide composite positive electrode material, preparation method thereof and application of lithium battery Download PDFInfo
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Abstract
A high-voltage lithium cobalt oxide composite cathode material, a preparation method thereof and application of a lithium battery. The chemical molecular formula of the anode material is aLi1‑xCoO2·bLi4Mn5O121 is more than or equal to a, b is more than or equal to 0, a + b is 1, and x is more than 0. The preparation method comprises the steps of mixing commercially prepared lithium cobaltate with a manganese-containing polymer solution, drying the mixed solution, calcining at high temperature to obtain a heterogeneous composite high-voltage lithium cobaltate positive electrode material, and finally applying the high-voltage lithium cobaltate composite positive electrode material to a lithium battery. The invention realizes the synthesis of the high-voltage lithium cobalt oxide anode material in a simpler way, has simple preparation operation and rich raw material sources, and obviously improves the 4.55V high-voltage cobaltThe cycle, rate capability and safety of lithium oxide in lithium batteries.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries and anode electrode materials thereof, and particularly relates to a preparation method of a high-voltage lithium cobalt oxide composite anode material.
Background
Lithium ion batteries have been widely used in energy storage systems for portable devices, electric vehicles, and smart grids because of their advantages of high energy density, long cycling, small self-discharge, and the like. Lithium cobaltate (LiCoO)2) The lithium ion battery anode material is the first generation of successfully commercialized lithium ion battery anode material, and has incomparable advantages in fields with higher requirements on battery volume, such as 3C product market, due to the extremely high volume energy density. Lithium cobaltate (LiCoO)2) The theoretical specific capacity is 274mAh/g, but the currently commercially available specific capacity is only 140mAh/g, the energy density of lithium cobaltate can be greatly improved by increasing the charging voltage, but the lithium cobaltate can generate irreversible change of the structure under high voltage, so that the problems of cycle and rate performance reduction, potential safety hazard and the like are caused, and the further development and application of the lithium cobaltate are severely restricted.
Element doping and surface coating are effective means for improving high-voltage lithium cobaltate. Chinese patent document CN103490063A discloses that Mn element doping treatment is performed on lithium cobaltate, and surface inert oxide layer treatment is also performed on the surface of lithium cobaltate, so that the performance of high-voltage lithium cobaltate is effectively improved, but the surface inert oxide is not favorable for ion transmission, and can hinder the performance of a lithium ion battery under high magnification. Patent document CN110224123A discloses that the performance of high voltage lithium cobaltate is also improved effectively by using gradient doping of aluminum and nickel as the core and composite oxide containing transition metal as the surface, but the operation is more complicated and the product consistency is problematic.
Disclosure of Invention
The invention aims to solve the problem of poor cycle and rate performance of high-voltage lithium cobaltate, provides a high-voltage lithium cobaltate composite positive electrode material and a preparation method thereof, and is applied to a lithium battery. According to the invention, a spinel surface coating technology is utilized to construct the heterogeneous composite high-voltage lithium cobaltate cathode material, so that surface side reactions can be reduced, the surface and bulk phase structure can be stabilized, charge transmission can be accelerated, the dynamics can be improved, the cycle performance, the rate capability and the safety of the material can be improved, and the method has the characteristics of low cost, simplicity in operation, obvious modification effect, easiness in large-scale production and the like.
The technical scheme of the invention is as follows:
the molecular formula of the high-voltage lithium cobalt oxide composite anode material is aLi1-xCoO2·bLi4Mn5O12，1≥a,b≥0,a+b＝1,x＞0。
The preparation method of the high-voltage lithium cobalt oxide composite positive electrode material comprises the following steps of:
the method comprises the following steps: dissolving a polymer in a (20mL) solvent, adding (3g) commercial non-high-voltage lithium cobaltate after the polymer is fully dissolved, dissolving a manganese soluble salt in the solution after uniformly stirring, then evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven;
step two: and calcining the dried precursor under a certain atmosphere according to a set calcination procedure to obtain the high-voltage lithium cobalt oxide composite positive electrode material.
And the calcining procedure is that the lithium cobaltate is calcined in a tube furnace under the atmosphere of oxygen or air, the calcining temperature is 650-900 ℃, the sintering time is 4-10 h, and then the lithium cobaltate is naturally cooled to the room temperature, so that the heterogeneous composite high-voltage lithium cobaltate cathode material is obtained. The calcination temperature is preferably 850 ℃ and the sintering time is 8 hours.
Further, in the step one, the polymer is at least one of polyvinylpyrrolidone (PVP), Polyacrylonitrile (PAN) and Polystyrene (PS), the solvent is at least one of water, ethanol and N, N-Dimethylformamide (DMF), preferably the polymer is PVP, and the solvent is water.
Further, the mass percentage concentration of the polyvinylpyrrolidone solution in the step one is 5% -15%, preferably 10%.
Further, the manganese soluble salt in the step one is at least one of sulfate, nitrate, acetate and chloride, and the molar ratio of the manganese soluble salt to the lithium cobaltate is 2-8%, preferably 5%.
The invention also provides a lithium battery, and the positive electrode material of the lithium battery comprises the high-voltage lithium cobalt oxide composite positive electrode material.
The invention has the advantages and beneficial effects that:
1. the preparation method is simple, has high compatibility with the existing production equipment, low price of raw materials, easy operation and high compatibility with the existing production equipment, and is suitable for large-scale production.
2. The surface of the prepared material has a spinel/layered heterostructure.
3. The capacity retention rate, rate capability and safety of the material in the application of the lithium battery are obviously improved.
Drawings
Fig. 1 is a schematic view of a preparation process of the heterogeneous composite cathode material provided by the invention.
FIG. 2 is a SEM test chart of example 3.
FIG. 3 is a TEM test chart of example 3.
Fig. 4 is an XRD test pattern of example 3.
FIG. 5 is a Raman test chart of example 3.
Fig. 6 is a graph of the cycling performance of button cells of the materials of example 3 and comparative example.
Detailed Description
For a further understanding of the present invention, reference is made to the following further description taken in conjunction with the accompanying drawings, which are included, however, not to limit the scope of the invention.
Example 1
Preparation of high-voltage lithium cobalt oxide composite positive electrode material with chemical formula of 0.99Li0.96CoO2·0.01Li4Mn5O12The polymer is polyvinylpyrrolidone (PVP), the solvent is water, and the mass percentage concentration is 5%.
The method comprises the following steps: dissolving PVP (polyvinyl pyrrolidone) in 20mL of water according to the mass percentage concentration of 5%, adding 3g of commercial lithium cobaltate after the PVP is fully dissolved, uniformly stirring, dissolving manganese nitrate in the solution according to the molar ratio of the manganese nitrate to the lithium cobaltate of 2%, evaporating solvent water to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) keeping the dried precursor at 800 ℃ in the air atmosphere for 10h, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Example 2
Preparation of high-voltage lithium cobalt oxide composite positive electrode material with chemical formula of 0.9Li0.66CoO2·0.1Li4Mn5O12The polymer is Polyacrylonitrile (PAN), the solvent is N, N-Dimethylformamide (DMF), and the mass percentage concentration is 15%.
The method comprises the following steps: dissolving PAN (Polyacrylonitrile) in 20ml of mixed solution of lithium cobaltate according to the mass percentage concentration of 15%, adding 3g of commercial lithium cobaltate after fully dissolving the PAN, dissolving manganese acetate in the solution according to the molar ratio of manganese acetate to lithium cobaltate of 10% after uniformly stirring, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) preserving the temperature of the dried precursor for 10h at 600 ℃ under an oxygen atmosphere, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Example 3
A high-voltage lithium cobaltate composite positive electrode material with a chemical formula of 0.95Li0.98CoO2·0.05Li4Mn5O12The polymer is polyvinylpyrrolidone (PVP), the solvent is water, and the mass percentage concentration is 10%.
The method comprises the following steps: dissolving PVP (polyvinyl pyrrolidone) in 20mL of water according to the mass percentage concentration of 10%, adding 3g of commercial lithium cobaltate after the PVP is fully dissolved, uniformly stirring, dissolving manganese nitrate in the solution according to the molar ratio of the manganese nitrate to the lithium cobaltate of 5%, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) preserving the temperature of the dried precursor for 8h at 850 ℃ in the air atmosphere, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
The preparation flow of the obtained high-voltage lithium cobaltate composite cathode material is shown in fig. 1, the characterization of a Scanning Electron Microscope (SEM) is shown in fig. 2, the characterization of a Transmission Electron Microscope (TEM) is shown in fig. 3, the characterization of X-ray powder diffraction (XRD) is shown in fig. 4, the characterization of Raman (Raman) is shown in fig. 5, and the electrochemical performance of a lithium battery is shown in fig. 6.
Example 4
Preparation of high-voltage lithium cobalt oxide composite positive electrode material with chemical formula of 0.92Li0.68CoO2·0.08Li4Mn5O12The polymer is polyvinylpyrrolidone (PVP), the solvent is a mixed solution of water and ethanol in a volume ratio of 1:1, and the mass percentage concentration is 5%.
The method comprises the following steps: dissolving PVP (polyvinyl pyrrolidone) in 20mL of mixed solution of water and ethanol according to the mass percentage concentration of 5%, adding 3g of commercial lithium cobaltate after the PVP is fully dissolved, dissolving manganese sulfate in the solution according to the molar ratio of manganese sulfate to lithium cobaltate of 8% after the PVP is uniformly stirred, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at the temperature of 100 ℃;
step two: and (3) preserving the temperature of the dried precursor at 900 ℃ in the air atmosphere for 6h, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Example 5
A high-voltage lithium cobaltate composite positive electrode material with a chemical formula of 0.98Li0.92CoO2·0.02Li4Mn5O12The polymer is Polystyrene (PS), the solvent is N, N-Dimethylformamide (DMF), and the mass percentage concentration is 5%.
The method comprises the following steps: dissolving PS in 20mLDMF according to the mass percentage concentration of 5%, adding 3g of commercial lithium cobaltate after fully dissolving, dissolving manganese acetate in the solution according to the molar ratio of manganese acetate to lithium cobaltate of 2% after uniformly stirring, then evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) keeping the dried precursor at 750 ℃ in the air atmosphere for 4h, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Example 6
A high-voltage lithium cobaltate composite positive electrode material with a chemical formula of 0.98Li0.90CoO2·0.06Li4Mn5O12The polymer is polyvinylpyrrolidone (PVP), the solvent is water, and the mass percentage concentration is 15%.
The method comprises the following steps: dissolving PVP (polyvinyl pyrrolidone) in 20mL of water according to the mass percentage concentration of 15%, adding 3g of commercial lithium cobaltate after the PVP is fully dissolved, uniformly stirring, dissolving manganese chloride in the solution according to the molar ratio of manganese chloride to lithium cobaltate being 6%, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) keeping the temperature of the dried precursor at 650 ℃ in the air atmosphere for 10h, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Example 7
Preparation of high-voltage lithium cobalt oxide composite positive electrode material with chemical formula of 0.96Li0.98CoO2·0.04Li4Mn5O12The polymer is Polyacrylonitrile (PAN), the solvent is N, N-Dimethylformamide (DMF), and the mass percentage concentration is 5%.
The method comprises the following steps: dissolving PAN (Polyacrylonitrile) in 20mL of water according to the mass percentage concentration of 5%, adding 3g of commercial lithium cobaltate after fully dissolving the PAN, uniformly stirring, dissolving manganese chloride in the solution according to the molar ratio of manganese chloride to lithium cobaltate of 4%, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven at 100 ℃;
step two: and (3) keeping the dried precursor at 700 ℃ in the air atmosphere for 8h, and naturally cooling to room temperature to obtain the heterogeneous high-voltage lithium cobalt oxide composite positive electrode material.
Comparative example 1
In order to prove the beneficial effect of the heterostructure on the high-voltage lithium cobalt oxide positive electrode material, the comparative sample is a commercial non-high-voltage lithium cobalt oxide material and is applied to rapid attenuation of the cycle capacity in a high-voltage lithium battery.
The above embodiments are merely illustrative of the principles and embodiments, and are not intended to limit the invention, and any modifications, equivalents, improvements and the like made without departing from the principles of the invention are intended to be included within the scope of the invention.
Claims (8)
1. A high-voltage lithium cobalt oxide composite positive electrode material is characterized in that the chemical formula of the composite positive electrode material is shown as formula (I):
aLi1-xCoO2·bLi4Mn5O12(Ⅰ)；
wherein, 1 is more than or equal to a, b is more than or equal to 0, a + b is 1, and x is more than 0.
2. The preparation method of the high-voltage lithium cobaltate composite positive electrode material according to claim 1, characterized by comprising the following steps of:
the method comprises the following steps: dissolving a polymer in a solvent, adding commercial non-high-voltage lithium cobaltate after the polymer is fully dissolved, uniformly stirring, dissolving manganese soluble salt in the solution, evaporating the solvent to obtain a precursor, and drying the precursor in a drying oven;
step two: and calcining the dried precursor in an atmosphere according to a set calcining program to obtain the high-voltage lithium cobalt oxide composite positive electrode material.
3. The method according to claim 2, wherein the polymer in the step one is at least one of polyvinylpyrrolidone (PVP), Polyacrylonitrile (PAN) and Polystyrene (PS), and the solvent is at least one of water, ethanol and N, N-Dimethylformamide (DMF).
4. The method for preparing a high-voltage lithium cobaltate composite positive electrode material according to claim 2, wherein the polymer in the first step is 5-15% by weight.
5. The method according to claim 2, wherein the soluble manganese salt in step one is at least one of manganese acetate, manganese sulfate, manganese nitrate and manganese chloride.
6. The method for preparing a high-voltage lithium cobaltate composite positive electrode material according to claim 2, wherein the molar ratio of the manganese soluble salt to the lithium cobaltate in the step one is 2-8%.
7. The method for preparing a high-voltage lithium cobaltate composite positive electrode material according to claim 2, wherein the calcination procedure in the second step is to heat the material to 650-900 ℃ in a tube furnace in an air or oxygen atmosphere, sinter the material for 4-10 h, and naturally cool the material to room temperature to obtain the high-voltage lithium cobaltate composite positive electrode material.
8. A lithium battery, characterized in that: the positive electrode material includes the high voltage lithium cobaltate positive electrode material according to claim 1.
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