CN112803011A - Surface modified positive electrode material, battery and preparation method and application thereof - Google Patents
Surface modified positive electrode material, battery and preparation method and application thereof Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- 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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a surface modified anode material, a battery, a preparation method and application thereof. The preparation method of the surface modified cathode material comprises the following steps: and carrying out an acidification reaction on the positive electrode material and the acidic solution. The lithium ion battery prepared from the surface modified cathode material has high capacity and good rate capability, and the surface modified cathode material and the lithium ion battery have simple preparation methods and low cost, and are suitable for industrial production.
Description
Technical Field
The invention relates to a surface modified anode material, a battery, a preparation method and application thereof.
Background
Lithium ion batteries are widely used, and not only relate to commonly used portable electronic products (such as mobile phones, computers, cameras and the like), but also relate to energy storage applications in automobiles and renewable energy environments such as solar energy or wind energy. The requirements of different application environments on the lithium ion battery are different, for example, in portable electronic products and energy storage applications, the lithium ion battery is required to have stable long cycle performance; when the lithium ion battery is applied as a power battery of an automobile, the lithium ion battery is required to have not only stable long cycle performance but also higher capacity and rate capability.
In order to improve the capacity and rate capability of the lithium ion battery, in the prior art, the anode material is subjected to coating modification or doping modification, and the de-intercalation amount of lithium ions is regulated and controlled, so that the capacity of the lithium ion battery is improved; meanwhile, the formation of a CEI film with ionic conduction and electronic insulation functions on the surface of the anode is accelerated by enhancing the reaction activity of the anode material and the interface material, and the rate capability of the lithium ion battery is improved. However, the uniformity of the cathode material obtained by coating modification or doping modification is not good, and the reaction activity of the cathode material obtained by coating modification and an interface substance is low, so that when the cathode material is used in a lithium ion battery, the capacity cannot be effectively improved, and the rate capability of the lithium ion battery cannot be improved.
Chinese patent document CN 104183821A discloses a surface modification technology of lithium nickel cobalt manganese oxide, wherein a lithium nickel cobalt manganese oxide positive electrode material is added into a modification solvent, stirred and filtered, and then the obtained filter cake is subjected to heat treatment to obtain a surface-modified lithium nickel cobalt manganese oxide positive electrode material; the nickel cobalt lithium manganate positive electrode material with the modified surface is used in a lithium ion battery, and has high cycle performance and high temperature performance. However, the modified solvent (ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate or propylene carbonate) used in the method has no conductivity, and thus the electron conduction is influenced; from the perspective of reaction kinetics, the nickel cobalt lithium manganate cathode material after surface modification has low reactivity, and when the nickel cobalt lithium manganate cathode material is used for a lithium ion battery, the capacity and rate capability of the lithium ion battery cannot be effectively improved.
Therefore, it is desirable to provide a surface modified cathode material that can effectively improve the capacity and rate capability of a lithium ion battery.
Disclosure of Invention
The invention aims to overcome the defects of low capacity or poor rate capability of a positive electrode material used in a lithium ion battery in the prior art, and provides a surface modified positive electrode material, a battery, a preparation method and application thereof. The lithium ion battery prepared by the surface modified cathode material has high capacity and better rate capability, and the surface modified cathode material and the lithium ion battery have simple preparation methods and low cost and are suitable for industrial production.
In order to achieve the purpose, the invention provides the following technical scheme:
one of the technical schemes provided by the invention is as follows: a method for preparing a surface modified anode material. The preparation method comprises the following steps: and carrying out an acidification reaction on the positive electrode material and the acidic solution.
In the invention, the cathode material can be a lithium-containing cathode material which is conventional in the field; such as one or more of lithium oxide, lithium manganese oxide, lithium sulfide, lithium chromium oxide, lithium phosphate, and lithium carbide; lithium oxide or lithium manganese oxide is preferred.
The lithium oxide may be conventional in the art, such as lithium nickel cobalt manganese oxide, among others.
The chemical formula of the nickel cobalt lithium manganate is generally LiaNixCoyMnzO2(ii) a Wherein x + y + z is 1, x may be 0.3 to 0.9, y may be 0 to 0.4, and z may be 0 to 0.4; the a can be 0.9-1.1.
Said a is preferably 1. Said x is preferably 0.33, 0.5 or 0.8. Preferably, y is 0.1, 0.2 or 0.33. Preferably, z is 0.1, 0.3 or 0.33.
More preferably, the lithium nickel cobalt manganese oxide is LiNi0.33Co0.33Mn0.33O2、LiNi0.5Co0.2Mn0.3O2Or LiNi0.8Co0.1Mn0.1O2。
In the invention, the acidic solution can be one or more of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution, nitric acid solution, hydrofluoric acid solution, hydrobromic acid solution, hydroiodic acid solution, perchloric acid solution, sulfurous acid solution, nitrous acid solution and acetic acid solution; preferably one or more of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution, nitric acid solution and hydrofluoric acid solution; more preferably a phosphoric acid solution or a hydrochloric acid solution.
The concentration of the acidic solution can be 0.01-20 mol/L; preferably 0.04-15 mol/L; more preferably 0.05 to 10 mol/L; further preferably 2 to 5mol/L, for example 4 mol/L.
In the present invention, the volume of the acidic solution per 1g of the positive electrode material may be 8 to 60mL, preferably 9 to 50mL, and more preferably 9.6mL, 23.8mL, or 45.5 mL. For example, when the mass of the positive electrode material is 2g, the volume of the acidic solution is 16-120 mL.
In the present invention, the acidification reaction may be performed after dispersing the cathode material in the acidic solution, according to a conventional method in the art.
Among them, the dispersion is preferably uniform. The temperature of the dispersion is preferably 20-30 ℃. More preferably, the acidification reaction is performed after the cathode material is uniformly dispersed in the acidic solution at 20-30 ℃.
The temperature of the acidification reaction can be 90-600 ℃; preferably 100-500 ℃; more preferably 120-300 ℃; for example 150 deg.c.
The time of the acidification reaction can be 0.5-8 h; preferably 1-6 h; more preferably 2-5 h; further preferably 2.5 hours.
In the invention, after the acidification reaction, the method also comprises the steps of solid-liquid separation and drying.
Wherein the solid-liquid separation may be conventional in the art, such as centrifugation.
The rotation speed of the centrifugation can be conventional in the field, for example, 3000-6000 rpm, and preferably 4000 rpm.
The number of centrifugation can be conventional in the art, and can be generally more than 1, for example 2-5. The time of each centrifugation can be 10-30 min, and preferably 20 min.
Wherein the drying temperature can be conventional in the field, such as 100-150 ℃, and is preferably 110 ℃.
The drying time may be conventional in the art, for example, 2 to 3 hours.
Preferably, the drying method further comprises a step of heat treatment after the drying is finished. The temperature of the heat treatment can be conventional in the art, for example, 200-300 ℃, and preferably 250 ℃. The time of the heat treatment can be conventional in the art, for example, 15 to 60min, preferably 30 min.
In the present invention, the method for preparing the surface-modified cathode material preferably includes the steps of: carrying out acidification reaction on the positive electrode material and an acidic solution, and then sequentially carrying out centrifugation, drying and heating treatment; wherein the positive electrode material is a lithium oxide; the acid solution is one or more of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution and nitric acid solution; the concentration of the acidic solution is 0.05-5 mol/L; the temperature of the acidification reaction is 100-200 ℃; the time of the acidification reaction is 2-3 h; the rotation speed of the centrifugation is 3500-4500 rpm; the centrifugation times are 2-4; the time of each centrifugation is 10-30 min; the drying temperature is 100-120 ℃; the drying time is 2-3 h; the temperature of the heating treatment is 220-280 ℃; the heating treatment time is 20-50 min.
In a preferred embodiment of the present invention, the method for preparing the surface-modified cathode material preferably includes the following steps: carrying out acidification reaction on the positive electrode material and an acidic solution, and then sequentially carrying out centrifugation, drying and heating treatment; wherein the positive electrode material is nickel cobalt lithium manganate; the chemical formula of the nickel cobalt lithium manganate is LiNi0.5Co0.2Mn0.3O2(ii) a The acid solution is phosphoric acid solution; the concentration of the acid solution is 4 mol/L; the temperature of the acidification reaction is 100 ℃; the time of the acidification reaction is 2.5 h; the rotation speed of the centrifugation is 4000 rpm; the centrifugation times are 3 times; the time of each centrifugation is 20 min; the drying temperature is 110 ℃; the drying time is 2-3 h; the temperature of the heating treatment is 250 ℃; the time of the heat treatment is 30 min.
The second technical scheme provided by the invention is as follows: the surface modified cathode material is prepared by the preparation method of the surface modified cathode material.
The third technical scheme provided by the invention is as follows: a surface modified anode material. The surface modified positive electrode material comprises a porous layer and a solid layer; the porous layer is located outside the solid layer;
in the porous layer, the diameter of pores is 10-2000 nm.
In the invention, the thickness of the porous layer accounts for 25-75% of the particle size of the surface modified cathode material; preferably 30-70%; more preferably 40 to 60%.
In the porous layer, the diameter of the pores is preferably 100-1000 nm; more preferably 300 to 800 nm.
The particle size of the surface modified anode material can be 0.5-10 mu m; preferably 2-8 μm; more preferably 4 to 6 μm.
The fourth technical scheme provided by the invention is as follows: an application of the surface modified cathode material in a lithium ion battery.
The fifth technical scheme provided by the invention is as follows: a lithium ion battery comprising a surface modified cathode material as described previously.
The preparation method of the lithium ion battery can be a conventional method in the field.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
(1) the surface modified anode material has large specific surface area, the pores in the porous layer are uniformly distributed, the deintercalation of lithium ions can be effectively promoted, the inherent impedance (below 9.6 omega) and the charge transfer impedance (below 23.3 omega) of the surface modified anode material are small, the interfacial reactivity of the porous layer is strong, a stable CEI film can be quickly formed, and the capacity and the rate capability of a lithium ion battery can be effectively improved when the surface modified anode material is used for the lithium ion battery.
(2) The preparation method of the surface modified cathode material is simple, low in cost and suitable for industrial production.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples or comparative examples, the commercially available source of NCM (111) and NCM (523) is north Hu capacitor lithium battery materials, Inc.
Examples 1 to 4 preparation of surface-modified cathode Material
Mixing the anode material with the acid solution at room temperature (25 ℃), uniformly dispersing the anode material in the acid solution, and carrying out an acidification reaction; then carrying out centrifugation, drying and heating treatment in sequence; and (4) finishing.
The type and mass of the positive electrode material, and the type and volume and concentration of the acidic solution are shown in table 1. The temperature and time of the acidification reaction, the rotation speed, the number of times and the time of centrifugation, the temperature and the time of drying, and the temperature and the time of heat treatment are shown in Table 2.
TABLE 1
TABLE 2
Comparative example 1
The positive electrode material of the lithium ion battery in comparative example 1 was commercially available NCM 111.
Comparative example 2
The positive electrode material of the lithium ion battery in comparative example 2 was a commercially available NCM 523.
Effects of the embodiment
Testing of intrinsic impedance and charge transfer impedance:
the surface modified positive electrode material in the examples or the positive electrode material in the comparative example was mixed with conductive carbon black (SP) and PVDF as a binder at a ratio of 92:4:4 to prepare a positive electrode slurry, which was coated on an aluminum foil, rolled and tabletted. A lithium plate as a negative electrode, a polypropylene diaphragm and 1M LiPF electrolyte6The solvent of the solution is 1: 1: 1 of Ethylene Carbonate (EC), dimethyl carbonate (DMC) and methyl ethyl carbonate (EMC). In a vacuum glove box protected by argon, a button cell is assembled and assembled according to the sequence of a positive electrode battery case, a positive electrode pole piece, a diaphragm, electrolyte, a lithium piece, foamed nickel and a negative electrode battery case, and the Electrochemical Impedance Spectroscopy (EIS) of the button cell is tested on an Autolab40 electrochemical test platform.
The test results are shown in table 3.
TABLE 3
| Examples or comparative examples | Natural impedance omega | Charge transfer impedance omega |
| Comparative example 1 | 10.4 | 26.8 |
| Comparative example 2 | 11.2 | 32.8 |
| Example 3 | 7.9 | 19.4 |
| Example 4 | 9.6 | 23.3 |
As can be seen from table 3, the surface-modified positive electrode materials in examples 3 to 4 have small charge transfer resistance, which indicates that the surface-modified positive electrode materials have strong interfacial reaction activity and good rate capability. The intrinsic impedance and the charge transfer impedance of examples 1 to 2 are equivalent to those of example 3, and compared with examples 1 to 3, the modification degree of example 4 is large, and the intrinsic impedance and the charge transfer impedance are slightly higher. The unmodified positive electrode materials in the comparative examples 1-2 have high charge transfer resistance, which shows that the interfacial reaction activity is weak and the rate performance is poor.
Meanwhile, the inherent impedance of the surface modified cathode material in the embodiments 3-4 is small, which indicates that the surface modified cathode material has larger capacity when being used in a lithium ion battery. The unmodified positive electrode materials in the comparative examples 1-2 have high inherent resistance, which shows that the capacity is small when the positive electrode materials are used in lithium ion batteries.
Claims (10)
1. The preparation method of the surface modified cathode material is characterized by comprising the following steps of: and carrying out an acidification reaction on the positive electrode material and the acidic solution.
2. The method of preparing a surface modified cathode material according to claim 1, wherein the cathode material is one or more of lithium oxide, lithium manganese oxide, lithium sulfide, lithium chromide, lithium phosphate, and lithium carbide; preferably lithium oxide or lithium manganese oxide;
and/or the acid solution is one or more of a phosphoric acid solution, a hydrochloric acid solution, a sulfuric acid solution, a nitric acid solution, a hydrofluoric acid solution, a hydrobromic acid solution, a hydroiodic acid solution, a perchloric acid solution, a sulfurous acid solution, a nitrous acid solution and an acetic acid solution; preferably one or more of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution, nitric acid solution and hydrofluoric acid solution; more preferably a phosphoric acid solution or a hydrochloric acid solution;
and/or the concentration of the acidic solution is 0.01-20 mol/L; preferably 0.04-15 mol/L; more preferably 0.05 to 10 mol/L; further preferably 2 to 5mol/L, for example 4 mol/L;
and/or the volume of the acid solution corresponding to each 1g of the cathode material is 8-60 mL, preferably 9-50 mL, more preferably 9.6mL, 23.8mL or 45.5 mL.
3. The method for producing a surface-modified positive electrode material according to claim 1 or 2, wherein the acidification reaction is performed after dispersing the positive electrode material in the acidic solution;
the dispersion is preferably a uniform dispersion; the preferable temperature of the dispersion is 20-30 ℃;
more preferably, the acidification reaction is carried out after the cathode material is uniformly dispersed in the acid solution at the temperature of 20-30 ℃;
and/or the temperature of the acidification reaction is 90-600 ℃; preferably 100-500 ℃; more preferably 120-300 ℃; such as 150 ℃;
and/or the time of the acidification reaction is 0.5-8 h; preferably 1-6 h; more preferably 2-5 h; further preferably 2.5 hours.
4. The method for producing a surface-modified positive electrode material according to claim 1 or 2, further comprising a step of solid-liquid separation and drying after the acidification reaction;
wherein the solid-liquid separation is preferably centrifugation;
the rotating speed of the centrifugation is preferably 3000-6000 rpm, and more preferably 4000 rpm;
the centrifugation frequency is preferably more than 1 time, for example 2-5 times; the time of each centrifugation is preferably 10-30 min, and more preferably 20 min;
wherein the drying temperature is preferably 100-150 ℃, and more preferably 110 ℃;
the drying time is preferably 2-3 h;
wherein, after the drying is finished, the method preferably further comprises the step of heating treatment;
the temperature of the heating treatment is preferably 200-300 ℃, and more preferably 250 ℃; the time of the heat treatment is preferably 15 to 60min, and more preferably 30 min.
5. The method of preparing a surface-modified positive electrode material according to claim 4, comprising the steps of: carrying out acidification reaction on the positive electrode material and an acidic solution, and then sequentially carrying out centrifugation, drying and heating treatment;
wherein the positive electrode material is a lithium oxide; the acid solution is one or more of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution and nitric acid solution; the concentration of the acidic solution is 0.05-5 mol/L; the temperature of the acidification reaction is 100-200 ℃; the time of the acidification reaction is 2-3 h; the rotation speed of the centrifugation is 3500-4500 rpm; the centrifugation times are 2-4; the time of each centrifugation is 10-30 min; the drying temperature is 100-120 ℃; the drying time is 2-3 h; the temperature of the heating treatment is 220-280 ℃; the heating treatment time is 20-50 min.
6. A surface-modified positive electrode material, characterized by being produced by the method for producing a surface-modified positive electrode material according to any one of claims 1 to 5.
7. A surface modified cathode material is characterized by comprising a porous layer and a solid layer; the porous layer is located outside the solid layer;
in the porous layer, the diameter of pores is 10-2000 nm.
8. The surface-modified positive electrode material according to claim 7, wherein the porous layer has a thickness of 25 to 75% based on the particle diameter of the surface-modified positive electrode material; preferably 30-70%; more preferably 40-60%;
and/or in the porous layer, the diameter of the pores is 100-1000 nm; preferably 300-800 nm;
and/or the particle size of the surface modified anode material is 0.5-10 μm; preferably 2-8 μm; more preferably 4 to 6 μm.
9. Use of the surface modified cathode material according to any one of claims 6 to 8 in a lithium ion battery.
10. A lithium ion battery, characterized in that it comprises the surface-modified positive electrode material according to any one of claims 6 to 8.
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