CN110444752B - Ternary cathode material of long-life lithium ion battery and preparation method and application thereof - Google Patents
Ternary cathode material of long-life lithium ion 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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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- H01M4/52—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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Abstract
The invention discloses a long-life lithium ion battery ternary anode material, which comprises a ternary material serving as a substrate and a polymer coating layer coated on the surface of the ternary material, wherein the polymer comprises a polymer
The structure of the polycarboxylic ester high molecular compound. The invention also provides a preparation method and application of the ternary cathode material of the long-life lithium ion battery. The ternary cathode material of the long-life lithium ion battery has good mechanical property, excellent capacitance characteristic, low price and simple preparation, and can be popularized and used as a commercial capacitor material.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a ternary cathode material of a long-life lithium ion battery, and a preparation method and application thereof.
Background
In recent years, with the increasing demands for electric vehicles, hybrid electric vehicles and large-scale energy storage, people have raised higher requirements for the energy density and the manufacturing cost of lithium ion batteries, and on one hand, the specific capacity and the specific energy of the anode material need to be greatly improved, and the demand for cobalt also needs to be reduced. In this context, ternary positive electrode materials have attracted a great deal of attention. The ternary positive electrode material has LiNi1-x-yCoxMyO2(1. gtoreq.x.gtoreq.0, 1. gtoreq.y.gtoreq.0, x + y < 1, and M ═ Mn, Al) includes currently common NCM811, NCM622, NCM523, NCM111, and NCA. The outstanding advantages of the material are that on one hand, the requirement for cobalt is greatly reduced, the material has obvious price advantage, and more importantly, the specific capacity of the material is also obviously improved and can reach 200mAh g-1Therefore, the lithium ion battery has important application value and prospect in future high-energy-density lithium ion batteries, and is an ideal positive electrode material for hybrid power electric vehicles.
However, most of the currently commonly used ternary cathode materials for lithium ion batteries contain relatively high Ni, particularly, Ni4+ therein has strong oxidizability, and can oxidize and induce obvious interface side reactions when being in direct contact with an electrolyte, and generate components such as organic acids to further erode the ternary cathode materials, so that on one hand, Ni dissolution and structural damage of the ternary cathode materials are caused, and on the other hand, the electrode/electrolyte interface resistance is also increased, so that the stable cycle stability, thermal stability and high rate performance of the materials are not good enough, and in this sense, the improvement of the interface stability of the ternary materials has important application value and development prospect for future wide scale application. In fact, in recent years, much work has been done on surface interface modification of lithium ion battery ternary positive electrode materials, and most of the work has focused on inorganic carbon material coating, oxide coating, phosphide coating, organic conductive polymer coating and the like. The carbon coating is mainly used for improving the electronic conductivity of the material and has little help on inhibiting the electrode/electrolyte interface reaction; the coating of the oxide and the phosphide is beneficial to reducing the interface reaction of the electrode/electrolyte, but the inorganic material has large brittleness, the coating is uneven and continuous, and the coating is easy to crack in the electrode charging and discharging process, so the function of the material is limited, the conductive polymer can realize the protection of the ternary anode material while improving the electronic conductivity of the electrode, but the material has poor oxidation resistance stability, and the nitrogen atoms, Ni, Co and Mn do not have chemical bonds to rent mutually, so the improvement effect is not ideal.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a ternary cathode material of a lithium ion battery with long service life and a preparation method thereof.
In order to solve the technical problems, the invention provides a ternary cathode material of a long-life lithium ion battery, which comprises a ternary material used as a substrate and a polymer coating layer coated on the surface of the ternary material, wherein the polymer comprises a polymer with a surface layer
The structure of the polycarboxylic ester high molecular compound.
Further, the polycarboxylate-type high-molecular compound is selected from one or more of polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate, polyisobutyl methacrylate, vinyl chloride methacrylate copolymer, polyglycidyl methacrylate, polyhydroxypropyl methacrylate and poly (trifluoroethyl 2,2, 2-methacrylate) similar structures.
The polymer may further include the above-mentioned polycarboxylate polymer compound mixed with other common polymer coating materials, such as polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF), etc.
Further, the ternary material has LiNi1-x-yCoxMyO2(x is more than or equal to 1 and more than or equal to 0, y is more than or equal to 1 and more than or equal to 0, x + y is less than 1, and M is Mn and Al).
Further, the ternary material is selected from one or a mixture of more than two of NCM811, NCM622, NCM523, NCM111 and NCA.
Further, the weight ratio of the polymer coating layer material to the ternary material is 0.2-5%.
The invention also provides a preparation method of the ternary cathode material of the long-life lithium ion battery, which comprises the following steps:
s1, dissolving the macromolecule in a solvent to obtain macromolecule solution;
s2, soaking the ternary cathode material in the polymer solution, and heating and stirring until the solvent is completely volatilized; and taking out the ternary cathode material, and drying to obtain the long-life lithium ion battery ternary cathode material.
Further, the solvent is one or a mixture of more than two of ethanol, glycerol, ethylene glycol, methanol, N, N dimethylformamide, N-methylpyrrolidone, isopropanol, dimethyl sulfoxide and acetone.
Further, the heating temperature is 30-200 ℃.
Further, the drying is drying under a vacuum condition, the drying time is 1-10 hours, and the drying temperature is 80-200 ℃.
The invention also provides application of the ternary cathode material of the long-life lithium ion battery in the field of lithium ion batteries.
The invention has the beneficial effects that:
1. according to the invention, a simple liquid phase coating technology is utilized, a uniform organic coating layer can be formed on the surface of the anode material, and the thickness of the coating layer can be regulated and controlled by adjusting the concentration and the dosage of the solution; oxygen atoms in the carboxylic ester in the coating layer can establish strong chemical bond interaction with metal ions on the surface of active substance particles, so that the coating effect is good; the wetting property between the polycarboxylate coating layer and the carbonate solution is good, and the interface impedance is small; the polycarboxylate has good electrochemical stability, the decomposition voltage is up to more than 4.6V, and the side reaction of the anode material and the electrolyte can be inhibited; such a tight coating layer helps to suppress dissolution of metal cations in the electrolyte, and protects the surface and structural stability of the positive electrode material.
2. The product obtained by the method provided by the invention has obviously improved cycle stability and rate capability, and meanwhile, the method provided by the invention does not need high-temperature treatment, is low in cost, low in energy consumption, easy to obtain raw materials, simple in process flow, environment-friendly and easy to realize large-scale production.
Drawings
FIG. 1 is a first charge-discharge diagram of examples 1, 2, 3 and comparative example 1;
FIG. 2 is a graph of the rate cycles for examples 1, 2, 3 and comparative example 1;
FIG. 3 is a 1C cycle chart for examples 1, 2, 3, 4, 5, 6 and comparative examples 1, 2, 3;
FIG. 4 is a plot of AC impedance after cycling for examples 1, 2, 3 and comparative example 1;
FIG. 5 is an electron micrograph of comparative example 1;
FIG. 6 an electron micrograph of example 1;
fig. 7 example 1 a coating preparation process flow diagram and a battery process preparation flow.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
This example provides a single crystal LiNi0.8Co0.1Mn0.1O2The interface modification and preparation method specifically comprises the following steps:
(a) 0.05g of polymethyl methacrylate (PMMA) is heated and dissolved in 10g of acetone solvent (molecular sieve dehydration), and stirred for 2 hours to form a uniform solution.
(b) 2g of single-crystal LiNi was taken0.8Co0.1Mn0.1O2And (3) slowly adding the active material into the PMMA solution at the temperature of 30 ℃, continuously stirring, and heating the solution under the condition of continuous stirring until the solvent is completely volatilized.
(c) Aging the powder product obtained in the step in a vacuum drying oven at the temperature of 60 ℃ for 8 hours to obtain the ternary coating anode material with the PMMA coating amount of 2.5%.
The invention also provides application of the coated ternary cathode material in a lithium ion battery, wherein the coated modified single crystal ternary cathode material obtained in the step is subjected to a battery flaking process, the battery is assembled in a dry room, and an electrochemical performance test is performed at room temperature. All batteries are firstly converted into 5 circles by 0.1C current and then subjected to 1C cycle test and rate test (0.5C full charge is sequentially subjected to 0.5, 1, 2, 5, 10 and 20 for discharge test, wherein the small rates of 0.1C and 0.2C are charged and discharged at the same rate)
Example 2
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2The preparation method of the cathode material is basically the same as that in example 1, except that 0.03g of polyethyl methacrylate (PEMA) is dissolved in 10g of toluene solvent for coating modification, and the ternary coating cathode material with the PEMA coating amount of 1.5% is obtained.
Example 3
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2Preparation of cathode materialThe preparation method is basically the same as that in example 1, except that 0.04g of the polyisoethyl methacrylate is dissolved in 10g of the toluene solvent for coating modification, and the polyisoethyl methacrylate ternary coating anode material with the coating amount of 2.0% is obtained.
Example 4
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2The preparation method of the cathode material is basically consistent with that in example 1, except that 0.04g of vinyl chloride methacrylate copolymer is dissolved in 10g of dimethyl sulfoxide solvent for coating modification, and the vinyl chloride methacrylate copolymer ternary coating cathode material with the coating amount of 2.0% is obtained.
Example 5
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2The preparation method of the cathode material is basically the same as that in example 1, except that 0.04g of polyhydroxypropylmethacrylate is dissolved in 10g of dimethyl sulfoxide solvent for coating modification, and the polyhydroxypropylmethacrylate ternary coating cathode material with the coating amount of 2.0% is obtained.
Example 6
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2The preparation method of the cathode material is basically consistent with that in example 1, except that 0.02g of PMMA and 0.02g of PVDF are dissolved in 10g N-methyl pyrrolidone for coating modification, and 0.04g of polyhydroxypropylmethacrylate in acetone solvent (molecular sieve water removal) is dissolved in 10g of dimethyl sulfoxide solvent for coating modification, so that the mixed coated cathode material of PMMA and PVDF with the coating amount of 2.0% is obtained.
Example 7
This example provides a coated single crystal LiNi0.8Co0.1Mn0.1O2The preparation method of the cathode material is basically the same as that in the embodiment 1, except that 0.02g of PMMA is dissolved in acetone to carry out coating modification on the ternary cathode material, and then 0.02g of PVDF is dissolved in 10g N-methylpyrrolidineAnd (3) carrying out coating modification in ketone to obtain a coated ternary single crystal positive electrode material with the PMMA and PVDF double-layer coating amount of 2.0%.
Comparative example 1
Comparative example 1 provides a non-cladding type single crystal LiNi0.8Co0.1Mn0.1O2And (3) carrying out a button cell flaking process on the material, assembling the cell in a dry chamber, and carrying out an electrochemical performance test at room temperature. All the batteries are firstly converted into 5 circles by 0.1C current and then subjected to test 1C cycle test and rate test (0.5C full charge is sequentially subjected to discharge tests at 0.5, 1, 2, 5, 10 and 20, wherein the small rates of 0.1C and 0.2C are charged and discharged at the same rate).
Comparative example 2
Comparative example 2 provides a PVDF-coated Single Crystal LiNi0.8Co0.1Mn0.1O2The preparation process of the material is basically the same as that in the example 1, except that 0.06g of PVDF is dissolved in N-methyl pyrrolidone to carry out coating modification on the ternary cathode material, so that the PVDF-coated ternary cathode material with the coating amount of 3.0% is obtained, and the test conditions are the same as those in the comparative example 1.
As can be seen from fig. 1, the initial charge-discharge capacity and coulombic efficiency of the polycarboxylate-coated ternary material prepared in different examples are both improved to a certain extent, and more importantly, the rate performance of the ternary material prepared in the example in fig. 2 is remarkably improved, and particularly, the material prepared in the example 1 still has a high capacity retention rate under the condition of 10C, and shows excellent rate charge-discharge properties.
Fig. 3 compares the cycle performance of the ternary cathode material obtained in different comparative examples and examples, and it can be seen that the cycle performance of the ternary cathode material using the polycarboxylate coating layer is significantly improved, and after 100 cycles, the capacity retention rate of the polycarboxylate coating modified material is significantly higher than that of the ternary cathode material coated and uncoated by PVDF.
FIG. 4 compares the impedance behavior of the polycarboxylate coated ternary material prepared in the different examples, and the electrochemical impedance of the material is significantly reduced compared to the comparative example.
Fig. 5 and fig. 6 compare the material morphology of comparative example 1 and example 1, and it can be seen that the organic material coating on the surface of the example is continuous and uniform, and the function advantage of the polycarboxylate coating is utilized to help to improve the macro electrochemical property of the ternary cathode material.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (8)
1. The ternary cathode material of the long-life lithium ion battery is characterized by comprising a ternary material serving as a substrate and a high polymer coating layer coated on the surface of the ternary material, wherein the high polymer comprises a polycarboxylate-type high polymer compound, and the polycarboxylate-type high polymer compound is selected from one or more of polyethyl methacrylate, polybutyl methacrylate, polyisobutyl methacrylate, vinyl chloride methacrylate copolymer, polyglycidyl methacrylate, polyhydroxypropyl methacrylate and poly (trifluoroethyl 2,2, 2-methacrylate); the weight ratio of the polymer coating layer to the ternary material is 0.2-5%.
2. The long life lithium ion battery ternary positive electrode material of claim 1, wherein said ternary material comprises LiNi1-x-yCoxMyO2(1 > x > 0, 1 > y > 0, x + y < 1, M ═ Mn, Al).
3. The long life lithium ion battery ternary positive electrode material of claim 2, wherein said ternary material is selected from one or a mixture of two or more of NCM811, NCM622, NCM523, NCM111 and NCA.
4. The preparation method of the ternary cathode material for the long-life lithium ion battery as claimed in any one of claims 1 to 3, characterized by comprising the following steps:
s1, dissolving the macromolecule in a solvent to obtain macromolecule solution;
s2, soaking the ternary material in the polymer solution, and heating and stirring until the solvent is completely volatilized; and taking out the ternary material, and drying to obtain the long-life lithium ion battery ternary cathode material.
5. The method for preparing the ternary cathode material for long-life lithium ion batteries according to claim 4, wherein the solvent is one or a mixture of two or more selected from ethanol, glycerol, ethylene glycol, methanol, N, N-dimethylformamide, N-methylpyrrolidone, isopropanol, dimethyl sulfoxide and acetone.
6. The method for preparing the ternary cathode material for the long-life lithium ion battery of claim 4, wherein the heating temperature is 30-200 ℃.
7. The method for preparing the ternary cathode material of the long-life lithium ion battery as claimed in claim 4, wherein the drying is carried out under vacuum condition, the drying time is 1-10 hours, and the drying temperature is 80-200 ℃.
8. The long-life lithium ion battery ternary cathode material as claimed in any one of claims 1 to 3, which is used in the field of lithium ion batteries.
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