CN111416117A - Preparation method of CdTe quantum dot modified lithium battery positive electrode material - Google Patents
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- CN111416117A CN111416117A CN202010166469.8A CN202010166469A CN111416117A CN 111416117 A CN111416117 A CN 111416117A CN 202010166469 A CN202010166469 A CN 202010166469A CN 111416117 A CN111416117 A CN 111416117A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- 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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a CdTe quantum dot modified lithium battery anode material. The CdTe quantum dot modified lithium battery positive electrode material prepared by the method disclosed by the invention is high in quantum dot stability, not easy to decompose and good in conductivity, and the CdTe quantum dot is used for modifying a ternary material and can be used for well enhancing the electrochemical performance of the ternary lithium battery material.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a CdTe quantum dot modified lithium battery anode material.
Background
Based on ternary transition goldMetal oxide (L iNi)xCoyMnzO2NCM) has been regarded as the most promising lithium ion battery material, compared to the conventional L iCoO positive electrode material2The ternary material NCM has the characteristics of high energy density, low cost, low toxicity and the like.
The traditional preparation method adopts a high-temperature solid phase method, uniformly mixes materials by a mechanical means, and then obtains the ternary cathode material by high-temperature sintering, but the defect is that the ternary cathode material is easily influenced by the mixing machinery, and different mixing means have great influence on the material. Secondly, mechanical solid-phase mixing is not beneficial to uniformly mixing effective elements, and the particle size of the material is difficult to uniformly sinter.
In addition, the lower cycling capability of the NCM material under high voltage charging conditions limits its use. To address this problem, various approaches have been attempted to optimize the material, including lattice doping and surface cladding. The methods can effectively improve the circulation capacity of the material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a CdTe quantum dot modified lithium battery positive electrode material, wherein the CdTe quantum dot modified lithium battery positive electrode material has high stability, is not easy to decompose and has good conductivity, and the CdTe quantum dot is used for modifying a ternary material and can well enhance the electrochemical performance of the ternary lithium battery material.
The technical scheme of the invention is as follows:
a preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing a ternary precursor solution: in a protective atmosphere, NiSO4、CoSO4And MnSO4Mixing the aqueous solution, heating, adding an alkaline solution to adjust the pH value, and violently stirring to obtain a ternary precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; CdCl is then prepared2An aqueous solution of a carboxylic acid and a carboxylic acid,introducing nitrogen to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding a mercaptosuccinic acid solution into the aqueous solution, quickly adding the prepared NaHTe solution under the condition of nitrogen, adding an alkaline solution to adjust the pH value, and continuously stirring under the protection of nitrogen to obtain a light yellow transparent solution, namely a quantum dot precursor solution; wherein the molar ratio of the components is Cd2+: mercaptosuccinic acid: NaHTe = 1: 1.2: 0.1;
(3) and mixing the ternary precursor solution and the quantum dot precursor solution to ensure that the mass percent of the CdTe quantum dots is 0.5-3%, and performing microwave treatment in a protective atmosphere to obtain the CdTe quantum dot modified lithium battery cathode material.
In the step (1), the molar ratio of Ni, Co and Mn is x: y: z, wherein x is more than or equal to 6, y is less than or equal to 2, z is less than or equal to 2, and x + y + z = 10.
And (3) adding an alkaline solution to adjust the pH value to 10-11.5 in the step (1) and the step (2).
The alkaline solution in the step (1) is a mixed solution of 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water, and the alkaline solution in the step (2) is 1 mol/L sodium hydroxide solution.
The time of vigorous stirring in the step (1) is 11-13 hours, and the temperature is 55-65 ℃.
In the step (2), the CdCl2The concentration of the aqueous solution was 1.25 x 10-3mol/L of the CdCl2The aqueous solution was purged with nitrogen for 30 min to remove dissolved oxygen from the aqueous solution.
In the step (2), after the pH value of the alkaline solution is adjusted, stirring is continued for 40-50 minutes under the protection of nitrogen, and a light yellow transparent solution, namely a quantum dot precursor solution, is obtained.
In the step (3), the protective atmosphere is an air atmosphere or an oxygen atmosphere.
In the step (3), the reaction power of the microwave treatment is 800-2000W, and the reaction time is 30-90 minutes.
The invention has the advantages that:
(1) due to the CdTe quantum dots in the lithium battery cathode material, the ternary lithium battery material has good conductivity, the surface defects of the material are reduced, and the cycle rate performance of the material is improved;
(2) the quantum dot precursor solution and the ternary precursor solution are mixed, so that the use amount of doping substances can be reduced, the use cost is reduced, and the substances in the material can be distributed more uniformly by using the solution mixing;
(3) the invention adopts the microwave pyrolysis method to prepare the ternary cathode material, thereby reducing the reaction time and improving the production efficiency.
Drawings
Fig. 1 is a capacity cycle diagram of assembled batteries of the lithium battery positive electrode materials prepared in examples 1, 2 and 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4Pumping the water solution (the cation molar ratio is Ni: Co: Mn = 8:1: 1) into a continuous stirred tank reactor, simultaneously adding 2 mol/L of sodium hydroxide solution and 2 mol/L of ammonia water, simultaneously adding alkaline solution to adjust the pH value to 10, and vigorously stirring at 60 ℃ for 12 hours to obtain NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting in a magnetic stirrerAfter several hours, the NaHTe solution is obtained; then, 1.25X 10 was prepared-3mol/L CdCl2Introducing nitrogen into the aqueous solution for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the aqueous solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 10, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparent solution, namely quantum dot precursor solution, wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to enable the mass fraction of the quantum dots to be 0.5%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating for 60 minutes with 800W power to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
Example 2
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4Pumping an aqueous solution (the cation molar ratio is Ni: Co: Mn = 8:1: 1) into a continuous stirred tank reactor, simultaneously adding a 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water, simultaneously adding an alkaline solution to adjust the pH value to 10.5, and violently stirring at 60 ℃ for 12 hours to obtain an NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; then, 1.25X 10 was prepared-3mol/L CdCl2Introducing nitrogen into the aqueous solution for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the water solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 10.5, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparentThe solution is quantum dot precursor solution; wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to enable the mass fraction of the quantum dots to be 1%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating with 1000W power for 60 minutes to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
Example 3
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4Pumping an aqueous solution (the cation molar ratio is Ni: Co: Mn = 8:1: 1) into a continuous stirred tank reactor, simultaneously adding a 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water, simultaneously adding an alkaline solution to adjust the pH value to 11.5, and violently stirring at 60 ℃ for 12 hours to obtain an NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; then, 1.25X 10 was prepared-3mol/L CdCl2Introducing nitrogen into the aqueous solution for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the aqueous solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 11.5, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparent solution, namely quantum dot precursor solution, wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to enable the mass fraction of the quantum dots to be 2%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating with 2000W power for 60 minutes to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
Example 4
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4Pumping an aqueous solution (the cation molar ratio is Ni: Co: Mn = 8:1: 1) into a continuous stirred tank reactor, simultaneously adding a 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water, simultaneously adding an alkaline solution to adjust the pH value to 11.5, and violently stirring at 60 ℃ for 12 hours to obtain an NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; then, 1.25X 10 was prepared-3mol/L CdCl2Introducing nitrogen into the aqueous solution for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the aqueous solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 11.5, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparent solution, namely quantum dot precursor solution, wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to enable the mass fraction of the quantum dots to be 2%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating for 90 minutes by using 1000W power to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
Example 5
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4(cation molar ratio Ni: Co: Mn = 8:1: 1) into a continuous stirred tankSimultaneously adding 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water into the reactor, simultaneously adding alkaline solution to adjust the pH value to 11, and violently stirring at 60 ℃ for 12 hours to obtain NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; then, 1.25X 10 was prepared-3mol/L CdCl2Introducing nitrogen into the aqueous solution for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the aqueous solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 11.5, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparent solution, namely quantum dot precursor solution, wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to enable the mass fraction of the quantum dots to be 2%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating with 1500W power for 30 minutes to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
Example 6
A preparation method of a CdTe quantum dot modified lithium battery anode material specifically comprises the following steps:
(1) preparing an NCM811 precursor: in N2Under the condition, the concentration is 2.0mol L-1NiSO (D)4、CoSO4And MnSO4Pumping an aqueous solution (the cation molar ratio is Ni: Co: Mn = 8:1: 1) into a continuous stirred tank reactor, simultaneously adding a 2 mol/L sodium hydroxide solution and 2 mol/L ammonia water, simultaneously adding an alkaline solution to adjust the pH value to 10.5, and violently stirring at 60 ℃ for 12 hours to obtain an NCM811 precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; then, 1.25X 10 was prepared-3mol/L CdCl2Aqueous solutionIntroducing nitrogen for 30 min to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding mercaptosuccinic acid solution (MSA) into the aqueous solution, rapidly adding the prepared NaHTe solution under the condition of nitrogen, adding 1 mol/L sodium hydroxide solution to adjust the pH value to 11, and continuously stirring for 45 minutes under the protection of nitrogen to obtain light yellow transparent solution, namely quantum dot precursor solution, wherein the molar ratio of the components is Cd2+:MSA:NaHTe = 1: 1.2 : 0.1;
(3) And mixing the ternary precursor solution and the quantum dot precursor solution to ensure that the mass fraction of the quantum dots is 3%, filtering the mixed solution, introducing oxygen into a microwave oven, and heating with 1000W power for 45 minutes to obtain the CdTe quantum dot modified ternary cathode material of the lithium battery.
And (3) performance testing:
the prepared positive electrode material is subjected to the following performance tests:
(1) the battery assembly is that the anode material prepared by the invention is made into an anode plate, the cathode is a metal lithium plate, the diaphragm is Celgard2400, and the electrolyte is L iPF of 1 mol/L6and/DMC + DEC, assembling to obtain CR2025 button cell. The preparation process of the positive pole piece comprises the following steps: mixing the prepared positive electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 8:1:1, using N-methylpyrrolidone NMP as a solvent to prepare slurry, coating the slurry on an aluminum foil, drying the aluminum foil at 120 ℃ for 24 hours, rolling and punching the aluminum foil into a wafer serving as a positive electrode piece.
(2) Electrochemical testing: under the condition of normal temperature, the charging and discharging voltage interval is 3.0-4.4V. Cycling at 1C current density for 50 weeks to test the capacity retention rate; and (3) rate performance test: and charging the battery to a charging cut-off voltage by adopting a current density of 0.5C, respectively testing the discharging specific capacities of the battery under the current densities of 0.1C, 0.2C, 1C and 3C, and calculating the ratios under different current densities. The lithium battery positive electrode materials prepared in the embodiments 1, 2 and 4 are assembled into a button cell and subjected to charge-discharge cycle performance test, a capacity cycle diagram is shown in figure 1, and multiplying power performance comparison is shown in the following table 1.
TABLE 1
Example number | 3C/0.1C | 3C/0.2C | 3C/1C |
Example 1 | 0.87235 | 0.91235 | 0.96224 |
Example 2 | 0.90887 | 0.91407 | 0.97415 |
Example 4 | 0.91419 | 0.92123 | 0.97473 |
As can be seen from fig. 1, the discharge capacities of examples 1, 2 and 4 were 195.1, 193.3 and 197.5mAh/g at 1C cycle, and after 50 cycles, the capacity retention rates were 93.82%, 97.76% and 96.94%. The data show that the capacity retention rate of the lithium battery can be improved by improving the reaction conditions of the quantum dots.
As can be seen from the data analysis in Table 1, after a certain amount of CdTe quantum dots are doped, the rate capability of the material can be effectively improved by adjusting the appropriate reaction time.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of a CdTe quantum dot modified lithium battery anode material is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) preparing a ternary precursor solution: in a protective atmosphere, NiSO4、CoSO4And MnSO4Mixing the aqueous solution, heating, adding an alkaline solution to adjust the pH value, and violently stirring to obtain a ternary precursor solution;
(2) preparing a quantum dot precursor solution: NaBH4Adding tellurium powder into the solution, and reacting for several hours in a magnetic stirrer to obtain a NaHTe solution; CdCl is then prepared2Adding nitrogen to remove CdCl2Dissolved oxygen in the aqueous solution; then CdCl2Adding a mercaptosuccinic acid solution into the aqueous solution, quickly adding the prepared NaHTe solution under the condition of nitrogen, adding an alkaline solution to adjust the pH value, and continuously stirring under the protection of nitrogen to obtain a light yellow transparent solution, namely a quantum dot precursor solution; wherein the molar ratio of the components is Cd2+: mercaptosuccinic acid: NaHTe = 1: 1.2: 0.1;
(3) and mixing the ternary precursor solution and the quantum dot precursor solution to ensure that the mass percent of the CdTe quantum dots is 0.5-3%, and performing microwave treatment in a protective atmosphere to obtain the CdTe quantum dot modified lithium battery cathode material.
2. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the molar ratio of Ni, Co and Mn is x: y: z, wherein x is more than or equal to 6, y is less than or equal to 2, z is less than or equal to 2, and x + y + z = 10.
3. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: and (3) adding an alkaline solution to adjust the pH value to 10-11.5 in the step (1) and the step (2).
4. The method for preparing the positive electrode material of the lithium battery modified by the CdTe quantum dots as claimed in claim 1, wherein the alkaline solution in the step (1) is a mixture of 2 mol/L of sodium hydroxide solution and 2 mol/L of ammonia water, and the alkaline solution in the step (2) is 1 mol/L of sodium hydroxide solution.
5. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: the time of vigorous stirring in the step (1) is 11-13 hours, and the temperature is 55-65 ℃.
6. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (2), the CdCl2The concentration of the aqueous solution was 1.25 x 10-3mol/L of the CdCl2The aqueous solution was purged with nitrogen for 30 min to remove dissolved oxygen from the aqueous solution.
7. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (2), after the pH value of the alkaline solution is adjusted, stirring is continued for 40-50 minutes under the protection of nitrogen, and a light yellow transparent solution, namely a quantum dot precursor solution, is obtained.
8. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the protective atmosphere is an air atmosphere or an oxygen atmosphere.
9. The preparation method of the CdTe quantum dot modified lithium battery positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the reaction power of the microwave treatment is 800-2000W, and the reaction time is 30-90 minutes.
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