CN111628151A - Surface modification method of ternary cathode material - Google Patents
Surface modification method of ternary cathode material Download PDFInfo
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- CN111628151A CN111628151A CN202010518596.XA CN202010518596A CN111628151A CN 111628151 A CN111628151 A CN 111628151A CN 202010518596 A CN202010518596 A CN 202010518596A CN 111628151 A CN111628151 A CN 111628151A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- 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
- 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
- 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
- H01M4/485—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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- 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
- 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
- H01M4/50—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
- 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
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a surface modification method of a ternary cathode material, which adopts acetylacetone metal composition solution as a coating solution of the ternary cathode material and utilizes a Plasma Enhanced Chemical Vapor Deposition (PECVD) technology to prepare the coating material of the ternary cathode material of a lithium ion battery. The plasma high-energy radiation promotes the elements to be decomposed and deposited on the surface of the material, so that the controllable deposition speed, the controllable deposition coating amount, the controllable deposition coating type and the controllable gradient of the coating material are realized. The method has the advantages of low reaction temperature, high speed, low cost and controllable content of the coating elements.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a surface modification method of a ternary cathode material.
Background
The most predominant electrolyte lithium salt in lithium ion batteries is LiPF6Lithium ion batteries are very sensitive to trace amounts of water, since the electrode reactions take place at the electrode/electrolyte interface. LiPF6Is less stable to heat and is easily decomposed into LiF(s) and PF5（g），PF5(g) And then reacted with water to produce HF. HF corrodes the anode material, causes the dissolution of metal ions in the material, and destroys the material structure, thereby deteriorating the electrochemical performance of the material. Because the electrode reaction of the lithium ion battery occurs at an electrode/electrolyte interface, the coating layer can prevent the main material from directly contacting with the electrolyte by performing surface coating modification on the ternary material, so that the capacity retention rate of the ternary material is improved, and the electrochemical performance of the ternary material is further improved.
At present, a physical mixing method, namely a solid phase method for coating and modifying the ternary cathode material is the most method for commercial production. The solid phase method is a physical mixing method, and the ternary cathode material and the coating material are mixed, so that the ternary cathode material is coated and modified. However, the high-strength rotary mixing process is prone to dissociation of the material itself, and even damages the structure of the material itself, the uniformity of the coating elements is difficult to control, and the material can be coated in a subsequent high-temperature and long-time sintering manner.
Therefore, it is important to find a preparation method for coating modification of the ternary cathode material, which has low reaction temperature, high speed, low cost and controllability.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problems to be solved by the invention are as follows: the surface modification method of the ternary cathode material with low reaction temperature, high speed, low cost and controllable coating element content is provided.
The solution of the invention is realized by the following steps:
a surface modification method of a ternary cathode material is characterized in that a solution obtained by dissolving an acetylacetone metal composition in a solvent is used as a coating solution of the ternary cathode material, and the surface modification of the ternary cathode material is completed in a plasma reaction furnace.
The invention adopts the acetylacetone metal composition to provide a stable metal source for plasma excitation.
More specifically, the surface modification method of the ternary cathode material comprises the following steps:
s1, preparing acetylacetone metal composition coating solution;
s2, placing the ternary cathode material in a plasma reaction furnace, and introducing inert gas into the reaction furnace; setting the frequency, power and reaction time of a plasma generator in the plasma reaction furnace;
and S3, when the furnace temperature of the plasma reaction furnace is raised to a certain temperature, according to the amount of the metal to be coated, injecting the coating solution into the plasma reactor, simultaneously starting the plasma generator, reacting for a certain time, then closing the plasma generator and the plasma reaction furnace, and obtaining the uniformly coated ternary cathode material after the reaction is finished.
Further, the solvent of the coating solution is preferably an alcohol or ether solvent.
Further, the solvent of the coating solution is preferably methanol.
Further, preferably, aluminum acetylacetonate is dissolved in a solvent to obtain a coating solution of the ternary cathode material.
Furthermore, the molar ratio of the acetylacetone metal composition to the solvent in the coating solution is 1:5 to 1: 10.
Further, the ternary cathode material is LiNixCoyMn1-x-yO2Wherein X is between 0.5 and 0.9.
Further, in the step S2, inert gas is introduced into the reaction furnace until the pressure in the reaction furnace is 1-10 MPa.
Further, in step S2, the power of the plasma generator is set to be 100-1200 w.
Further, in step S3, the temperature of the plasma reaction furnace is raised to 100-400 ℃.
Further, in step S3, after the plasma generator is turned on, the reaction time is continued for 2 to 30 min.
Further, the injection rate of the coating solution in step S3 is 30mL/h to 100 mL/h.
The injection speed and the coating amount have positive correlation in a certain range, the coating amount can be influenced in the early stage, the faster the injection speed is, the more the coating amount is, but after the injection speed reaches a certain speed, the coating amount cannot be obviously influenced; the injection speed affects the uniformity of the coating and needs to be adjusted according to the material.
Furthermore, coating solutions of different metal elements can be injected, the injected coating solution is coated on the inner layer, and the injected coating solution is coated on the outer layer, so that the gradient controllability of the material is formed.
The surface modification method of the ternary cathode material provided by the invention adopts a Plasma Enhanced Chemical Vapor Deposition (PECVD) technology to prepare the coating material of the ternary cathode material of the lithium ion battery, utilizes high-energy radiation of plasma to promote element decomposition and deposit on the surface of the material, and realizes controllable deposition speed, controllable deposition coating amount, controllable deposition coating type and controllable gradient of the coating material.
Compared with the prior art, the invention has the following beneficial effects:
1. the plasma is adopted for assistance, so that the reaction temperature is reduced, and the production cost is saved;
2. the invention realizes the controllable deposition speed of the cladding metal, the controllable deposition cladding amount and the controllable deposition type, and greatly improves the production efficiency.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention.
Fig. 1 is an SEM image of an uncoated modified positive electrode material of a comparative example;
FIG. 2 is an SEM image of a coating modified ternary cathode material prepared in example 1;
FIG. 3 is an SEM image of a coating modified ternary cathode material prepared in example 2;
fig. 4 is a graph of the cycle performance of a comparative example uncoated modified ternary cathode material and the coated modified ternary cathode material prepared in example 2.
Detailed Description
The invention is described in detail below, and the description in this section is merely exemplary and explanatory and should not be construed as limiting the scope of the invention in any way. Furthermore, features from embodiments in this document and from different embodiments may be combined accordingly by a person skilled in the art from the description in this document.
The comparative example and the example of the invention adopt the same ternary cathode material LiNi0.6CoyMn0.4-yO2。
Comparative example:
the ternary cathode material is not subjected to coating modification.
Fig. 1 is an SEM image of an uncoated modified ternary positive electrode material.
Example 1:
the surface modification method of the ternary cathode material comprises the following steps:
s1, dissolving a proper amount of aluminum acetylacetonate composition in a methanol solution to prepare a coating solution; wherein the mol ratio of the ethylene acetone aluminum to the methanol is 1: 6;
s2, preparing a ternary cathode material LiNi0.6CoyMn0.4-yO2Placing the reaction furnace in a plasma reaction furnace, and introducing inert gas helium into the reaction furnace until the gas pressure in the reaction furnace is 2 Mpa; setting the frequency, power and reaction time of a plasma generator in the plasma reaction furnace; wherein the power is set to 800W;
s3, setting the furnace temperature of the plasma reaction furnace to be 200 ℃, then injecting the coating solution into the plasma reactor at a constant speed of 40ml/h, simultaneously starting the plasma generator, closing the plasma generator and the plasma reaction furnace after reacting for 5min, and obtaining the uniformly coated ternary cathode material after the reaction is finished.
Fig. 2 is an SEM image of the coating-modified ternary cathode material prepared in this example, and the coating amount is small.
Example 2:
the surface modification method of the ternary cathode material comprises the following steps:
s1, dissolving a proper amount of aluminum acetylacetonate composition in a methanol solution to prepare a coating solution; wherein the mol ratio of the ethylene acetone aluminum to the methanol is 1: 6;
s2, preparing a ternary cathode material LiNi0.6CoyMn0.4-yO2Placing the reaction furnace in a plasma reaction furnace, and introducing inert gas helium into the reaction furnace until the gas pressure in the reaction furnace is 2 Mpa; setting the frequency, power and reaction time of a plasma generator in the plasma reaction furnace; wherein the power is set to 800W;
s3, setting the furnace temperature of the plasma reaction furnace to be 300 ℃, then injecting the coating solution into the plasma reactor at a constant speed of 60ml/h, simultaneously starting the plasma generator, closing the plasma generator and the plasma reaction furnace after reacting for 10min, and obtaining the uniformly coated ternary cathode material after the reaction is finished.
Fig. 3 is an SEM image of the coating-modified ternary cathode material prepared in this example, in which the coating amount is larger than that in example 1.
The electrical properties of the uncoated modified ternary cathode material of the comparative example and the coated modified ternary cathode material described in example 2 were analyzed in comparison, and the specific results can be seen in fig. 4. The electrical property of the coated and modified ternary cathode material is obviously improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A surface modification method of a ternary cathode material is characterized in that acetylacetone metal composition solution is used as coating solution of the ternary cathode material, and surface modification of the ternary cathode material is completed in a plasma reaction furnace.
2. The surface modification method of a ternary cathode material as claimed in claim 1, comprising the steps of:
s1, preparing acetylacetone metal composition coating solution;
s2, placing the ternary cathode material in a plasma reaction furnace, and introducing inert gas into the reaction furnace; setting the frequency, power and reaction time of a plasma generator in the plasma reaction furnace;
and S3, when the furnace temperature of the plasma reaction furnace is raised to a certain temperature, according to the amount of the metal to be coated, injecting the coating solution into the plasma reactor, simultaneously starting the plasma generator, reacting for a certain time, then closing the plasma generator and the plasma reaction furnace, and obtaining the uniformly coated ternary cathode material after the reaction is finished.
3. The surface modification method of the ternary cathode material according to claim 2, wherein the solvent of the coating solution is preferably an alcohol or ether solvent.
4. The surface modification method of the ternary cathode material according to claim 2 or 3, wherein the solvent of the coating solution is preferably methanol, and the acetylacetone metal composition is preferably aluminum acetylacetonate.
5. The surface modification method of the ternary cathode material according to claim 2 or 3, wherein the molar ratio of the acetylacetone metal composition to the solvent in the coating solution is 1:5 to 1: 10.
6. The surface modification method of the ternary cathode material as claimed in claim 2, wherein the pressure of the inert gas introduced into the reaction furnace in step S2 is 1Mpa to 10 Mpa.
7. The method for modifying the surface of a ternary cathode material as claimed in claim 2, wherein in step S3, the temperature of the plasma reaction furnace is raised to 100 to 400 ℃.
8. The method for modifying the surface of a ternary cathode material as claimed in claim 2, wherein in step S3, the plasma generator is turned on and then the reaction is continued for 2-30 min.
9. The method for modifying the surface of a ternary cathode material as claimed in claim 2, wherein the injection rate of the coating solution in step S3 is 30mL/h to 100 mL/h.
10. The method for modifying the surface of a ternary positive electrode material as defined in claim 2, wherein the coating solutions of different metal elements are injected in stages.
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Application publication date: 20200904 |