CN111689527A - Preparation method of one-pot double-coated lithium ion battery NCM ternary cathode material - Google Patents
Preparation method of one-pot double-coated lithium ion battery NCM ternary cathode material Download PDFInfo
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- 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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Abstract
The invention provides a method for double-coating a lithium ion battery NCM ternary cathode material by a one-pot method, which comprises the steps of adding raw materials, and sequentially coating an oxide and a conductive polymer on the surface of the ternary material by the one-pot method by utilizing the difference between the hydrolysis speed of an organic metal compound and the polymerization speed of the polymer so as to obtain the NCM ternary cathode material with high electrochemical performance. The invention utilizes oxide coating to stabilize the interface of the ternary material and facilitate the transmission of lithium ions, and the conductive polymer or carbon material facilitates the electron transmission, thereby not only improving the capacity of the material, but also improving the safety and stability of the material, and the invention has simple and convenient process and is easy to popularize in a large range.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a preparation method of a one-pot double-coated lithium ion battery NCM ternary cathode material.
Background
As one of the rechargeable energy storage devices, lithium ion batteries are one of the main driving forces for promoting the development of the global electric industry, especially the electric automobile market. In order to partially or completely replace fossil energy sources in the future, lithium ion batteries with the lightest metal ions and the largest energy density are the best choice. However, there is still a long way to obtain a lithium ion battery system with high energy density and power, and safety and environmental protection. The focus of current development is on how to obtain stable electrodes and electrode-electrolyte interfaces.
Unlike the conventional lithium ion battery positive electrode materials Lithium Cobaltate (LCO) and lithium iron phosphate (LFP), the layered ternary Nickel Cobalt Manganese (NCM) positive electrode material exhibits a higher specific capacity, wherein the NCM material also faces higher safety and risk of capacity fading with the increase of the Ni ion ratio as a major capacity contribution. In view of the above problems, it is a main solution to coat a stable nanomaterial on the surface of a positive electrode to reduce the side reactions caused by direct contact between electrolyte and the positive electrode material, and the most commonly used coating agents are metal oxides, phosphates, and fluorides, while the most commonly used and inexpensive carbon materials with stable structure are rarely mentioned, mainly because the carbon reacts with 4-valent manganese to destroy the layered structure at high temperature through reduction.
The invention provides a feasible carbon-coated NCM ternary positive electrode method, which not only improves the capacity of the material, but also improves the safety and stability of the material.
Disclosure of Invention
The invention provides a method for double-coating a lithium ion battery NCM ternary positive electrode material by a one-pot method, and aims to obtain a method for coating a carbon-coated NCM ternary positive electrode, which can improve the capacity of the material and the safety and stability of the material.
In order to achieve the aim, the invention provides a preparation method of a one-pot double-coated lithium ion battery NCM ternary cathode material, which comprises the following steps:
dispersing an NCM ternary positive electrode material in an ethanol solution; or dispersing the NCM ternary cathode material in a surfactant solution;
selecting an oxide coating layer, adding a conductive polymer material and an organic metal compound corresponding to the oxide coating layer into the mixed solution obtained in the step one while stirring, and uniformly stirring until the reaction is complete to obtain a mixed solution;
and step three, filtering the mixture obtained in the step two to obtain a primary material, and drying or sintering the primary material to obtain the lithium ion battery NCM ternary cathode material.
Preferably, the NCM ternary cathode material in the first step is Li (Ni)xCoyMn1-x-y)O2Wherein x is more than or equal to 0.3 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.5.
Preferably, the concentration of the ethanol solution in the first step is 30-70%; the surfactant is CTAB or PVP, and the concentration of the surfactant solution is 0.5-2%.
Preferably, the conductive polymer material in the second step includes one or more of dopamine, polysaccharides, resins and conductive polymers.
Preferably, the concentration of the conductive polymer solution in the second step is 0.02mol/L-0.08mol/L, and the mass ratio of the NCM ternary cathode material to the polymer is 1: 0.02-0.1.
Preferably, the stirring speed when the conductive polymer material is added simultaneously in the step two while stirring is 300-.
Preferably, the oxide coating layer in the second step includes Al2O3，TiO2，MgO，SiO2，ZrO2，V2O5，Nb2O5，ZnO，MoO3And Y2O3。
Preferably, the organometallic compound in the second step includes alcohols, esters and saccharides.
Preferably, the drying in the third step comprises the following specific operations: dispersing the material by filtering, and then drying in an oven at the temperature of 100-120 ℃ for 5-10h to obtain the lithium ion battery NCM ternary positive electrode material with a metal oxide coating layer and a polymer coating; the sintering operation is to carry out calcination in an inert atmosphere, wherein the calcination temperature is 300-800 ℃, and the calcination time is 2-12 h.
The method realizes double coating of the oxide polymer of the NCM ternary positive electrode by a one-pot method. Coating metal oxide and polymer on the surface of the NCM ternary cathode material in sequence by using the difference between the hydrolysis speed of the organic metal compound and the polymerization speed of the polymer in a one-pot method; the coating of the metal oxide not only stabilizes the interface of the ternary material, but also is beneficial to the transmission of lithium ions, and the carbon material is beneficial to the electron transmission. The method can select different coatings according to the characteristics of different ternary materials, thereby obtaining the NCM ternary cathode material with high electrochemical performance. The polymer in the invention can be selected from dopamine, polysaccharides, resins, conductive polymers and the like to obtain polymer layers with different structures and different element dopings, the amount range of the polymer is 0.2-1 g (the carbon content accounts for 1 per thousand-10% of the total mass), the polymer layers with different thicknesses are obtained, the amount of the polymer is too small, the coating cannot be uniform, and the polymer layer is too thick to influence the capacity of the material if the amount of the polymer is too large.
The scheme of the invention has the following beneficial effects:
(1) according to the invention, the NCM ternary anode is coated in a double-coating manner by a one-pot method, the oxide coating stabilizes the interface of the ternary material and is beneficial to the transmission of lithium ions, and the carbon material is beneficial to the electron transmission and can effectively improve the electrochemical performance of the NCM ternary anode.
(2) The method can use the carbon material as the coating layer of the lithium battery, the carbon material has stable structure and low price, and the economic benefit can be effectively improved.
(3) The method can realize double-layer coating of the oxide and the polymer in one step, is quick, simple and convenient, can greatly shorten the preparation time, and improves the economic benefit of enterprises.
Drawings
FIG. 1 shows a ternary positive electrode material Li (Ni) for NCM in example 1 before carbon coating0.5Co0.2Mn0.3)O2SEM image of
FIG. 2 shows a carbon-coated NCM ternary positive electrode material Li (Ni) in example 10.5Co0.2Mn0.3)O2SEM picture of (1);
FIG. 3 shows a carbon-coated NCM ternary positive electrode material Li (Ni) in example 10.5Co0.2Mn0.3)O2A TEM image of (B);
fig. 4 is a graph comparing cell data before and after carbon coating in example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides a method for double-coating a lithium ion battery NCM ternary cathode material by a one-pot method aiming at the existing problems.
Example 1
Step one, 1g of Li (Ni) before coating0.5Co0.2Mn0.3)O2(shown in figure 1) is dispersed in a mixed solvent of 140ml of water and 60ml of ethanol;
step two, TiO is selected2As an oxide coating layer, 0.64g of resorcinol, 0.96ml of formaldehyde, 0.64ml of ethylenediamine, 3ml of ammonia water and 0.3ml of tetrabutyl titanate are slowly added in this order at a speed of 300r/min with stirring, stirred for 6 hours, and then the mixture C is added under an alkaline environment16H36O4Hydrolysis of Ti to form nano TiO2The layer is coated on the surface of the ternary material, resorcinol, formaldehyde and ethylenediamine are polymerized to form Polybenzoxazine (PB) polymer coated on TiO2A surface;
step three, dispersing the filtered material, and then putting the dispersed material into a 120 ℃ oven for drying for 10 hours to obtain the product with TiO2And polybenzoxazine PB coated Li (Ni)0.5Co0.2Mn0.3)O2And (3) a positive electrode material.
As shown in fig. 2 and 3, when the SEM image and TEM coating are coated on the surface of the material, the coated material also shows higher specific capacity, which is close to 160mAh/g at 0.2C current density, which is 5mAh/g more than the capacity before coating, and is at the leading level of the same proportion of material.
Example 2
Step one, 1gLi (Ni)0.8Co0.1Mn0.1)O2Dispersing in 140ml of mixed solvent of water and 60ml of ethanol;
selecting Al2O3As an oxide coating layer, 0.64g of ammonium persulfate, 1ml of pyrrole and 0.3g of aluminum isopropoxide are slowly added in turn at the speed of 600r/min while stirring, the stirring is carried out for 10 hours, and the aluminum isopropoxide is hydrolyzed to form nano Al2O3The layer is coated on the surface of the ternary material, and the pyrrole forms polypyrrole under the action of ammonium persulfate to coat Al2O3A surface;
step three, dispersing the filtered material, and then putting the dispersed material into a 100 ℃ oven for drying for 5 hours to obtain Al2O3And polypyrrole coated Li (Ni)0.8Co0.1Mn0.1)O2And (3) a positive electrode material.
Table one: carbon-coated Li (Ni)08Co01Mn01)O2Comparison of before and after data
As shown in Table one, carbon-coated Li (Ni)0.8Co0.1Mn0.1)O2The specific capacity is obviously improved, the surface residual alkali capacity is greatly reduced, and the stability is greatly improved.
Example 3
Step one, 1g of Li (Ni)0.8Co0.1Mn0.1)O2Dispersing in a mixed solvent of 120ml of water and 60ml of ethanol;
selecting SiO2As an oxide coating layer, the coating layer was continued at 500r/mSlowly adding 0.5g of dopamine hydrochloride and 3ml of tetraethyl orthosilicate in turn at the speed of in while stirring, stirring for 10 hours, and hydrolyzing the tetraethyl orthosilicate to form nano SiO2The layer is coated on the surface of the ternary material, and dopamine hydrochloride forms polydopamine coated SiO under the alkaline condition2A surface;
step three, dispersing the filtered material, and then putting the dispersed material into a 100 ℃ oven for drying for 5 hours to obtain the material with SiO2And polydopamine coated Li (Ni)0.8Co0.1Mn0.1)O2And (3) a positive electrode material.
Example 4
Step one, 1g of Li (Ni)0.8Co0.1Mn0.1)O2Dispersing in a mixed solvent of 80ml of water and 60ml of ethanol;
step two, selecting MgO as an oxide coating, slowly adding 0.3g of resorcinol, 0.4ml of formaldehyde and 0.5g of magnesium ethoxide in turn at the speed of 800r/min while stirring, stirring for 10h, and hydrolyzing the magnesium ethoxide to form Mg (OH)2The layer is coated on the surface of the ternary material, the pyrrole forms polypyrrole under the action of ammonium persulfate and is coated on Mg (OH)2A surface;
step three, dispersing the filtered material, putting the dispersed material into a 100 ℃ oven for drying for 5h, then putting the dried material into a furnace for sintering for 4h at 500 ℃, and putting the sintered material into a Mg (OH)2Decomposing into MgO, decomposing the phenolic resin into carbon, and finally obtaining Li (Ni) with MgO and carbon coating0.8Co0.1Mn0.1)O2And (3) a positive electrode material.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A preparation method of a one-pot double-coated lithium ion battery NCM ternary cathode material is characterized by comprising the following steps:
dispersing an NCM ternary positive electrode material in an ethanol solution; or dispersing the NCM ternary cathode material in a surfactant solution;
selecting an oxide coating layer, adding a conductive polymer material and an organic metal compound corresponding to the oxide coating layer into the mixed solution obtained in the step one while stirring, and uniformly stirring until the reaction is complete to obtain a mixed solution;
and step three, filtering the mixture obtained in the step two to obtain a primary material, and drying or sintering the primary material to obtain the lithium ion battery NCM ternary cathode material.
2. The method according to claim 1, wherein the NCM ternary positive electrode material in the first step is Li (Ni)xCoyMn1-x-y)O2Wherein x is more than or equal to 0.3 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.5.
3. The preparation method according to claim 1, wherein the concentration of the ethanol solution in the first step is 30-70%; the surfactant is CTAB or PVP, and the concentration of the surfactant solution is 0.5-2%.
4. The method according to claim 1, wherein the conductive polymer material in the second step includes one or more of dopamine, polysaccharides, resins, and conductive polymers.
5. The preparation method according to claim 1, wherein the concentration of the conductive polymer solution in the second step is 0.02mol/L to 0.08mol/L, and the mass ratio of the NCM ternary cathode material to the polymer is 1:0.02 to 0.1.
6. The method as claimed in claim 1, wherein the stirring speed in step two is 300-600r/min for 5-10 h.
7. The method according to claim 1, wherein the oxide coating layer in the second step comprises Al2O3，TiO2，MgO，SiO2，ZrO2，V2O5，Nb2O5，ZnO，MoO3And Y2O3。
8. The method according to claim 1, wherein the organometallic compound in the second step includes alcohols, esters and saccharides.
9. The preparation method according to claim 1, wherein the drying in the third step comprises the following specific operations: dispersing the material by filtering, and then drying in an oven at the temperature of 100-120 ℃ for 5-10h to obtain the lithium ion battery NCM ternary positive electrode material with a metal oxide coating layer and a polymer coating; the sintering operation is to carry out calcination in an inert atmosphere, wherein the calcination temperature is 300-800 ℃, and the time is 2-12 h.
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| CN112436121A (en) * | 2020-11-24 | 2021-03-02 | 上海华谊（集团）公司 | Composite material with core-shell structure and preparation method thereof |
| CN112599779A (en) * | 2020-12-15 | 2021-04-02 | 上海华谊（集团）公司 | Double-layer coated lithium ion battery anode material and preparation method thereof |
| CN112864368A (en) * | 2021-03-18 | 2021-05-28 | 贵州梅岭电源有限公司 | Preparation method of composite coated modified lithium manganese iron phosphate cathode material |
| CN113140715A (en) * | 2021-04-12 | 2021-07-20 | 广东佳纳能源科技有限公司 | Composite cathode material, preparation method thereof and lithium ion battery |
| CN113571693A (en) * | 2021-07-30 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Modified ternary positive electrode material precursor of lithium ion battery and preparation method thereof |
| CN114256461A (en) * | 2020-09-24 | 2022-03-29 | 比亚迪股份有限公司 | Lithium ion battery positive electrode material, preparation method and lithium ion battery |
| CN114256457A (en) * | 2021-12-31 | 2022-03-29 | 国联汽车动力电池研究院有限责任公司 | Lithium-rich manganese-based positive electrode material with homogeneous composite coating layer and preparation method thereof |
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| CN112436121A (en) * | 2020-11-24 | 2021-03-02 | 上海华谊（集团）公司 | Composite material with core-shell structure and preparation method thereof |
| CN112436121B (en) * | 2020-11-24 | 2023-01-31 | 上海华谊（集团）公司 | Composite material with core-shell structure and preparation method thereof |
| CN112599779A (en) * | 2020-12-15 | 2021-04-02 | 上海华谊（集团）公司 | Double-layer coated lithium ion battery anode material and preparation method thereof |
| CN112864368A (en) * | 2021-03-18 | 2021-05-28 | 贵州梅岭电源有限公司 | Preparation method of composite coated modified lithium manganese iron phosphate cathode material |
| CN113140715A (en) * | 2021-04-12 | 2021-07-20 | 广东佳纳能源科技有限公司 | Composite cathode material, preparation method thereof and lithium ion battery |
| CN113140715B (en) * | 2021-04-12 | 2022-08-26 | 广东佳纳能源科技有限公司 | Composite cathode material, preparation method thereof and lithium ion battery |
| CN113571693A (en) * | 2021-07-30 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Modified ternary positive electrode material precursor of lithium ion battery and preparation method thereof |
| CN114256457A (en) * | 2021-12-31 | 2022-03-29 | 国联汽车动力电池研究院有限责任公司 | Lithium-rich manganese-based positive electrode material with homogeneous composite coating layer and preparation method thereof |
| CN114256457B (en) * | 2021-12-31 | 2023-12-05 | 国联汽车动力电池研究院有限责任公司 | Lithium-rich manganese-based positive electrode material with homogeneous composite coating layer and preparation method thereof |
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Application publication date: 20200922 |