CN111933929B - F-doped anode material and preparation method thereof - Google Patents
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Abstract
The invention belongs to the field of lithium ion battery electrode materials, and provides an F-doped anode material with a structural formula of LizMAO2. Also provides a preparation method of the F-doped anode material, which comprises the following steps: mixing and sintering an oxide precursor containing transition metal M and a compound containing F, and crushing to obtain a transition metal M precursor with F deposited on the surface; mixing and sintering the precursor, a lithium source and a compound of a doping element, and then crushing a coating layer by using crushing equipment to obtain a defective positive electrode material; and mixing and sintering the defective positive electrode material and the compound of the coating element, and crushing to obtain the F-doped positive electrode material. F in the F-doped anode material is a distribution form of bulk phase gradient distribution and surface enrichment state formed by depositing the surface of the precursor and sintering the anode material, so that the performances of the anode material of the lithium ion battery such as circulation, storage, floating charge and the like under high voltage can be obviously improved.
Description
Technical Field
The invention relates to an F-doped anode material and a preparation method thereof, belonging to the field of lithium ion battery electrode materials.
Background
At present, in a high-voltage development stage of the anode material, modification of elements such as Mg, Ti, Al and the like in an early material system cannot meet the requirement, more new elements are gradually modified in the development process of a higher-voltage material, and doping modification of anions and the like begins to occur in the aspect of doping and coating of the new elements.
For example, chinese patent application No. CN201780035058.1, "lithium ion battery positive electrode material, preparation method thereof, and lithium ion battery" discloses that F ions coat the surface of lithium cobaltate to improve high voltage performance. Also, for example, the chinese patent application No. CN201810660986.3, "synthesis of metal oxide and lithium ion battery", discloses that doping cobalt oxide with F, P, S, Cl, N, As, Se, Br, Te, I, and At makes anions occupy O sites, increases the number of O holes, reduces interface impedance, and stabilizes the surface crystal structure. However, patent CN201780035058.1 is only the design of surface coating layer, and patent CN210810660986.3 is more in the form of homogeneous distribution of bulk phase, and the above patent introduces anions, but cannot obtain the distribution mode of gradient distribution and surface enrichment of bulk phase.
Disclosure of Invention
The invention aims to provide an F-doped anode material and a preparation method thereof, wherein F in the F-doped anode material is deposited on the surface of a precursor, and then forms a distribution form of bulk phase gradient distribution and surface enrichment state through the sintering process of the anode material, so that the performances of the anode material of a lithium ion battery, such as circulation, storage, floating charge and the like under high voltage, can be remarkably improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
an F-doped anode material, the structural formula of which is LizMAO2(ii) a M comprises Co and at least one of Ni and Mn; a comprises F and at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y, Zr and F.
Further, M ═ Ni1-x-yMnxCoy，0≤x≤1，0＜y≤1，1＜z≤1.2。
A preparation method of an F-doped positive electrode material comprises the following steps:
(1) uniformly mixing an oxide precursor containing a transition metal M and a compound containing F, wherein the transition metal M comprises Co; sintering for 6-20 hours at 300-1000 ℃, and crushing after sintering to obtain a transition metal M precursor with F deposited on the surface, wherein the mass ratio of F is 0.01% -1%;
(2) mixing a transition metal M precursor with F deposited on the surface, a lithium source and a compound of a doping element according to the mass ratio of Li/M (1-1.2) to the doping element of 0.01-1%, wherein the doping element comprises F; sintering at 700-1100 ℃ for 5-20 hours, and crushing the coating layer by using crushing equipment after sintering to obtain a defective positive electrode material;
(3) uniformly mixing the defective positive electrode material I and a compound of a coating element according to the mass ratio of the coating element of 0.01-1%, wherein the coating element comprises F; sintering the mixture for 8 to 20 hours at 500 to 1050 ℃, and crushing the sintered mixture to obtain the F-doped anode material, wherein the structural formula of the material is LizMAO2Z is more than 1 and less than or equal to 1.2, and A comprises doping elements and coating elements.
Further, the transition metal M further includes at least one of Ni and Mn.
Further, in the steps (1) and (2), the mixing method is a dry method or a wet method.
Further, the lithium source comprises one or more of lithium carbonate, lithium oxide, lithium hydroxide and lithium acetate.
Furthermore, the doping element also comprises at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y, Zr and F.
Further, the coating element also comprises at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y, Zr and F.
Further, the compound of the doping element includes at least one of metal oxide, metal hydroxide, metal alkoxide, metal ester salt, metal nitrate, metal sulfate, and metal acetate, and preferably metal oxide and/or metal hydroxide.
Further, the compound of the coating element comprises at least one of metal oxide, metal hydroxide, metal alkoxide, metal ester salt, metal nitrate, metal sulfate and metal acetate, and preferably metal oxide and/or metal hydroxide.
Further, the structural formula LizMAO2M in (1) is Ni1-x-yMnxCoy，0≤x≤1，0＜y≤1。
The invention has the following advantages:
1. the invention provides a F-doped anode material LizMAO2The negative ion F doping is introduced, the precursor is precipitated, the mass ratio of the modified element A to the primary doping element and the secondary coating element is 0.01-1%, and the F element improves the lithium ion transmission rate and the interface stability of the material through a special distribution mode of gradient distribution and surface enrichment state, so that the electrochemical stability of the lithium ion battery anode material under high voltage is improved, and the problems of circulation, storage, floating charge and the like in the development of the high voltage material are solved.
2. The preparation method of the F-doped anode material provided by the invention is simple and convenient in operation process, low in raw material cost and easy to realize industrial production.
Drawings
Fig. 1 is a flow chart of a method for preparing an F-doped positive electrode material.
Fig. 2A-2D are SEM images of F-doped positive electrode materials prepared in examples 1-4.
Fig. 3 is a graph showing charge and discharge characteristics of the F-doped positive electrode materials prepared for examples 1 to 4 and comparative example.
Detailed Description
In order to make the technical solution of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
(1) Uniformly mixing a precursor containing cobalt oxide and an oxide containing F by a wet method, sintering for 6 hours at 1000 ℃, and crushing after sintering to obtain a transition metal precursor with F deposited on the surface, wherein the mass ratio of F is 0.01%;
(2) mixing a transition metal precursor with F deposited on the surface, lithium acetate, and oxides of doping elements Ti and F by a dry method, wherein Li/Co is 1, the mass ratio of Ti to F is 0.005%, sintering at 1100 ℃ for 5 hours, and crushing a coating layer by using crushing equipment after sintering is finished to obtain a defective positive electrode material;
(3) and uniformly mixing the defective positive electrode material with hydroxides of coating elements Mg and F by a dry method, wherein the mass ratio of Mg to F is 0.005%, sintering at 500 ℃ for 8 hours, and crushing after sintering to obtain the F-doped positive electrode material.
Example 2
(1) Uniformly mixing a precursor containing cobalt oxide, nickel oxide and manganese oxide with an oxide containing F by a wet method, sintering at 300 ℃ for 20 hours, and crushing after sintering to obtain a transition metal precursor with F deposited on the surface, wherein the mass ratio of F is 1%;
(2) mixing a transition metal precursor with F deposited on the surface, lithium carbonate, and hydroxides of doping elements Al and F by a dry method, wherein Li/(Co + Ni + Mn) is 1.06, the mass ratio of Al to F is 0.5%, sintering at 700 ℃ for 20 hours, and crushing a coating layer by using crushing equipment after sintering is finished to obtain a defective positive electrode material;
(3) and uniformly mixing the defective positive electrode material with oxides of coating elements Mg, Ti, Al and F by a dry method, wherein the mass ratio of Mg, Ti, Al and F is 0.25%, sintering at 1050 ℃ for 20 hours, and crushing after sintering to obtain the F-doped positive electrode material.
Example 3
(1) Uniformly mixing a precursor containing cobalt oxide and manganese oxide with an oxide containing F by a dry method, sintering at 700 ℃ for 16 hours, and crushing after sintering to obtain a transition metal precursor with F deposited on the surface, wherein the mass ratio of F is 0.05%;
(2) mixing a transition metal precursor with F deposited on the surface, lithium oxide and hydroxides of doping elements La, Y, Zr and F by a dry method, wherein the mass ratio of Li/(Co + Mn) is 1.08, and the mass ratio of La, Y, Zr and F is 0.05 percent respectively, sintering at 900 ℃ for 10 hours, and crushing a coating layer by using crushing equipment after sintering is finished to obtain a defective positive electrode material;
(3) and uniformly mixing the defective positive electrode material with hydroxides of coating elements La, Y, Zr and F by a dry method, wherein the mass ratio of La, Y, Zr and F is 0.01%, sintering at 900 ℃ for 10 hours, and crushing after sintering to obtain the F-doped positive electrode material.
Example 4
(1) Uniformly mixing a precursor containing cobalt oxide and nickel oxide with an oxide containing F by a dry method, sintering at 900 ℃ for 9 hours, and crushing after sintering to obtain a transition metal precursor with F deposited on the surface, wherein the mass ratio of F is 0.1%;
(2) mixing a transition metal precursor with F deposited on the surface, lithium oxide and lithium hydroxide, and sulfates doped with elements Mg, Ca, Sn, Zn and F by a wet method, wherein the mass ratio of Li/(Co + Ni) is 1.20, and the mass ratio of Mg, Ca, Sn, Zn and F is 0.01%, sintering at 1000 ℃ for 15 hours, and crushing a coating layer by using crushing equipment after sintering is finished to obtain a defective positive electrode material;
(3) and uniformly mixing the defective positive electrode material with nitrates of the coating elements of Ca, Sn, Zn and F by a dry method, wherein the mass ratio of Ca to Sn to Zn to F is 0.02%, sintering at 1000 ℃ for 15 hours, and crushing after sintering to obtain the F-doped positive electrode material.
The following comparative examples were prepared using one of the methods commonly used in the art to prepare F-doped positive electrode materials, in comparison with the above examples:
mixing an oxide containing a transition metal M, a lithium source, a compound containing F and an oxide of a doping element A according to the ratio of Li/M to 1.2, wherein the mass ratio of F is 1%, the mass ratio of A is 1%, sintering at 1100 ℃ for 20 hours, and crushing a coating layer by using crushing equipment after sintering is finished to obtain a defective positive electrode material; and uniformly mixing the defective positive electrode material I and the hydroxide of the coating element A according to the mass percentage of 1% of the modified element A, sintering at 1050 ℃ for 20 hours, and crushing after sintering to obtain the F-doped positive electrode material.
The button-type full-cell metal dissolution test was performed on the F-doped positive electrode material samples prepared in examples 1 to 4 and comparative example, and the test method was: uniformly coating the anode material, carbon black and PVDF on an aluminum foil according to the proportion of 90:5:5, forming a button type full cell with a C cathode, charging and discharging for 1 week at 4.5V and 0.2C for activation, then charging to 4.6V from 0.2C, keeping constant voltage for 4 hours, dismantling the cell in a glove box after the constant voltage is completed, digesting the cathode by acid, testing the solubility of Ni, Co and Mn (see table 1), and judging the thermal stability, the cycle performance and the like of the material according to metal dissolution data.
Table 1 metal dissolution data
| Metal dissolution | |
| Example 1 | Co40ppm |
| Example 2 | Co90ppm，Ni85ppm，Mn120ppm |
| Example 3 | Co35ppm，Mn65ppm |
| Example 4 | Co40ppm，Ni70ppm |
| Comparative example | Co200ppm，Ni210ppm，Mn220ppm |
From the comparison of the data in table 1, it can be seen that the metal dissolution of the material prepared by the method of the present invention is much lower than that of the prior art.
The above embodiments are only intended to illustrate the technical solution of the present invention, but not to limit it, and a person skilled in the art can modify the technical solution of the present invention or substitute it with an equivalent, and the protection scope of the present invention is subject to the claims.
Claims (10)
1. The F-doped anode material is characterized in that the structural formula of the anode material is LizMAO2(ii) a M comprises Co and at least one of Ni and Mn; a comprises F and at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y and Zr, wherein the F element is distributed in a gradient way and in a surface enrichment state; the F-doped anode material is prepared by a method, which comprises the following steps:
(1) uniformly mixing an oxide precursor containing a transition metal M and a compound containing F, wherein the transition metal M comprises Co and at least one of Ni and Mn; sintering for 6-20 hours at 300-1000 ℃, and crushing after sintering to obtain a transition metal M precursor with F deposited on the surface, wherein the mass ratio of F is 0.01% -1%;
(2) mixing a transition metal M precursor with F deposited on the surface, a lithium source and a compound of a doping element according to the mass ratio of Li/M (1-1.2) to the doping element of 0.01-1%, wherein the doping element comprises F; sintering at 700-1100 ℃ for 5-20 hours, and crushing the coating layer by using crushing equipment after sintering to obtain a defective positive electrode material;
(3) uniformly mixing the defective positive electrode material I and a compound of a coating element according to the mass ratio of the coating element of 0.01-1%, wherein the coating element comprises F; sintering the mixture for 8 to 20 hours at 500 to 1050 ℃, and crushing the sintered mixture to obtain the F-doped anode material, wherein the structural formula of the material is LizMAO2Z is more than 1 and less than or equal to 1.2, and A comprises doping elements and coating elements.
2. The F-doped positive electrode material of claim 1, wherein M ═ Ni1-x-yMnxCoy，0≤x≤1，0＜y≤1，1＜z≤1.2。
3. A preparation method of an F-doped positive electrode material is characterized by comprising the following steps:
(1) uniformly mixing an oxide precursor containing a transition metal M and a compound containing F, wherein the transition metal M comprises Co; sintering for 6-20 hours at 300-1000 ℃, and crushing after sintering to obtain a transition metal M precursor with F deposited on the surface, wherein the mass ratio of F is 0.01% -1%;
(2) mixing a transition metal M precursor with F deposited on the surface, a lithium source and a compound of a doping element according to the mass ratio of Li/M (1-1.2) to the doping element of 0.01-1%, wherein the doping element comprises F; sintering at 700-1100 ℃ for 5-20 hours, and crushing the coating layer by using crushing equipment after sintering to obtain a defective positive electrode material;
(3) uniformly mixing the defective positive electrode material I and a compound of a coating element according to the mass ratio of the coating element of 0.01-1%, wherein the coating element comprises F; sintering the mixture for 8 to 20 hours at 500 to 1050 ℃, and crushing the sintered mixture to obtain the F-doped anode material, wherein the structural formula of the material is LizMAO2Z is more than 1 and less than or equal to 1.2, A comprises doping elements and coating elements, and F is distributed in a gradient mode and a surface enrichment state mode.
4. The method of claim 3, wherein the transition metal M further comprises at least one of Ni and Mn.
5. The method of claim 4, wherein M ═ Ni1-x-yMnxCoy，0≤x≤1，0＜y≤1。
6. The method of claim 3, wherein the mixing in steps (1) and (2) is dry mixing or wet mixing.
7. The method of claim 3, wherein the lithium source comprises at least one of lithium carbonate, lithium oxide, lithium hydroxide, and lithium acetate.
8. The method of claim 3, wherein the doping element further comprises at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y, Zr; the coating element also comprises at least one of Mg, Ti, Al, Ca, Sn, Zn, La, Y and Zr.
9. The method of claim 8, wherein the compound of the doping element comprises at least one of a metal oxide, a metal hydroxide, a metal alkoxide, a metal ester salt, a metal nitrate, a metal sulfate, and a metal acetate.
10. The method of claim 8, wherein the compound of the coating element comprises at least one of a metal oxide, a metal hydroxide, a metal alkoxide, a metal ester salt, a metal nitrate, a metal sulfate, and a metal acetate.
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