CN110783563A - Method for improving surface structure stability of lithium ion battery anode material - Google Patents

Method for improving surface structure stability of lithium ion battery anode material Download PDF

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Publication number
CN110783563A
CN110783563A CN201910901287.8A CN201910901287A CN110783563A CN 110783563 A CN110783563 A CN 110783563A CN 201910901287 A CN201910901287 A CN 201910901287A CN 110783563 A CN110783563 A CN 110783563A
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anode material
lithium ion
ion battery
surface structure
improving
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陈龙
夏昕
李道聪
杨茂萍
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 discloses a method for improving the surface structure stability of a lithium ion battery anode material, which comprises the following steps: mixing a nickel-cobalt-manganese laminar anode material and a nano oxide, and sintering in an atmosphere to obtain a surface pre-coated anode material; and adding the pre-coated anode material into water, stirring and cleaning, and then separating and drying to obtain the lithium ion battery anode material with a stable surface structure. According to the invention, the nano oxide is used for primarily consuming free lithium on the surface of the material to enable the material to occupy part of the stable surface of the anode material, and the remaining free lithium on the surface of the material is washed and cleaned by water and then dried at low temperature, so that the precipitation of crystal lattice lithium is prevented, the pH increase of the material is prevented, the humidity tolerance of the surface of the anode material can be improved, the processing performance is improved, and the cycle stability of the anode material is improved.

Description

Method for improving surface structure stability of lithium ion battery anode material
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for improving the surface structure stability of a lithium ion battery anode material.
Background
Nickel-cobalt-manganese-based layered cathode material Li (Ni) xCo yMn zM 1-x-y-z)O 2(0.8≤x<1，0<y is less than or equal to 0.1, z is less than or equal to 0 and less than or equal to 0.1) and the high-energy system of the lithium ion power battery is mainly designed due to the characteristic of high theoretical capacity (275 mAh/g). However, as the content of nickel increases, the content of free lithium on the surface of the material increases, which leads to higher residual alkalinity of the material, and the surface structure is damaged in the repeated lithium ion deintercalation process and reacts with the electrolyte, which leads to poor cycle performance. Meanwhile, the residual alkali on the surface of the residual material can cause a serious flatulence phenomenon, and the safety performance of the full battery is seriously influenced.
The main idea for solving the problems is to stabilize the interface by doping the stable crystal lattice in the bulk phase and by reducing the surface alkali residue through water washing and coating the surface of the material. In the patent of improving the structural stability by Ni content more than 80 mol%, the water washing process adopted by the lithium-rich material in the Chinese patent with the publication number of CN104518214A is a mixed raw material process, and the result of reducing the pH value cannot be achieved. In the patent with publication number CN107394160A, after the water washing process is adopted, the material needs to be stabilized by adopting the secondary high-temperature sintering of boron element. The patent publication No. CN108807969A discloses that the washing time is controlled by adding an ethanol washing step. The patent publication No. CN108878863A fills up the surface lattice lithium loss caused by washing by secondary sintering lithium supplement after washing. The patent with publication number CN108878819A is to directly add nano-oxide in the water washing process to achieve washing and coating in one step. The prior art can realize the purposes of reducing the content of free lithium on the surface and improving the structural stability, but all relate to secondary sintering after water washing, and when the secondary sintering temperature reaches more than 450 ℃, lattice lithium is inevitably separated out, and the pH value is increased. For the layered positive electrode material Li (Ni) with higher Ni content xCo yMn zM 1-x-y-z)O 2(0.6<x<1，0<y<0.2，0≤z<0.2) and sensitive to moisture, and the high pH value can cause the material to have poor processability and severe performance degradation during the process of manufacturing the battery.
Disclosure of Invention
In view of the above, the present invention needs to provide a method for improving surface structure stability of a lithium ion battery anode material, which comprises pre-coating, washing with water, primarily consuming free lithium on the surface of the material by using a nano oxide, allowing the material to occupy a part of the surface stable surface of the anode material, washing the surface of the material with water, and drying at a low temperature, thereby preventing precipitation of lattice lithium, preventing pH increase of the material, improving humidity tolerance of the surface of the anode material, improving processability, and improving cycle stability of the anode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for improving the surface structure stability of a lithium ion battery anode material comprises the following steps:
s1, mixing the nickel-cobalt-manganese layered positive electrode material with the nano oxide, and sintering in the atmosphere to obtain a positive electrode material with a pre-coated surface;
and S2, adding the pre-coated anode material into water, stirring and cleaning, separating and drying to obtain the lithium ion battery anode material with a stable surface structure.
Further, in step S1, the chemical formula of the nickel-cobalt-manganese layered positive electrode material is Li (Ni) aCo bMn c)O 2Wherein a is more than or equal to 0.8 and less than or equal to 0.95, b is more than or equal to 0.03 and less than or equal to 0.1, and a + b + c is 1, and the nickel-cobalt-manganese hydroxide, the lithium hydroxide monohydrate and the dopant are uniformly mixed and then sintered for one time to obtain the lithium manganese oxide.
Preferably, the nickel cobalt manganese hydroxide and the lithium hydroxide monohydrate are in the range of Li: the molar ratio of (Ni + Co + Mn) is 1.03-1.09:1, and the addition amount of the dopant is 0-5000ppm relative to the nickel-cobalt-manganese layered cathode material.
Further, the dopant is an oxide of an element M, wherein the element M is at least one of B, Al, Ti and Zr.
Further, the atmosphere of the primary sintering is pure oxygen, the temperature is 730-.
Further, in step S1, the nano-oxide is at least one of zirconia and alumina, and the total addition amount of the nano-oxide is 0.2 to 0.8 wt%.
Further, in step S1, the atmosphere is pure oxygen, the sintering temperature is 500-700 ℃, and the time is 2-5 h.
Further, in step S2, the mass ratio of the water to the surface pre-coated cathode material is (1.5-2):1, the temperature of the water is 40-60 ℃, and the stirring and cleaning time is 3-5 min.
Further, in step S2, the separation is suction filtration or centrifugation.
Further, in step S2, the drying temperature is 100-200 ℃ and the drying time is 2-5 h.
Compared with the prior art, the invention has the following beneficial effects:
the method adopts two steps of pre-coating and washing, utilizes the nano oxide to pre-coat the surface of the nickel-cobalt-manganese layered anode material, primarily consumes free lithium on the surface of the material, occupies part of the stable surface of the anode material, improves the stability of the anode material and the next washing step, further removes the residual free lithium on the surface of the anode material through washing, and dries at low temperature, thereby effectively preventing crystal lattice lithium from being separated out, reducing the pH value on the surface of the material, simultaneously preventing the pH value of the material from being increased, and effectively improving the humidity tolerance on the surface of the anode material, thereby improving the processing performance of the material and improving the cycling stability of the anode material.
Drawings
FIG. 1 is a scanning electron microscope image of the cathode material without being coated and washed in example 3;
fig. 2 is a scanning electron microscope image of the surface of the positive electrode material subjected to the pre-coating and water washing treatment in example 3.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
The precursor Ni 0.8Co 0.1Mn 0.1(OH) 2And lithium hydroxide monohydrate according to the molar ratio of Li/(Ni + Co + Mn) of 1.09, taking the materials, wherein the addition amount of the doping agent is 0ppm, uniformly mixing in a high-speed mixer, and sintering at 790 ℃ for 12h in a pure oxygen atmosphere to obtain the nickel-cobalt-manganese layered anode material. Nickel cobalt manganese laminar anode material and 0.3 wt% of nano Al 2O 3Uniformly mixing, and sintering at 700 ℃ for 1h in a pure oxygen atmosphere to obtain the surface pre-coated anode material. And mixing the positive electrode material with the surface pre-coated with pure water at 60 ℃ according to the mass ratio of 1.5:1, stirring for 3min, carrying out suction filtration or centrifugation to obtain wet powder, and drying the wet powder at 200 ℃ for 2h to obtain the positive electrode material with a stable surface structure.
Example 2
The precursor Ni 0.82Co 0.12Mn 0.6(OH) 2Taking the lithium hydroxide monohydrate according to the molar ratio of Li/(Ni + Co + Mn) of 1.07, and B 2O 3And ZrO 2The addition amounts of the dopants are respectively 1000ppm and 3000ppm, and the nickel-cobalt-manganese layered anode material is obtained by uniformly mixing in a high-speed mixer and sintering at 770 ℃ for 20h in pure oxygen atmosphere. Nickel cobalt manganese laminated anode material and 0.8wt% of nano ZrO 2Uniformly mixing, and sintering at 600 ℃ for 2h in a pure oxygen atmosphere to obtain the surface pre-coated anode material. Mixing the surface pre-coated anode material with 50 ℃ pure water according to the mass ratio of 2:1, stirring for 2min, performing suction filtration or centrifugation to obtain wet powder, and drying the wet powder at 150 ℃ for 3h to obtain the anode material with stable surface structureAnd (3) a positive electrode material.
Example 3
The precursor Ni 0.85Co 0.1Mn 0.5(OH) 2Taking the mixture and lithium hydroxide monohydrate according to the molar ratio of Li/(Ni + Co + Mn) of 1.05, and taking Al 2O 3And ZrO 2The addition amounts of the dopants are respectively 1000ppm and 2000ppm, and after being uniformly mixed in a high-speed mixer, the mixture is sintered for 15 hours at 740 ℃ in a pure oxygen atmosphere to obtain the nickel-cobalt-manganese laminated cathode material (marked as a comparative sample of example 3). Nickel cobalt manganese laminar anode material, 0.3 wt% of nano Al 2O 3And 0.3 wt% of nano ZrO 2Uniformly mixing, and sintering at 550 ℃ for 3h in pure oxygen atmosphere to obtain the surface pre-coated anode material. And mixing the positive electrode material with the surface pre-coated with pure water at 45 ℃ according to a mass ratio of 2:1, stirring for 2min, carrying out suction filtration or centrifugation to obtain wet powder, and drying the wet powder at 120 ℃ for 3h to obtain the positive electrode material with a stable surface structure.
The nickel-cobalt-manganese layered positive electrode material (comparative example of example 3) and the positive electrode material with stable surface structure (example 3) in this example were exposed to 50 RH% humidity air for 20 minutes, and the surfaces thereof were observed, respectively, and fig. 1 shows that the surface of the material had a heterogeneous phase and the structure of the material was damaged, and fig. 2 shows that the surface of the material was smooth and the humidity resistance of the material was improved after the pre-coating and water washing treatment.
Example 4
The precursor Ni 0.9Co 0.06Mn 0.04(OH) 2Taking the material and lithium hydroxide monohydrate according to the molar ratio of Li/(Ni + Co + Mn) of 1.03, and taking Al 2O 3And TiO 2The addition amounts of the doping agents are 3000ppm and 1000ppm respectively, and the nickel-cobalt-manganese laminar anode material is obtained by uniformly mixing in a high-speed mixer and sintering for 15 hours at 720 ℃ in a pure oxygen atmosphere. Nickel cobalt manganese laminar anode material, 0.3 wt% of nano Al 2O 3And 0.5 wt% of nano ZrO 2Uniformly mixing, and sintering at 500 ℃ for 5h in a pure oxygen atmosphere to obtain the surface pre-coated anode material. Mixing the surface pre-coated anode material with pure water at 40 ℃ according to the mass ratio of 2:1, stirring for 2min, performing suction filtration or centrifugation to obtain wet powder, and placing the wet powder in a containerDrying for 5h at 100 ℃ to obtain the cathode material with stable surface structure.
Example 5
The precursor Ni 0.95Co 0.03Mn 0.02(OH) 2Taking the mixture and lithium hydroxide monohydrate according to the molar ratio of Li/(Ni + Co + Mn) of 1.02, and taking Al 2O 3And TiO 2The addition amounts of the dopants are 3000ppm and 5000ppm respectively, and the nickel-cobalt-manganese layered anode material is obtained by uniformly mixing in a high-speed mixer and sintering at 710 ℃ for 20h in pure oxygen atmosphere. Nickel cobalt manganese laminar anode material, 0.3 wt% of nano Al 2O 3And 0.5 wt% of nano ZrO 2Uniformly mixing, and sintering at 600 ℃ for 3h in pure oxygen atmosphere to obtain the surface pre-coated anode material. And mixing the positive electrode material with the surface pre-coated with pure water at 50 ℃ according to a mass ratio of 2:1, stirring for 2min, carrying out suction filtration or centrifugation to obtain wet powder, and drying the wet powder at 100 ℃ for 4h to obtain the positive electrode material with a stable surface structure.
Comparative example 1
The method and data in example 3 in patent publication No. CN108878819A are cited as comparative example 1, the proportion of nickel, cobalt and manganese elements in the present application is consistent with that in comparative example 1, but the types and amounts of doping elements are different, so that the capacity and rate performance are slightly different, but the pH calculated according to the residual alkali (LiOH) disclosed in CN108878819A is taken as comparison (the calculation mode is pH 12.62+ lg (percent content of LiOH)), and the comparison shows that the phenomenon that crystal lattice lithium is precipitated due to secondary burning after coating in the patent publication No. CN108878819A is avoided, and meanwhile, the phenomenon that the pH is increased back is finally controlled, so that the cycle performance can be effectively improved.
The positive electrode materials with stable surface structures obtained in examples 1 to 5 and comparative example 1 were assembled into a 2016-button cell, and tested under the conditions of 2.75 to 4.3V discharge interval and 1C theoretical capacity of 200mAh/g, and the results are shown in Table 1.
TABLE 1 electrochemical Properties of the materials of examples 1-5
Figure BDA0002211889960000051
From table 1, it can be seen that the positive electrode material with stable surface structure in the example has low pH value, high capacity and good cycle performance. In the embodiment 3 as an example, the technical features of the above embodiments may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A method for improving the surface structure stability of a lithium ion battery anode material is characterized by comprising the following steps:
s1, mixing the nickel-cobalt-manganese layered positive electrode material with the nano oxide, and sintering in the atmosphere to obtain a positive electrode material with a pre-coated surface;
and S2, adding the pre-coated anode material into water, stirring and cleaning, separating and drying to obtain the lithium ion battery anode material with a stable surface structure.
2. The method for improving the surface structure stability of the lithium ion battery cathode material according to claim 1, wherein in step S1, the chemical formula of the nickel-cobalt-manganese layered cathode material is Li (Ni) aCo bMn c)O 2Wherein a is more than or equal to 0.8 and less than or equal to 0.95, b is more than or equal to 0.03 and less than or equal to 0.1, and a + b + c =1, and the nickel-cobalt-manganese hydroxide, the lithium hydroxide monohydrate and the dopant are uniformly mixed and then are subjected to primary firingAnd (4) obtaining the finished product.
3. The method for improving the surface structure stability of the positive electrode material of the lithium ion battery according to claim 2, wherein the nickel cobalt manganese hydroxide and the lithium hydroxide monohydrate are in a ratio of Li: the molar ratio of (Ni + Co + Mn) is 1.03-1.09:1, and the addition amount of the dopant is 0-5000ppm relative to the nickel-cobalt-manganese layered cathode material.
4. The method for improving the surface structure stability of the lithium ion battery cathode material according to claim 2, wherein the dopant is an oxide of an element M, wherein the element M is at least one of B, Al, Ti and Zr.
5. The method for improving the surface structure stability of the lithium ion battery anode material as claimed in claim 2, wherein the primary sintering atmosphere is pure oxygen, the temperature is 730-790 ℃, and the time is 12-20 h.
6. The method for improving the surface structure stability of the positive electrode material of the lithium ion battery according to claim 1, wherein in step S1, the nano oxide is at least one of zirconia and alumina, and the total addition amount of the nano oxide is 0.2 to 0.8 wt%.
7. The method of claim 1, wherein in step S1, the atmosphere is pure oxygen, the sintering temperature is 500-700 ℃, and the sintering time is 2-5 h.
8. The method for improving the surface structure stability of the positive electrode material of the lithium ion battery according to claim 1, wherein in the step S2, the mass ratio of the water to the positive electrode material with the surface pre-coated is (1.5-2):1, the temperature of the water is 40-60 ℃, and the stirring and cleaning time is 3-5 min.
9. The method for improving the surface structure stability of the lithium ion battery cathode material according to claim 1, wherein the separation is suction filtration or centrifugation in step S2.
10. The method as claimed in claim 1, wherein the step S2, the drying temperature is 100-200 ℃ and the drying time is 2-5 h.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103872328A (en) * 2014-03-12 2014-06-18 南通瑞翔新材料有限公司 Positive electrode active material for lithium ion secondary battery and preparation method for positive electrode active material
CN107394160A (en) * 2017-07-24 2017-11-24 合肥国轩高科动力能源有限公司 A kind of anode material for lithium-ion batteries and preparation method thereof
CN110137488A (en) * 2019-05-28 2019-08-16 郑州中科新兴产业技术研究院 A kind of nickelic positive electrode of secondary lithium batteries and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103872328A (en) * 2014-03-12 2014-06-18 南通瑞翔新材料有限公司 Positive electrode active material for lithium ion secondary battery and preparation method for positive electrode active material
CN107394160A (en) * 2017-07-24 2017-11-24 合肥国轩高科动力能源有限公司 A kind of anode material for lithium-ion batteries and preparation method thereof
CN110137488A (en) * 2019-05-28 2019-08-16 郑州中科新兴产业技术研究院 A kind of nickelic positive electrode of secondary lithium batteries and preparation method thereof

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Application publication date: 20200211