CN108091852B - Molybdenum trioxide coated lithium ion battery positive electrode material and preparation method thereof - Google Patents
Molybdenum trioxide coated lithium ion battery positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a molybdenum trioxide coated lithium ion battery anode material and a preparation method thereof. The core is made of single or doped modified ternary materials such as lithium cobaltate, lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate, lithium manganate, lithium iron phosphate and the like, and the coating layer is molybdenum trioxide. The preparation process method of the composite lithium ion battery anode material disclosed by the invention is simple, controllable in process and convenient for industrial production.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a molybdenum trioxide coated lithium ion battery anode material and a preparation method thereof.
Background
With the rapid development of new energy automobiles, the lithium ion battery industry has entered a rapid development stage. The key materials influencing the performance of the lithium ion battery mainly comprise a positive electrode material, a negative electrode material, electrolyte and the like. The positive electrode material is a main factor which currently limits the performance of the battery and also a main factor which accounts for the higher cost of the lithium ion battery, and is close to 40%.
At present, the anode material mainly comprises lithium cobaltate, lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate ternary material, lithium manganate, lithium iron phosphate and the like, but the materials have respective defects, such as high price of lithium cobaltate, poor overcharge resistance and limited capacity exertion under low voltage; the lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate ternary material has the problems of low compaction density, poor compatibility with electrolyte, gas expansion and the like; the high-temperature cycle and high-temperature storage performance of lithium manganate are poor; lithium iron phosphate has the problems of poor low-temperature performance and the like. In order to solve these problems, the surface coating technique is the most common and effective improvement means, and can improve the surface structure stability of the positive electrode material and improve the cycle performance of the battery under high voltage. Many documents and patents are reported at home and abroad about coating modification, but certain problems still exist in the coating mode and the selection of a coating object, and the uniformity, gram capacity, discharge voltage platform and the like of the material are influenced.
Therefore, a more uniform coating mode is designed, and a proper coating object is selected, so that the lithium ion battery cathode material with more excellent performance can be obtained.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a molybdenum trioxide coated lithium ion battery cathode material and a preparation method thereof. The core is made of single or doped modified ternary materials such as lithium cobaltate, lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate, lithium manganate, lithium iron phosphate and the like, and the coating layer is molybdenum trioxide.
The composite oxide particle inner core at least comprises lithium and one or more of nickel, cobalt and manganese, and has an average composition expressed by the following chemical formula: lixNiaCobMncM1-a-b-cO2Or LixFedM1-dPO4(ii) a Wherein M represents at least one element selected from Mn, Cr, Co, Ni, V, Ti, Al, Ga, Nb and Mg, and a is 0. ltoreq. a.ltoreq.1, b is 0. ltoreq. b.ltoreq.1, c is 0. ltoreq. c.ltoreq.1, d is 0. ltoreq. d.ltoreq.1, and x is 0.4. ltoreq. x.ltoreq.1.5. The coating layer is molybdenum trioxide and covers at least a part of the surface of the composite oxide particle.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a molybdenum trioxide coated lithium ion battery anode material, which comprises the following steps:
(1) placing the composite oxide particles at the tail end of the tube furnace, close to the air outlet;
(2) placing a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment under protective atmosphere at 600-1200 ℃, and preserving heat for 0.5-48 h;
(3) controlling the gas flow and the position of the composite oxide particles to coat the surface with molybdenum trioxide to obtain the final product.
According to the invention, the high-temperature sublimation characteristic of molybdenum trioxide is skillfully utilized, the molybdenum trioxide is deposited on the surface of the composite oxide particles in the low-temperature area, the coating is uniform, the process is controllable, the molybdenum trioxide coated lithium ion battery anode material is obtained, and the electrochemical performance of the material is improved.
According to the present invention, the molybdenum trioxide in the step (2) may be a molybdenum trioxide particle, a molybdenum trioxide solution, or a material that generates molybdenum trioxide by thermal decomposition, such as ammonium molybdate, sodium molybdate, and the like, and the present invention is not particularly limited.
According to the invention, the protective atmosphere in step (2) is any one or a combination of at least two of nitrogen, argon or helium, and for example, may be any one of nitrogen, argon or helium; typical but non-limiting combinations are: nitrogen and argon; argon and helium; nitrogen and helium; nitrogen, argon, helium, and the like, are not exhaustive for purposes of space and simplicity.
According to the present invention, the heat treatment temperature in step (2) is 600-.
The heat treatment temperature in the step (2) of the invention is preferably 700 ℃ to 1000 DEG C
According to the present invention, the heat treatment time in step (2) is 0.5-48h, for example, 0.5h, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 3h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h, 29h, 30h, 31h, 32h, 33h, 34h, 35h, 36h, 37h, 38h, 39h, 40h, 41h, 42h, 43h, 44h, 45h, 46h, 47h or 48h, and specific values therebetween are limited to the order of brevity and the present invention is not limited to the list.
The heat treatment time in the step (2) of the present invention is preferably 2 to 10 hours.
According to the invention, the heating rate of the heat treatment in step (2) is 1-30 ℃/min, for example, 1 ℃/min, 3 ℃/min, 6 ℃/min, 10 ℃/min, 12 ℃/min, 15 ℃/min, 18 ℃/min, 20 ℃/min, 23 ℃/min, 26 ℃/min or 30 ℃/min, and the specific values therebetween are limited to space and for the sake of brevity, and the invention is not exhaustive.
According to the invention, the mass ratio of the coating layer molybdenum trioxide to the composite oxide particle inner core is (0.0001-0.5): 1, for example, can be 0.0001:1, 0.0003:1, 0.0005:1, 0.0007:1, 0.001:1, 0.003:1, 0.005:1, 0.007:1, 0.01:1, 0.03:1, 0.05:1, 0.07:1, 0.1:1, 0.3:1, or 0.5:1, and specific values therebetween, limited to space and for brevity, are not exhaustive.
According to the invention, the composite oxide core is ternary material such as lithium cobaltate, lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate, lithium manganate, lithium iron phosphate or doped modified substance of the above materials, and the particle size is preferably 1-20 μm.
According to the present invention, the amount of gas flow and the position of the composite oxide particles are not particularly limited depending on the length and diameter of the tube furnace, and it is preferable that the amount of gas flow is lower than the sublimation temperature of molybdenum trioxide so that molybdenum trioxide can be deposited on the surface of the composite oxide particles.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the invention, molybdenum trioxide is coated on the surface of the composite oxide particles in a deposition mode, and the coating layer is uniform and continuous in thickness.
(2) The molybdenum trioxide has the advantages of good chemical stability and the like, can generate a layer of uniform protective film on the surface of the composite oxide, can isolate electrolyte and active substances, reduces the occurrence of side reactions, and avoids the decomposition of the electrolyte under higher voltage. Therefore, the obtained cathode material can still keep better cycle stability and capacity retention rate under higher voltage, and has excellent high-temperature storage and low-temperature performance.
Detailed Description
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Typical but non-limiting examples of the invention are as follows:
example 1
(1) Placing 20g of lithium nickelate particles at the tail end of the tube furnace, close to the position of an air outlet;
(2) putting a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment at 1200 ℃ in a nitrogen atmosphere, and preserving heat for 4 hours; (ii) a
(3) Controlling the gas flow and the position of the lithium nickelate particles to coat the surface with molybdenum trioxide to obtain a final product, wherein the mass ratio of the molybdenum trioxide to the inner core of the lithium nickelate particles is 0.2: 1.
the obtained composite material is used as a lithium ion battery anode material for electrochemical performance test, and the pole piece ratio is as follows: acetylene black: PVDF 90:5: 5. And preparing the CR2025 button cell by taking a lithium sheet as a reference electrode. Under the voltage window of 2.5-4.2V and the current density of 0.1C, the first cyclic discharge specific capacity is 205mAh/g, and the capacity retention rate of 200 cycles is 90%.
Example 2
(1) 3g of lithium iron phosphate particles are placed at the tail end of the tubular furnace and close to the air outlet;
(2) placing a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment at 800 ℃ under the argon atmosphere, and preserving heat for 48 hours;
(3) controlling the gas flow and the position of the lithium iron phosphate particles to coat the surface with molybdenum trioxide to obtain a final product, wherein the mass ratio of the molybdenum trioxide to the lithium iron phosphate particle cores is 0.0001: 1.
the obtained composite material is used as a lithium ion battery anode material for electrochemical performance test, and the pole piece ratio is as follows: acetylene black: PVDF 90:5: 5. And preparing the CR2025 button cell by taking a lithium sheet as a reference electrode. Under the voltage window of 2.5-3.9V and the current density of 0.1C, the first cyclic discharge specific capacity is 152mAh/g, and the capacity retention rate of 200 cycles is 93%. .
Example 3
(1) Placing 0.5g of lithium nickel cobalt aluminate particles at the end of the tube furnace, close to the gas outlet;
(2) placing a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment under the atmosphere of helium at 600 ℃, and keeping the temperature for 0.5h, wherein the mass ratio of the molybdenum trioxide to the nickel cobalt lithium aluminate particle inner core is 0.5: 1;
(3) controlling the gas flow and the position of the nickel cobalt lithium aluminate particles to coat the surface of the molybdenum trioxide to obtain the final product.
The obtained composite material is used as a lithium ion battery anode material for electrochemical performance test, and the pole piece ratio is as follows: acetylene black: PVDF 90:5: 5. And preparing the CR2025 button cell by taking a lithium sheet as a reference electrode. Under the voltage window of 2.5-4.2V and the current density of 0.1C, the first cyclic discharge specific capacity is 185mAh/g, and the capacity retention rate of 200 cycles is 92%.
Example 4
(1) Placing 10g of nickel cobalt lithium manganate particles at the tail end of a tube furnace, and placing the nickel cobalt lithium manganate particles close to a gas outlet;
(2) placing a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment at 700 ℃ in a mixed atmosphere of nitrogen and argon, and preserving heat for 5 hours;
(3) controlling the gas flow and the position of the nickel cobalt lithium manganate particles, and coating molybdenum trioxide on the surface to obtain a final product, wherein the mass ratio of the molybdenum trioxide to the nickel cobalt lithium manganate particle cores is 0.5: 1.
the obtained composite material is used as a lithium ion battery anode material for electrochemical performance test, and the pole piece ratio is as follows: acetylene black: PVDF 90:5: 5. And preparing the CR2025 button cell by taking a lithium sheet as a reference electrode. Under the voltage window of 2.5-4.2V and the current density of 0.1C, the first cyclic discharge specific capacity is 175mAh/g, and the capacity retention rate of 200 cycles is 91%.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (6)
1. A preparation method of a molybdenum trioxide coated lithium ion battery anode material is characterized by comprising the following steps:
(1) placing the composite oxide particles at the tail end of the tube furnace, close to the air outlet;
(2) placing a certain amount of molybdenum trioxide in a constant-temperature area of a tubular furnace, carrying out heat treatment under protective atmosphere at 600-1200 ℃, and preserving heat for 0.5-48 h;
(3) controlling the gas flow and the position of the composite oxide particles to coat the surface with molybdenum trioxide to obtain a final product, namely the molybdenum trioxide coated lithium ion battery anode material;
the positive electrode material includes: a composite oxide particle core and a coating layer;
(1) the composite oxide particle inner core at least comprises lithium and one or more of nickel, cobalt and manganese, and has an average composition expressed by the following chemical formula: lixNiaCobMncM1-a-b-cO2Or LixFedM1-dPO4(ii) a Wherein M represents at least one element selected from Mn, Cr, Co, Ni, V, Ti, Al, Ga, Nb and Mg, and a is 0-1, b is 0-1, c is 0-1, d is 0-1, x is 0.4-1.5;
(2) the coating layer is molybdenum trioxide and covers at least a part of the surface of the composite oxide particle.
2. The method of claim 1, wherein the protective atmosphere in step (2) is any one of nitrogen, argon or helium or a combination of at least two thereof.
3. The method according to claim 1, wherein the mass ratio of the coating layer of molybdenum trioxide to the composite oxide particle core is (0.0001 to 0.5): 1.
4. the method according to claim 1, wherein the composite oxide core is lithium cobaltate, lithium nickel cobalt manganese oxide, lithium nickel cobalt aluminate, layered lithium manganese oxide, lithium iron phosphate.
5. The method according to claim 1, wherein the composite oxide core has a particle size of 1 to 20 μm.
6. The molybdenum trioxide coated lithium ion battery cathode material prepared by the preparation method according to any one of claims 1 to 5.
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| CN108682839B (en) * | 2018-06-05 | 2021-04-02 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material and preparation method thereof |
| CN110120513A (en) * | 2019-05-24 | 2019-08-13 | 哈尔滨理工大学 | A method of nickle cobalt lithium manganate/molybdenum oxide spheric electrode material is prepared using atomic vapor deposition technology |
| CN110783538B (en) * | 2019-09-22 | 2022-08-02 | 英德市科恒新能源科技有限公司 | Ternary positive electrode material of lithium battery with metal oxide coated in gas phase and preparation method thereof |
| CN113054168B (en) * | 2019-12-28 | 2022-06-03 | 巴斯夫杉杉电池材料有限公司 | Tungsten-molybdenum composite coated ternary cathode material and preparation method thereof |
| CN112701261A (en) * | 2020-12-25 | 2021-04-23 | 清远道动新材料科技有限公司 | MoO (MoO)3Coated high-nickel ternary positive electrode material and preparation method thereof |
| KR20220132983A (en) * | 2021-03-24 | 2022-10-04 | 현대자동차주식회사 | Positive electrode material for lithium secondary battery and Lithium secondary batteries comprising the same |
| 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 |
| CN114361441A (en) * | 2022-01-07 | 2022-04-15 | 江苏大学 | Preparation method of in-situ coated single crystal high-nickel ternary cathode material |
| CN115304108B (en) * | 2022-07-13 | 2023-10-27 | 合肥国轩电池材料有限公司 | Preparation method and device of tungsten-coated ternary cathode material |
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| CN103956476A (en) * | 2014-03-20 | 2014-07-30 | 中国科学院长春应用化学研究所 | Surface-modified lithium-rich manganese material and its preparation method and use in lithium ion battery |
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