CN104979553B - Preparation method of core-shell structure nickel cobalt lithium aluminate material - Google Patents
Preparation method of core-shell structure nickel cobalt lithium aluminate material Download PDFInfo
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- CN104979553B CN104979553B CN201410137884.5A CN201410137884A CN104979553B CN 104979553 B CN104979553 B CN 104979553B CN 201410137884 A CN201410137884 A CN 201410137884A CN 104979553 B CN104979553 B CN 104979553B
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Abstract
The invention relates to a preparation method of a nickel-cobalt-aluminum material with a core-shell structure, belonging to the technical field of application of a lithium ion battery anode material, wherein the core-shell structure material is divided into two layers, wherein the core part of an inner layer is as follows: LiNiCo 1-a-bAlbO2, wherein (a is more than 0.7, 0.05 is more than or equal to b and more than or equal to 0, 1 is more than a + b), the molecular formula of the shell part is LiNiCo 1-c-dAldO2, wherein (c is more than 0.5, 0.5 is more than d and more than 0, and 1 is more than c + d). In order to ensure that the two materials have consistent crystal forms and compact structures in the crystallization process, the invention uses two alkali solutions as precipitating agents, and simultaneously uses a solubility gradient method in the alkali solution alternating process to ensure that the core-shell structure material has consistent crystal forms, high crystallinity and no obvious core-shell interface. Compared with the common homogeneous phase material, the nickel-cobalt lithium aluminate material prepared by the method provided by the invention has the advantages that the high capacity is kept, the cycle stability and the thermal stability of the material are effectively improved, the gas expansion rate of the material is obviously reduced, the cost performance advantage is higher, and the nickel-cobalt lithium aluminate material is more suitable for being applied to power batteries.
Description
Technical Field
the invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a high-specific-capacity anode material for a lithium ion battery and a preparation method thereof.
background
At present, lithium ion batteries are widely applied to various mobile electric appliances, such as mobile phones, cameras, notebook computers and the like, and along with the continuous increase of the power consumption of portable equipment, the demand of battery manufacturers for lithium ion secondary batteries with smaller volume, lighter weight, higher specific capacity and better safety performance is continuously increased. At present, the NCA material is more and more paid attention by battery manufacturers at home and abroad as a high-specific energy material, and the application of the material also enters the application field of the anode material of the power battery of the electric vehicle from the field of portable batteries. However, the material has high nickel content, and the high-valence nickel on the surface of the material generates a great amount of gas through oxidation-reduction reaction with electrolyte in the charging and discharging processes, so that the application of the NCA material is severely restricted, and the material also has the defects of poor overcharge resistance, poor thermal stability and the like.
At present, the preparation methods of nickel-cobalt-aluminum materials mainly comprise solid-phase synthesis and liquid-phase synthesis. The solid phase synthesis method generally mixes nickel, cobalt and aluminum compounds with lithium source compounds and then sinters the mixture, but the solid mixing mode cannot achieve the uniformity of atomic level, and the performance is difficult to give full play; although the liquid phase method can solve the problem, the process is complex, the performance is poor and the yield is low.
Disclosure of Invention
The method provided by the invention is to nucleocapsid the NCA material, so that the nucleocapsid structural material is divided into two layers, wherein the core part of the inner layer is a material with higher nickel content and lower aluminum content, and the molecular formula is as follows: LiNiCo 1-a-bAlbO2, wherein (a is more than 0.7, 0.05 is more than or equal to b and more than or equal to 0, 1 is more than a + b), the shell part is a material with higher aluminum content and lower nickel content, and the molecular formula is LiNiCo 1-c-dAldO2, wherein (c is more than 0.5, 0.5 is more than d and more than 0, and 1 is more than c + d). The two alkali solutions are used for coprecipitation reaction, and a concentration gradient method is used when the alkali solutions are alternated to ensure that crystal forms of two core-shell parts of the material are not changed and the structure is compact, so that the nickel content on the surface of the material can be greatly reduced, the decomposition of electrolyte in the charging and discharging processes is reduced, the gas production can be reduced to the 523 type ternary material level, and the cycle stability and the thermal stability of the material are improved.
In order to solve the technical problems, the invention provides a method for preparing a core-shell structure nickel cobalt lithium aluminate material, which comprises the following steps:
The method comprises the following steps: preparing a salt solution A containing nickel salt, cobalt salt and aluminum salt, wherein Ni, Co and Al are a: 1-a-b: b, and (a is more than 0.7, b is more than or equal to 0.05 and more than or equal to 0, and 1 is more than a + b) are used as salt solutions for preparing core materials; preparing a salt solution B containing nickel salt, cobalt salt and aluminum salt, wherein Ni, Co and Al are c: 1-c-d: d, wherein c is more than 0.5, 0.5 is more than d is more than 0, and 1 is more than c + d) and used as a salt solution for preparing a shell material; preparing a sodium hydroxide alkali solution C mixed with ammonia water; preparing sodium carbonate alkali solution D containing ammonia water.
Step two: injecting the prepared salt solution A into a reaction kettle with a base solution at a constant speed, and adding an alkali solution C to adjust the pH value of the solution in the reaction kettle to be between 10 and 13; after 2/3-3/4 of the saline solution A is injected, continuously injecting the alkaline solution C into the reaction kettle at a descending rate of 10-1000ml per hour, gradually adding the alkaline solution D into the reaction kettle at an ascending rate of 10-1000ml per hour from zero, continuously injecting the saline solution B after the saline solution A is completely injected into the reaction kettle, reducing the flow rate of the alkaline solution C to 0 when the saline solution B is injected into 1/4-1/3, and continuously adding the alkaline solution D at a constant speed until the saline solution B is completely injected into the reaction kettle.
Step three: and after the saline solution B is injected, carrying out solid-liquid separation, and washing, drying and sieving the separated solid product to obtain the nickel-cobalt-aluminum precursor material.
Step four: mixing the prepared precursor material with a lithium source according to a molar ratio of Li to M (1.1-0.95) to 1, wherein M represents the sum of the molar numbers of nickel, cobalt and aluminum; then, roasting under the condition of introducing oxygen; and cooling, crushing and sieving to prepare the core-shell structure nickel-cobalt lithium aluminate material.
The nickel cobalt lithium aluminate material prepared by the invention is used as the anode material of the lithium ion battery.
The core-shell structure method greatly reduces the nickel content on the surface of the material, reduces the decomposition of the electrolyte in the charging and discharging process, reduces the gas production to 523 type ternary material level, and simultaneously improves the cycle stability and the thermal stability of the material. The process is simple and feasible, and can be used for large-scale industrial production.
Drawings
FIG. 1 is an XRD pattern of a core-shell structured material prepared in example 1 of the present invention;
FIG. 2-1 is an SEM image of a precursor material prepared in example 1 of the present invention;
FIG. 2-2 is an SEM image of a lithium nickel cobalt aluminate material prepared in example 1 of the present invention;
fig. 3 is a graph showing the initial charge-discharge curve of 2032 button cell made of nickel cobalt lithium aluminate material prepared in example 1 of the present invention, wherein the current density at normal temperature is 0.1C, and the voltage is 3.0-4.3V;
fig. 4 is a cycle curve diagram of current density 1C voltage 3.0-4.3V of 2032 button cell made of nickel cobalt lithium aluminate material prepared in example 1 of the invention.
FIG. 5 is a DSC chart of the charged 4.3V nickel cobalt lithium aluminate material and homogeneous nickel cobalt lithium aluminate material prepared by the method of example 1.
Detailed Description
The following describes the detailed procedures of the present invention by way of examples, which are provided for the convenience of understanding and are in no way limiting of the present invention.
example 1:
Preparing 8L of a salt solution A containing nickel and cobalt with the total molar concentration of 2M, wherein the ratio of Ni to Co is 9: 1, and taking the salt solution A as a salt solution for preparing a core material; preparing 4L of salt solution B containing nickel salt, cobalt salt and aluminum salt with the total molar concentration of 2M, wherein the ratio of Ni to Co to Al is 6: 2.5: 1.5, the salt solution B is used for preparing a shell material, preparing 8L of sodium hydroxide solution with the concentration of 2M, adding ammonia water, uniformly mixing, and then taking the ammonia concentration of 4M in the mixed solution as an alkali solution C; 4L of 2M sodium carbonate solution is prepared, ammonia water is added and mixed evenly, and the ammonia concentration of the mixed solution is 4M and is used as an alkali solution D.
injecting the prepared salt solution A into a reaction kettle with a base solution at a constant speed of 0.4L/h, and adding an alkali solution C to adjust the pH value of the solution in the reaction kettle to 10-11; after 6L of the saline solution A is injected, continuously injecting the alkaline solution C into the reaction kettle at a descending rate of 53ml per hour, simultaneously gradually adding the alkaline solution D into the reaction kettle at an ascending rate of 53ml per hour from zero, continuously injecting the saline solution B into the reaction kettle after the saline solution A is completely injected, when 1L of the saline solution B is injected, reducing the flow rate of the alkaline solution C to 0, and continuously adding the alkaline solution D at a constant speed until the saline solution B is completely injected into the reaction kettle. And after the reaction is finished, carrying out solid-liquid separation, and washing, drying and sieving the separated solid product to obtain the core-shell structure nickel-cobalt-aluminum precursor material. Mixing the prepared precursor material with a lithium source according to a molar ratio of Li to M of 1.05 to 1 (wherein M represents the sum of the molar numbers of nickel, cobalt and aluminum), and roasting for 4 hours at 300 ℃ under the condition of introducing oxygen, wherein the roasting time at 800 ℃ is 12 hours; and cooling to room temperature, crushing and sieving to prepare the core-shell structure lithium nickel cobalt aluminate LiNi0.8Co0.15Al0.05O2 material.
The XRD test result of the nickel cobalt lithium aluminate material is shown in figure 1, the crystal structure of the nickel cobalt lithium aluminate material is complete, and no mixed peak is found. As shown in FIGS. 2-1 and 2-2, it can be seen from SEM that the material precursor and the baked core-shell structure lithium nickel cobalt aluminate material have spherical morphology. The average particle size of the nickel cobalt lithium aluminate material is 6.9um, the tap density is 2.51g/cm3, the first charge capacity under the voltage of 0.1C current density 3.0-4.3V at normal temperature after the nickel cobalt lithium aluminate material is made into a 2032 button cell is 211.8mAh/g, the discharge capacity is 194.5mAh/g, and the first efficiency is 91.9%, as shown in figure 3. The 1C current density is 3.0-4.3V, the 50-time cycle retention rate is 89.5%, as shown in FIG. 4. As shown in FIG. 5, the highest thermal decomposition temperature in DSC test under 4.3V charging state is 250.5 ℃, which is obviously improved compared with 238 ℃ of homogeneous phase material, and the heat release is greatly reduced.
Example 2:
Preparing 4L of a nickel-cobalt-aluminum salt-containing solution A with the total molar concentration of 2M, wherein the ratio of Ni to Co to Al is 9: 0.5, and the solution is used as a salt solution for preparing a core material; preparing 8L of salt solution B containing nickel salt, cobalt salt and aluminum salt with the total molar concentration of 2M, wherein the ratio of Ni to Co to Al is 6: 1.25: 2.75 to be used as a salt solution for preparing a shell material, preparing 4L of sodium hydroxide solution with the concentration of 2M, adding ammonia water, uniformly mixing, and then taking the ammonia concentration of 4M in the mixed solution as an alkali solution C; preparing 8L of 2M sodium carbonate solution, adding ammonia water, and uniformly mixing to obtain a mixed solution with 4M ammonia concentration as an alkali solution D.
Injecting the prepared salt solution A into a reaction kettle with a base solution at a constant speed of 0.6L/h, and adding an alkali solution C to adjust the pH value of the solution in the reaction kettle to be 11-13; after 3L of the saline solution A is injected, continuously injecting the alkaline solution C into the reaction kettle at a descending rate of reducing 120ml per hour, simultaneously gradually adding the alkaline solution D into the reaction kettle at an ascending rate of increasing 120ml per hour from zero, continuously injecting the saline solution B after the saline solution A is completely injected into the reaction kettle, reducing the flow rate of the alkaline solution C to 0 when the saline solution B is injected into 2L, and continuously adding the alkaline solution D at a constant speed until the saline solution B is completely injected into the reaction kettle. And after the reaction is finished, carrying out solid-liquid separation, and washing, drying and sieving the separated solid product to obtain the core-shell structure nickel-cobalt-aluminum precursor material. Mixing the prepared precursor material with a lithium source according to a molar ratio of Li to M of 1.05 to 1 (wherein M represents the sum of the molar numbers of nickel, cobalt and aluminum), and roasting at 500 ℃ for 8h under the condition of introducing oxygen, wherein the roasting time at 850 ℃ is 24 h; cooling to room temperature, crushing and sieving to obtain the core-shell structure nickel cobalt lithium aluminate LiNi0.7Co0.1Al0.2O2 material.
The average particle size of the nickel cobalt lithium aluminate material obtained in the embodiment 2 is 7.8um, the tap density is 2.54g/cm3, the first charge capacity is 208.4mAh/g, the discharge capacity is 185.4mAh/g, and the first efficiency is 89% under the voltage of 0.1C current density 3.0-4.3V at normal temperature after the material is prepared into a 2032 button cell. The 1C current density is 3.0-4.3V, and the 50-time cycle retention rate is 89.5%.
In conclusion, the synthesis process of the core-shell structure nickel cobalt lithium aluminate prepared by the method is simple, has low requirements on equipment, and is suitable for industrial production. The prepared nickel cobalt lithium aluminate material has good crystallinity, spherical appearance, and better normal temperature cycle and high temperature cycle, safety performance and gas production rate than homogeneous phase nickel cobalt lithium aluminate materials. While the present invention has been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are intended to be illustrative rather than restrictive, and many modifications may be made by those skilled in the art without departing from the spirit of the present invention within the scope of the appended claims.
Claims (9)
1. the core-shell structure nickel cobalt lithium aluminate material is characterized in that the total molecular formula of the material is LiNixCo1-x-yAlyO2, wherein x is more than or equal to 0.7, y is more than or equal to 0.2 and more than or equal to 0.05, and 1 is more than x + y, the structure is composed of a core part and a shell part, wherein the molecular formula of the core part is as follows: LiNiCo 1-a-bAlbO2, wherein a is more than 0.7, b is more than or equal to 0.05 and more than or equal to 0, 1 is more than a + b, and the molecular formula of the shell part is LiNiCo 1-c-dAldO2, wherein c is more than 0.5, 0.5 is more than d is more than 0, and 1 is more than c + d.
2. a preparation method of a core-shell structure nickel cobalt lithium aluminate material comprises the following steps:
The method comprises the following steps: preparing a salt solution A containing nickel salt, cobalt salt and aluminum salt, wherein the ratio of Ni to Co to Al is a: 1-a-b: b, a is more than 0.7, b is more than or equal to 0.05 and more than or equal to 0, and 1 is more than a + b and is used as a salt solution for preparing a core material; preparing a salt solution B containing nickel salt, cobalt salt and aluminum salt, wherein Ni, Co and Al are c: 1-c-d: d, wherein c is more than 0.5, 0.5 is more than d is more than 0, and 1 is more than c + d and is used as a salt solution for preparing a shell material; preparing a sodium hydroxide alkali solution C mixed with ammonia water; preparing a sodium carbonate alkali solution D mixed with ammonia water;
Step two: injecting the prepared salt solution A into a reaction kettle with a base solution at a constant speed, and adding an alkali solution C to adjust the pH value of the solution in the reaction kettle to be between 10 and 13; after 2/3-3/4 of the saline solution A is injected, continuously injecting the alkaline solution C into the reaction kettle at a descending rate of 10-1000ml per hour, gradually adding the alkaline solution D into the reaction kettle at an ascending rate of 10-1000ml per hour from zero, continuously injecting the saline solution B after the saline solution A is completely injected into the reaction kettle, reducing the flow rate of the alkaline solution C to 0 when the saline solution B is injected into 1/4-1/3, and continuously adding the alkaline solution D at a constant speed until the saline solution B is completely injected into the reaction kettle;
Step three: after the saline solution B is injected, carrying out solid-liquid separation, and washing, drying and sieving the separated solid product to obtain a nickel-cobalt-aluminum precursor material;
Step four: mixing the prepared precursor material with a lithium source according to a molar ratio of Li to M of 1.1-0.95 to 1, wherein M represents the sum of the molar numbers of nickel, cobalt and aluminum; then, roasting under the condition of introducing oxygen; and cooling, crushing and sieving to prepare the core-shell structure nickel-cobalt lithium aluminate material.
3. The method for preparing the core-shell structure nickel cobalt lithium aluminate material according to claim 2, wherein the nickel salt, the cobalt salt and the aluminum salt are soluble salts, and the nickel salt is any one of nickel sulfate, nickel nitrate, nickel chloride and nickel acetate; the cobalt salt is any one of cobalt sulfate, cobalt nitrate, cobalt chloride and cobalt acetate; the aluminum salt is any one of aluminum nitrate, aluminum sulfate and aluminum chloride.
4. the method for preparing the core-shell structure nickel cobalt lithium aluminate material according to claim 2, wherein the total molar ratio concentration of nickel, cobalt and aluminum of the salt solution A and the salt solution B is the same, and the volume ratio of the salt solution A to the salt solution B injected into the reaction kettle is as follows: 1-10: 1.
5. The preparation method of the core-shell structure nickel cobalt lithium aluminate material according to claim 2, wherein the concentration of sodium hydroxide in the alkali solution C is 2-10M, and the content of ammonia water in the alkali solution C is 1-8M; the concentration of sodium carbonate in the alkali solution D is 0.5-2M, and the content of ammonia water is 1-8M.
6. the method for preparing the core-shell structure nickel cobalt lithium aluminate material according to claim 2, characterized in that: two kinds of alkaline solution precipitants are used, and an alkaline solution C and an alkaline solution D are injected into the reaction kettle in a concentration gradient mode in 1/4-1/3 processes starting from the last 1/4-1/3 of the injection of the saline solution A and the saline solution B.
7. the method for preparing the nickel cobalt lithium aluminate material with the core-shell structure according to claim 2, which is characterized in that: the lithium source is lithium carbonate or lithium hydroxide.
8. The preparation method of the core-shell structure nickel cobalt lithium aluminate material according to claim 2, wherein the roasting is carried out by a two-stage method, the roasting temperature of the first stage is 300-500 ℃, the roasting time of the first stage is 4-8 h, the roasting temperature of the second stage is 650-850 ℃, and the roasting time of the second stage is 12-24 h.
9. The application of the nickel cobalt lithium aluminate material is characterized in that the core-shell structure nickel cobalt lithium aluminate material prepared by the preparation method of the core-shell structure nickel cobalt lithium aluminate material according to claim 2 is used as a positive electrode material of a lithium ion battery.
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| CN105552361A (en) * | 2016-01-25 | 2016-05-04 | 荆门市格林美新材料有限公司 | Positive electrode material precursor of lithium ion battery and preparation method thereof |
| WO2018026650A1 (en) * | 2016-08-02 | 2018-02-08 | Apple Inc. | Coated nickel-based cathode materials and methods of preparation |
| CN106340641B (en) * | 2016-11-17 | 2018-11-20 | 兰州理工大学 | Can autonomous adjustment aperture hollow sphere nickle cobalt lithium manganate preparation method |
| CN110337745B (en) * | 2017-03-31 | 2024-03-19 | 松下控股株式会社 | Positive electrode active material for nonaqueous electrolyte secondary battery and method for producing same |
| KR102123541B1 (en) | 2017-06-29 | 2020-06-16 | 주식회사 엘지화학 | Method for preparing positive electrode active material precursor for lithium secondary battery |
| KR102268079B1 (en) * | 2017-11-21 | 2021-06-23 | 주식회사 엘지화학 | Positive electrode active material for secondary battery, method for preparing the same and lithium secondary battery comprising the same |
| EP3797446A4 (en) * | 2018-05-21 | 2022-03-16 | Microvast Power Systems Co., Ltd. | Methods for preparing particle precursor and cathode active particles, and particle precursor prepared thereby |
| US20210020913A1 (en) * | 2018-06-11 | 2021-01-21 | Microvast Power Systems Co., Ltd. | Methods for preparing particles precursor, and particle precursor prepared thereby |
| CN108987726B (en) * | 2018-08-22 | 2021-07-20 | 成都巴莫科技有限责任公司 | Preparation method of carbon dynamic coated lithium-rich oxide solid solution material |
| CN114772556B (en) * | 2022-06-20 | 2022-11-04 | 天津蓝天太阳科技有限公司 | Porous structure precursor, hollow structure oxide and application in anode material |
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