CN110504447B - Fluorine-doped nickel-cobalt-manganese precursor and preparation method and application thereof - Google Patents
Fluorine-doped nickel-cobalt-manganese precursor and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
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- 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
- 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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- 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
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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
- 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
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- 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 provides a fluorine-doped nickel-cobalt-manganese precursor and a preparation method and application thereof, wherein the method comprises the following steps: preparing soluble salts of nickel and cobalt into a first mixed solution containing nickel salt and cobalt salt; preparing a second mixed solution from a soluble salt solution of manganese and a soluble fluoride salt complexing agent under the condition of introducing protective gas; and adding the first mixed solution, the second mixed solution, a sodium hydroxide solution and an ammonia water solution into a reaction kettle with an ultrasonic device in a parallel flow manner, keeping the temperature at 50-60 ℃, stirring at the speed of 500-800 r/min until the reaction is finished, aging and carrying out solid-liquid separation to obtain a precipitate, and washing and drying the obtained precipitate to obtain the fluoride ion-doped nickel-cobalt-manganese precursor. The obtained precursor material has a sphere-like structure and a specific surface area of 5.6-6.3 m2(ii) a tap density of 2.2 to 2.7g/cm3And the obtained cathode material has good electrochemical performance.
Description
Technical Field
The invention relates to the technical field of battery material preparation, in particular to a fluorine-doped nickel-cobalt-manganese precursor and a preparation method and application thereof.
Background
The lithium ion battery has the advantages of high energy, long service life, no memory effect, low pollution and the like, and is widely applied to various fields of mobile phones, computers, electric automobiles and the like. Currently, the positive electrode materials adopted by lithium ion batteries mainly include lithium cobaltate, lithium iron phosphate, lithium manganate, lithium nickel cobalt manganese, and the like. The anode material with the largest market share is lithium cobaltate, but cobalt is used as a strategic resource, so that the storage capacity is small, the price is high, and the safety performance of the lithium cobaltate is poor, so that the further development of the material is limited. The nickel cobalt lithium manganate has the advantages of high specific capacity, good thermal stability, low price and the like, is the most potential anode material of the lithium ion battery, and has good application prospect in the power fields of electric vehicles, electric tools and the like.
At present, the common methods for preparing the nickel cobalt lithium manganate comprise a high-temperature solid phase method and a coprecipitation-high-temperature solid phase method. The high-temperature solid phase method is that a nickel source, a cobalt source, a manganese source and a lithium source are ball-milled uniformly and then are calcined at high temperature. The method has the disadvantages that the nickel, cobalt and manganese are difficult to be uniformly mixed, so that the synergistic effect of the three elements cannot be fully exerted, the morphology of the prepared material is difficult to control, the synthesized powder material is generally composed of irregular particles, and the tap density and the flowability of the material are poor, so that the preparation of the anode material is not facilitated. The other method is a coprecipitation-high temperature solid phase method, namely, firstly preparing a nickel-cobalt-manganese hydroxide precursor by the coprecipitation method, and then adding a lithium source for sintering to obtain the nickel-cobalt-manganese lithium manganate. According to the method, the morphology and the granularity of the precursor are not changed basically in the sintering process after the lithium source is added, and the morphology and the granularity of the nickel cobalt lithium manganate material play a key role in various performances of the lithium ion battery. Therefore, the synthesis of the nickel-cobalt-manganese hydroxide precursor with appropriate morphology and particle size becomes a key factor influencing the performance of nickel-cobalt-manganese acid lithium.
However, the synthesis of the nickel-cobalt-manganese hydroxide precursor by the traditional coprecipitation method is difficult, mainly because the precipitation concentration product of manganese ions is different from the precipitation concentration product of nickel and cobalt elements by several orders of magnitude, the precipitation speed of the manganese ions and hydroxide radicals is very high during the coprecipitation reaction, flocculent precipitates are easily formed, the particle size growth of the precursor is difficult, and the prepared precursor has low tap density, poor sphericity, small particle size, difficulty in cleaning and the like.
Therefore, it is necessary to regulate and control the deposition speed of manganese hydroxide in the process of synthesizing the precursor by a coprecipitation method, so as to realize homogeneous deposition of manganese elements, cobalt and nickel elements, improve the tap density and specific surface area of the precursor, and improve the electrochemical performance of the anode material.
Disclosure of Invention
The invention provides a fluorine-doped nickel-cobalt-manganese precursor and a preparation method and application thereof, and aims to improve the tap density and specific surface area of the precursor and improve the electrochemical performance of a positive electrode material.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of fluorine-doped nickel-cobalt-manganese precursor comprises the following steps:
(1) preparing soluble salts of nickel and cobalt into a first mixed solution containing nickel salt and cobalt salt; preparing a second mixed solution from a soluble salt solution of manganese and a soluble fluoride salt complexing agent; wherein the molar ratio of fluorine ions to manganese ions is 1-5: 1;
(2) adding the first mixed solution and the second mixed solution obtained in the step (1), a sodium hydroxide solution and an ammonia water solution into a reaction kettle with an ultrasonic device in a parallel flow manner under the condition of introducing protective gas, keeping the temperature at 50-60 ℃, stirring at the speed of 500-800 r/min until the reaction is finished, aging and carrying out solid-liquid separation to obtain a precipitate, and washing and drying the obtained precipitate to obtain a fluorine ion doped nickel-cobalt-manganese precursor;
wherein the addition amount of the sodium hydroxide solution is to keep the pH value of the solution at 9-12; the ratio of the mole number of the ammonia water to the total mole of the three metal ions of nickel, cobalt and manganese is 1-10: 1; the power of the ultrasonic device is set to be 520-560W.
Preferably, the nickel salt in step (1) is nickel sulfate, nickel chloride, nickel acetate or nickel nitrate; the cobalt salt is cobalt sulfate, cobalt acetate or cobalt nitrate; the manganese salt is manganese sulfate, manganese chloride, manganese acetate or manganese nitrate.
Preferably, the soluble fluoride salt in step (1) is sodium fluoride, ammonium fluoride or potassium fluoride.
Preferably, the protective gas in step (2) is nitrogen or argon.
Preferably, the concentration of the sodium hydroxide solution in the step (2) is 2-8 mol/L.
Preferably, the concentration of the ammonia water solution in the step (2) is 5-10 mol/L.
Preferably, the aging time in the step (2) is 24-72 h.
Preferably, the drying in the step (2) is vacuum drying, the drying temperature is 90-105 ℃, and the drying time is 20-24 hours.
The invention also provides a fluorine-doped nickel-cobalt-manganese precursor, which is prepared by the method.
The invention also provides a fluorine-doped nickel cobalt lithium manganate positive electrode material, which is prepared by mixing and sintering the fluorine-doped nickel cobalt manganese precursor and a lithium source.
According to the preparation method of the fluorine-doped nickel-cobalt-manganese precursor, a soluble salt solution of manganese and a soluble fluoride complexing agent are prepared into a second mixed solution, the second mixed solution, a mixed salt solution of nickel and cobalt, a sodium hydroxide solution and an ammonia water solution are added into a reaction kettle with an ultrasonic device in a parallel flow manner, and the fluorine ion-doped nickel-cobalt-manganese precursor precipitate is generated after stirring reaction. Wherein manganese ions are mixed with fluorine ions to form a majority of [ MnF6]4-And a minority of [ MnF4]2-Complex ions of (2), which can slowly release Mn2+And F—Ions to achieve effective control of Mn2+And (OH)—Generation of Mn (OH)3Rate of precipitation of Mn2+And Ni2+、CO2+And homogeneous deposition is carried out together, a more uniform spheroidal structure is formed, and the tap density and the specific surface area of the precursor are improved.
The scheme of the invention has the following beneficial effects:
according to the preparation method of the fluorine-doped nickel-cobalt-manganese precursor, the fluorine ions and the manganese ions in the soluble fluoride salt complexing agent form complex ions, and the complex ions can slowly release the manganese ions and the fluorine ions, so that the deposition speed of the manganese ions and hydroxyl groups is effectively controlled, the manganese ions and the hydroxyl groups are uniformly deposited together with the nickel ions and the cobalt ions, and the tap density and the specific surface area of the precursor are improved. The fluorine-doped nickel-cobalt-manganese precursor powder material prepared in the embodiment has a uniform spheroidal structure, and the specific surface area is 5.6-6.3 m2(ii) a tap density of 2.2 to 2.7g/cm3。
The invention provides a preparation method of a nickel-cobalt-manganese precursor, which comprises the following steps of (2) adding a first mixed solution, a second mixed solution, a sodium hydroxide solution and an ammonia water solution into a reaction kettle with an ultrasonic device in a concurrent flow manner, wherein the action of ultrasonic waves in the preparation method is represented as follows: on one hand, all raw materials are dispersed more uniformly in the reaction process, and the agglomeration of the nano material in the reaction process can be obviously inhibited; on the other hand, local high temperature and high energy brought by ultrasonic cavitation are helpfulThe reaction time is effectively shortened by the formation of crystal nucleus, and the size and the shape of the particles can be controlled by adjusting the frequency of the ultrasonic wave. According to the invention, the power of the ultrasonic device is set to 520-560W, precursor powder with a sphere-like structure is formed, and the electrochemical performance of the material is effectively improved. The precursor prepared in the embodiment is made into a positive electrode material and then assembled into a button cell, and the test result is 179.5mAhg-1(0.2C)，170mAhg-1(0.5C)，162.5mAhg-1(1C)，151mAhg-1(2C)，139mAhg-1(5C)，124.5mAhg-1(10C) In that respect The capacity retention rate is more than 90.2 percent after 2C circulation for 300 weeks.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
Example 1
The preparation method of the fluorine-doped nickel-cobalt-manganese precursor provided by the embodiment comprises the following steps:
(1) preparing a first mixed solution containing nickel salt and cobalt salt from nickel nitrate and cobalt nitrate, wherein the concentration of the first mixed solution is 1 mol/L, and preparing a second mixed solution from manganese nitrate and sodium fluoride, wherein the molar ratio of nickel ions to cobalt ions to manganese ions is 5:2:3, and the molar ratio of fluorine ions to manganese ions is 2: 1;
(2) taking an ammonia water solution with the pH value of 10 as a base solution, adding the first mixed solution and the second mixed solution obtained in the step (1), a sodium hydroxide solution with the concentration of 2 mol/L and an ammonia water solution with the concentration of 5 mol/L into a reaction kettle with an ultrasonic device in a cocurrent flow mode under the condition that argon is introduced as a protective gas, keeping the temperature at 60 ℃, stirring at the speed of 500r/min until the reaction is finished, carrying out solid-liquid separation after aging for 36h to obtain a precipitate, washing the obtained precipitate, and then carrying out vacuum drying for 24h at the temperature of 90 ℃ to obtain a fluoride ion doped nickel-cobalt-manganese precursor;
wherein the sodium hydroxide solution is added in an amount to maintain the pH of the solution at 9; the ratio of the mole number of the ammonia water to the total mole of the three metal ions of nickel, cobalt and manganese is 1: 1; the power of the ultrasonic device was set to 540W.
The fluorine-doped nickel-cobalt-manganese precursor prepared by the process is of a spheroidal structure, particles are relatively uniform, and the specific surface area is 5.6m2(ii)/g, tap density 2.5g/cm3。
(3) L i2CO3Uniformly mixing the fluorine-doped nickel cobalt manganese precursor obtained in the step (2) according to a molar ratio of 1.03 to obtain a lithium preparation precursor, sintering the lithium preparation precursor at 850 ℃ for 12h, naturally cooling to room temperature, and then crushing and sieving to obtain a fluorine-doped nickel cobalt lithium manganate positive electrode material;
the button cell assembled by the positive electrode material obtained in the embodiment is tested, and the method specifically comprises the following steps:
a. according to the positive electrode material: carbon black: mixing the vinylidene fluoride (PVF) at a ratio of 90:2:8, adding a proper amount of N-methyl pyrrolidone, stirring to form uniform slurry, uniformly coating the obtained slurry on an aluminum foil, and drying, rolling and cutting to form a positive plate;
b. assembling a positive plate, a negative electrode (lithium plate), electrolyte, a diaphragm and a battery shell into a button battery in an argon-protected glove box, and carrying out electrochemical performance test to obtain a test result of 179.5mAhg-1(0.2C)，170mAhg-1(0.5C)，162.5mAhg-1(1C)，151mAhg-1(2C)，139mAhg-1(5C)，124.5mAhg-1(10C) In that respect The capacity retention rate is more than 90.2 percent after 2C circulation for 300 weeks.
Example 2
The preparation method of the fluorine-doped nickel-cobalt-manganese precursor provided by the embodiment comprises the following steps:
(1) preparing a first mixed solution containing nickel salt and cobalt salt from nickel chloride and cobalt chloride, wherein the concentration of the first mixed solution is 1.5 mol/L, and preparing a second mixed solution from manganese chloride and potassium fluoride, wherein the molar ratio of nickel ions to cobalt ions to manganese ions is 1:1:1, and the molar ratio of fluorine ions to manganese ions is 1: 1;
(2) taking an ammonia water solution with the pH value of 11 as a base solution, adding the first mixed solution and the second mixed solution obtained in the step (1), a sodium hydroxide solution with the concentration of 6 mol/L and an ammonia water solution with the concentration of 8 mol/L into a reaction kettle with an ultrasonic device in a cocurrent flow mode under the condition that nitrogen is introduced as a protective gas, keeping the temperature at 50 ℃, stirring at the speed of 700r/min until the reaction is finished, carrying out solid-liquid separation after aging for 72 hours to obtain a precipitate, washing the obtained precipitate, and then carrying out vacuum drying for 20 hours at the temperature of 105 ℃ to obtain a fluoride ion doped nickel-cobalt-manganese precursor;
wherein the sodium hydroxide solution is added in an amount to maintain the pH of the solution at 11; the ratio of the mole number of the ammonia water to the total mole of the three metal ions of nickel, cobalt and manganese is 8: 1; the power of the ultrasonic device was set to 520W.
The fluorine-doped nickel-cobalt-manganese precursor prepared by the process is of a spheroidal structure, particles are relatively uniform, and the specific surface area is 6.1m2(ii)/g, tap density 2.7g/cm3。
(3) L i2CO3Uniformly mixing the fluorine-doped nickel cobalt manganese precursor obtained in the step (2) according to a molar ratio of 1.03 to obtain a lithium preparation precursor, sintering the lithium preparation precursor at 850 ℃ for 12h, naturally cooling to room temperature, and then crushing and sieving to obtain a fluorine-doped nickel cobalt lithium manganate positive electrode material;
the cathode material obtained in the example was assembled into a button cell by the method described in example 1, and the test result was 173.5mAhg-1(0.2C)，164mAhg-1(0.5C)，155.5mAhg-1(1C)，146mAhg-1(2C)，134mAhg-1(5C)，121.5mAhg-1(10C) In that respect The capacity retention rate after 300 weeks of 2C circulation is more than 90.4%.
Example 3
The preparation method of the fluorine-doped nickel-cobalt-manganese precursor provided by the embodiment comprises the following steps:
(1) preparing a first mixed solution containing nickel salt and cobalt salt from nickel chloride and cobalt chloride, wherein the concentration of the first mixed solution is 1.5 mol/L, and preparing a second mixed solution from manganese chloride and potassium fluoride, wherein the molar ratio of nickel ions to cobalt ions to manganese ions is 5:2:3, and the molar ratio of fluorine ions to manganese ions is 5: 1;
(2) taking an ammonia water solution with the pH value of 11 as a base solution, adding the first mixed solution and the second mixed solution obtained in the step (1), a sodium hydroxide solution with the concentration of 8 mol/L and an ammonia water solution with the concentration of 10 mol/L into a reaction kettle with an ultrasonic device in a cocurrent flow mode under the condition that nitrogen is introduced as a protective gas, keeping the temperature at 55 ℃, stirring at the speed of 800r/min until the reaction is finished, carrying out solid-liquid separation after aging for 24 hours to obtain a precipitate, washing the obtained precipitate, and then carrying out vacuum drying for 22 hours at the temperature of 100 ℃ to obtain a fluoride ion doped nickel-cobalt-manganese precursor;
wherein the sodium hydroxide solution is added in an amount to maintain the pH of the solution at 12; the ratio of the mole number of the ammonia water to the total mole of the three metal ions of nickel, cobalt and manganese is 10: 1; the power of the ultrasonic device was set to 560W.
The fluorine-doped nickel-cobalt-manganese precursor prepared by the process is of a spheroidal structure, particles are relatively uniform, and the specific surface area is 6.3m2(ii)/g, tap density 2.6g/cm3。
(3) L i2CO3Uniformly mixing the fluorine-doped nickel cobalt manganese precursor obtained in the step (2) according to a molar ratio of 1.03 to obtain a lithium preparation precursor, sintering the lithium preparation precursor at 850 ℃ for 12h, naturally cooling to room temperature, and then crushing and sieving to obtain a fluorine-doped nickel cobalt lithium manganate positive electrode material;
the cathode material obtained in the example was assembled into a button cell by the method described in example 1, and the test result was 176.5mAhg-1(0.2C)，165mAhg-1(0.5C)，154.5mAhg-1(1C)，142mAhg-1(2C)，130mAhg-1(5C)，117.5mAhg-1(10C) In that respect The capacity retention rate after 300 weeks of 2C circulation is more than 89.5%.
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 (10)
1. A preparation method of fluorine-doped nickel-cobalt-manganese precursor is characterized by comprising the following steps:
(1) preparing soluble salts of nickel and cobalt into a first mixed solution containing nickel salt and cobalt salt; preparing a second mixed solution from a soluble salt solution of manganese and a soluble fluoride salt complexing agent; wherein the molar ratio of fluorine ions to manganese ions is 1-5: 1;
(2) adding the first mixed solution and the second mixed solution obtained in the step (1), a sodium hydroxide solution and an ammonia water solution into a reaction kettle with an ultrasonic device in a parallel flow manner under the condition of introducing protective gas, keeping the temperature at 50-60 ℃, stirring at the speed of 500-800 r/min until the reaction is finished, aging and carrying out solid-liquid separation to obtain a precipitate, and washing and drying the obtained precipitate to obtain a fluorine ion doped nickel-cobalt-manganese precursor;
wherein the addition amount of the sodium hydroxide solution is to keep the pH value of the solution at 9-12; the ratio of the mole number of the ammonia water to the total mole of the three metal ions of nickel, cobalt and manganese is 1-10: 1; the power of the ultrasonic device is set to be 520-560W.
2. The production method according to claim 1, wherein the nickel salt in the step (1) is nickel sulfate, nickel chloride, nickel acetate or nickel nitrate; the cobalt salt is cobalt sulfate, cobalt acetate or cobalt nitrate; the soluble salt of manganese is manganese sulfate, manganese chloride, manganese acetate or manganese nitrate.
3. The method according to claim 1, wherein the soluble fluoride salt in the step (1) is sodium fluoride, ammonium fluoride or potassium fluoride.
4. The method according to claim 1, wherein the protective gas in the step (2) is nitrogen or argon.
5. The preparation method according to claim 1, wherein the concentration of the sodium hydroxide solution in the step (2) is 2-8 mol/L.
6. The method according to claim 1, wherein the concentration of the aqueous ammonia solution in the step (2) is 5 to 10 mol/L.
7. The method according to claim 1, wherein the aging time in step (2) is 24 to 72 hours.
8. The preparation method according to claim 1, wherein the drying in the step (2) is vacuum drying, the drying temperature is 90-105 ℃, and the drying time is 20-24 h.
9. A fluorine-doped nickel-cobalt-manganese precursor, characterized in that it is prepared by the method of any one of claims 1 to 8.
10. The fluorine-doped nickel cobalt lithium manganate positive electrode material is characterized in that the positive electrode material is prepared by mixing and sintering the fluorine-doped nickel cobalt manganese precursor according to claim 9 or the fluorine-doped nickel cobalt manganese precursor prepared by the method according to any one of claims 1 to 8 and a lithium source.
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| CN114212803B (en) * | 2021-10-28 | 2023-09-12 | 广东邦普循环科技有限公司 | Preparation method of fluorine-doped Prussian blue sodium ion battery positive electrode material |
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