CN114873657A - Preparation method and application of modified lithium-rich manganese-based positive electrode material - Google Patents
Preparation method and application of modified lithium-rich manganese-based positive electrode material Download PDFInfo
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- CN114873657A CN114873657A CN202210558709.8A CN202210558709A CN114873657A CN 114873657 A CN114873657 A CN 114873657A CN 202210558709 A CN202210558709 A CN 202210558709A CN 114873657 A CN114873657 A CN 114873657A
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- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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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Abstract
The invention relates to the field of lithium batteries, in particular to a preparation method and application of a modified lithium-rich manganese-based positive electrode material. The preparation method of the modified lithium-rich manganese-based positive electrode material comprises the following steps: (1) preparing a lithium-rich manganese-based precursor; (2) mixing the precursor and a lithium source; (3) and modifying the lithium-rich manganese base. The prepared anode material can have excellent stability and voltage attenuation resistance effect of the anode material, and can effectively and fundamentally solve the problem of oxygen precipitation in the use process of the lithium-rich manganese-based anode material, so that the problem of pain in the field of the lithium-rich manganese-based anode material is fundamentally solved, and the lithium-rich manganese-based anode material is suitable for being popularized in the field of lithium batteries.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a preparation method and application of a modified lithium-rich manganese-based positive electrode material.
Background
A lithium ion battery, as a rechargeable secondary battery, mainly operates by deintercalation of lithium ions between a positive electrode and a negative electrode. The lithium ion battery has the advantages of high working voltage, long cycle life, large specific capacity, good safety performance, small self-discharge, no memory effect and the like.
Among them, lithium-rich manganese-based positive electrode materials have been widely used in recent years for lithium battery positive electrode materials due to their excellent capacity (> 250 mAhg). However, the lithium-rich manganese-based cathode material still exists: serious voltage decline and poor cycle stability. These problems are mainly caused by the occurrence of oxygen evolution reaction and irreversible phase change during the first charge and discharge at high voltage.
The prior art (CN202011100886.9) provides a preparation method of a lithium-rich manganese-based cathode material, which prepares a fluorine and magnesium doped precursor mainly by a binary system coprecipitation method, claims that the preparation process is simple, and can effectively improve the stability and voltage attenuation of the cathode material. However, since it does not substantially solve the problem of oxygen evolution during use of the positive electrode material, the problem of voltage drop is not fundamentally solved.
Therefore, in order to solve the above problems, the present applicant provides a method for preparing a modified lithium-rich manganese-based positive electrode material having excellent cycle stability and voltage fade resistance.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a method for preparing a modified lithium-rich manganese-based positive electrode material, which comprises the following steps: (1) preparing a lithium-rich manganese-based precursor; (2) mixing the precursor and a lithium source; (3) and modifying the lithium-rich manganese base.
As a preferred scheme, the preparation of the lithium-rich manganese-based precursor comprises the following specific operations: (1) introducing nitrogen into the reaction kettle, adding a dilute ammonia solution serving as a base solution into the reaction kettle through a peristaltic pump, and adding an aqueous solution of metal salt into the reaction kettle according to a certain molar ratio through a coprecipitation method; (2) adding a precipitant solution, continuously stirring and reacting for 20-100 h at the temperature of 45-65 ℃, controlling the pH of a reaction system to be 10.5-11.5, and filtering, washing and drying precipitate crystals generated by the reaction to obtain a precursor.
In a preferred embodiment, the metal salt is at least one of a sulfate, a carbonate and a nitrate of nickel, cobalt and manganese metals.
As a preferable scheme, the compound molecular formula of nickel, cobalt and manganese in the metal salt is Ni a Co b Mn c Wherein a is more than or equal to 0.10 and less than or equal to 0.50, b is more than or equal to 0.05, c is more than or equal to 0.50 and less than or equal to 0.90, and the total amount of a + b + c is 1.
In a preferred embodiment, the molar ratio of nickel, cobalt and manganese in the metal salt is 30:3:67, the compound molecular formula is Ni 0.3 Co 0.03 Mn 0.67 。
As a preferred scheme, the precipitant solvent is a mixture of metal alkali solution, sulfate solution and ammonia water; the molar ratio of the metal alkali solution to the sulfate solution to the ammonia water is 2-3: 1-2: 1.
as a preferable mode, the molar ratio of the metal alkali solution, the sulfate solution and the ammonia water is 2.5:1.5: 1.
as a preferred scheme, the specific operations of compounding the precursor and the lithium source are as follows: (1) uniformly mixing the precursor with a lithium source and an additive; (2) heating to 300-1000 ℃, reacting for 5-20 hours under heat preservation, cooling, sieving and demagnetizing to obtain the matrix material.
In a preferred embodiment, the lithium source is at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium chloride, and lithium oxalate.
In a preferred embodiment, the molar ratio of lithium in the lithium source to metal ions in the precursor is (1.1-1.5): 1.
Preferably, the additive is at least one of oxide, hydroxide and inorganic acid salt containing Al, Mg, Ti, Y, La and Ce elements.
As a preferred scheme, the additive is Al 2 O 3 。
As a preferable scheme, the addition amount of the additive is 2000-4000 ppm of the total weight of the precursor and the lithium source after compounding.
As a preferable scheme, the specific operation of the modification and modification of the lithium-rich manganese base is as follows: (1) dissolving a modifier in ethanol or ultrapure water, dispersing the base material in the modifier solution, and stirring for 10-60 min; (2) adding a reducing agent, washing, and calcining at 200-800 ℃ for 1-20 hours to obtain the catalyst.
In a preferred embodiment, the modifier is at least one of inorganic salts of Ni, Co, Mn, Mg, Sr, Ti, Zr, Mo, Y, La, Ce, Al.
In a preferred embodiment, the modifier is La (NO).
As a preferred scheme, the reducing agent is NaBH 4 、KBH 4 And a sulfite solution.
As a preferred scheme, the reducing agent is NaBH 4 。
Preferably, the molar ratio of the reducing agent solution to the metal element in the modifier is 100 (20-70).
As a preferable mode, the molar ratio of the reducing agent solution to the metal element is 100: 50.
In the application, the voltage decay resistance and the electrochemical stability of the anode material are effectively improved by adding the reducing agent and the modifying agent in the step (3) and limiting the compounding ratio. The applicant believes that: NaBH as used in this application 4 And when the molar ratio of La (NO) to La (NO) is 100:50, the proper compound dosage of the La (NO) and the La (NO) can be used for coating the surface of the anode material by a reduction method and modifying oxygen vacancies on the surface of the anode material, so that the problem of oxygen precipitation of the oxygen vacancies in the charging and discharging process is greatly reduced, and the existence of the coating layer can effectively stabilize the surface of the material, thereby inhibiting the voltage attenuation phenomenon under the high-voltage cycle. When the amount of La (NO) is large, the excessive La metal compound forms an excessive coating layer which easily blocks the flow of electrons and stabilizes the voltage, thereby decreasing the positive voltageThe electrochemical performance of the common anode material.
The invention provides an application of the preparation method of the modified lithium-rich manganese-based positive electrode material, and the application of the method in a process for preparing the positive electrode material and the negative electrode material of the lithium battery is included.
Has the advantages that:
1. the modified lithium-rich manganese-based positive electrode material provided by the application can have excellent stability and voltage attenuation resistance of the positive electrode material, and can effectively and fundamentally solve the problem of oxygen precipitation in the previous use process of the lithium-rich manganese-based positive electrode material, so that the pain point in the field of the lithium-rich manganese-based positive electrode material is fundamentally solved.
2. The application provides a modified lithium-rich manganese-based positive electrode material, and NaBH (sodium borohydride) capable of being adopted in the modified lithium-rich manganese-based positive electrode material 4 And when the molar ratio of La (NO) to La (NO) is 100:50, the voltage fading resistance and the electrochemical stability of the anode material are effectively improved, La metal compound coating can be carried out on the surface of the anode material, and the oxygen vacancy on the surface of the anode material is modified, so that the problem of oxygen precipitation of the oxygen vacancy in the charge and discharge process is greatly reduced, and meanwhile, the existence of the coating layer can effectively stabilize the surface of the material, so that the voltage attenuation phenomenon is inhibited under the high-voltage cycle.
Drawings
Fig. 1 is an electron micrograph of polycrystals of the positive electrode materials prepared in example 1 and comparative example 2 of the present invention.
Fig. 2 is a comparison graph of the normal and high temperature cycle curves of the positive electrode materials prepared in example 1 and comparative example 1 of the present invention as a positive electrode material of a lithium ion battery.
Detailed Description
Example 1
Embodiment 1 provides a method for preparing a modified lithium-rich manganese-based positive electrode material, which comprises the following steps: (1) preparing a lithium-rich manganese-based precursor; (2) mixing the precursor and a lithium source; (3) and modifying the lithium-rich manganese base.
The specific operation is as follows: (1) sulfate of nickel, cobalt and manganese is prepared according to the proportion of Ni: co: the molar ratio of Mn to Mn is 30:3:67 and is prepared into 2mAn ol/L salt mixed solution; diluting 30 wt% concentrated sodium hydroxide lye (about 11.7M) into dilute lye of 5 mol/L; adding water into 22 wt% concentrated ammonia water (about 12.5M) to dilute and prepare 1mol/L dilute ammonia solution; introducing nitrogen into a 10L reaction kettle, firstly adding 5L of 2mol/L diluted ammonia water as a base solution through a peristaltic pump, respectively introducing the nickel sulfate solution, the cobalt sulfate solution and the manganese sulfate solution into the reaction kettle according to the molar ratio of Ni: Co: Mn: 30:3:67 through a coprecipitation method, and simultaneously introducing the diluted alkali solution and concentrated ammonia water, wherein the sodium hydroxide diluted alkali solution (NaOH), the metal salt solution (MSO4) and the concentrated ammonia water solution (NH3, aq.) are added according to the proportion of NaOH: MSO 4 :NH 3 ·H 2 Adding O at a molar ratio of 2.5:1.5: 1; continuously stirring and reacting for 12h at 50 ℃; the online pH meter monitored pH 11; filtering, washing and drying the precipitate generated by the reaction to obtain a lithium-rich manganese-based precursor Ni 0.30 Co 0.03 Mn 0.67 (OH) 2 。
(2) Mixing the lithium-rich manganese-based precursor obtained in the step (1) with Li 2 CO 3 Mixing according to the molar ratio of 1:1.4, adding a lithium-rich manganese-based precursor and Li 2 CO 3 Additive Al in an amount of 3000ppm based on the total weight 2 O 3 Uniformly mixing, keeping the temperature at 900 ℃ for 12h, cooling, crushing by a pair of rollers, and sieving to remove magnetism to obtain the lithium-rich manganese-based positive electrode material.
(3) Dissolving La (NO) with the La element being 1 wt% of the lithium-rich manganese-based positive electrode material in mass ratio into ultrapure water, dispersing the lithium-rich manganese-based positive electrode material synthesized in the step (2) into a metal solution, and adding NaBH 4 BH4 of + : stirring the reducing agent with the molar ratio of the La element of 100:50 for 20min, washing, and roasting at 600 ℃ for 6h to obtain the La compound coated and oxygen vacancy modified lithium-rich manganese-based anode material.
The final product obtained is Li 1.167 Ni 0.250 Co 0.025 Mn 0.558 O 2 。
Example 2
The preparation method is the same as example 1, and in the step (3), the La element: the mass ratio of the lithium-rich manganese-based positive electrode material became 2 wt%.
Example 3
The preparation method is the same as example 1, and in the step (3), the La element: the mass ratio of the lithium-rich manganese-based positive electrode material became 0.5 wt%.
Example 4
The preparation method is the same as example 1, and in the step (3), NaBH is added 4 BH4 of + : the molar ratio of La element became 100: 30.
Example 5
The preparation method is the same as example 1, and in the step (3), NaBH is added 4 BH4 of + : the molar ratio of La element became 100: 80.
Example 6
The preparation method was the same as example 1 except that in the step (3), the calcination temperature was changed to 400 ℃.
Example 7
The preparation method was the same as example 1 except that in the step (3), the calcination temperature was changed to 800 ℃.
Example 8
The preparation method is the same as example 1, and the roasting time in the step (3) is changed to 12 h.
Example 9
The preparation method is the same as example 1, and the roasting time in the step (3) is changed into 2 h.
Example 10
The preparation method was the same as example 1, except that La element in step (3) was changed to Al element.
Example 11
The preparation method was the same as example 1, except that the La element in step (3) was replaced with Co.
Comparative example 1
The preparation method was the same as in steps (1) and (2) of example 1, except for step (3).
Comparative example 2
The preparation method is the same as that of example 1, the metal salt is not added in the step (3), pure water is used, and the test method is the same as that of the above example 1.
Evaluation of Performance
And (4) relevant testing: the modified lithium-rich manganese-based lithium ion battery anode material and the metal lithium are used as the cathode material, the assembled battery is tested under the conditions that the discharge cut-off voltage is 2.0V and the charge cut-off voltage is 4.7V, and the test results are shown in Table 1.
TABLE 1
The embodiment, the comparative example and the table 1 show that the modified lithium-rich manganese-based positive electrode material provided by the invention has excellent stability and voltage attenuation resistance effect of the positive electrode material, and can effectively and fundamentally solve the problem of oxygen precipitation in the previous use process of the lithium-rich manganese-based positive electrode material, so that the pain point in the field of the lithium-rich manganese-based positive electrode material is fundamentally solved, and the modified lithium-rich manganese-based positive electrode material is suitable for being popularized in the field of lithium batteries and has a wide development prospect.
Claims (10)
1. A preparation method of a modified lithium-rich manganese-based positive electrode material is characterized by comprising the following steps: the method comprises the following steps: (1) preparing a lithium-rich manganese-based precursor; (2) mixing the precursor and a lithium source; (3) and modifying the lithium-rich manganese base.
2. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 1, characterized in that: the preparation method of the lithium-rich manganese-based precursor comprises the following specific operations: (1) introducing nitrogen into the reaction kettle, adding a dilute ammonia solution serving as a base solution into the reaction kettle through a peristaltic pump, and adding an aqueous solution of metal salt into the reaction kettle according to a certain molar ratio through a coprecipitation method; (2) adding a precipitant solution, continuously stirring and reacting for 20-100 h at the temperature of 45-65 ℃, controlling the pH of a reaction system to be 10.5-11.5, and filtering, washing and drying precipitate crystals generated by the reaction to obtain a precursor.
3. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 2, characterized in that: the metal salt is at least one of sulfate, carbonate and nitrate of nickel, cobalt and manganese metals.
4. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 3, characterized in that: the compound molecular formula of nickel, cobalt and manganese in the metal salt is Ni a Co b Mn c Wherein a is more than or equal to 0.10 and less than or equal to 0.50, b is more than or equal to 0.05, c is more than or equal to 0.50 and less than or equal to 0.90, and the total amount of a + b + c is 1.
5. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 4, characterized in that: the specific operation of mixing the precursor and the lithium source is as follows: (1) uniformly mixing the precursor with a lithium source and an additive; (2) heating to 300-1000 ℃, reacting for 5-20 hours under heat preservation, cooling, sieving and demagnetizing to obtain the matrix material.
6. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 5, characterized in that: the lithium source is at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium chloride and lithium oxalate.
7. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 6, characterized in that: the molar ratio of lithium in the lithium source to metal ions in the precursor is (1.1-1.5): 1.
8. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 7, characterized in that: the additive is at least one of oxide, hydroxide and inorganic acid salt containing Al, Mg, Ti, Y, La and Ce elements.
9. The preparation method of the modified lithium-rich manganese-based positive electrode material according to claim 8, wherein the preparation method comprises the following steps: the specific operation of the modification and modification of the lithium-rich manganese base is as follows: (1) dissolving a modifier in ethanol or ultrapure water, dispersing the base material in the modifier solution, and stirring for 10-60 min; (2) adding a reducing agent, washing, and calcining at 200-800 ℃ for 1-20 hours to obtain the catalyst.
10. The application of the preparation method of the modified lithium-rich manganese-based positive electrode material as claimed in any one of claims 1 to 9 is characterized in that: the method is applied to the process for preparing the anode and cathode materials of the lithium battery.
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