CN115528239B - Modified lithium manganate and preparation method and application thereof - Google Patents
Modified lithium manganate and preparation method and application thereof Download PDFInfo
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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
- H01M4/50—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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1235—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]2-, e.g. Li2Mn2O4, Li2[MxMn2-x]O4
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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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- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of lithium batteries, and particularly relates to modified lithium manganate and a preparation method and application thereof. The invention provides modified lithium manganate, which has a molecular formula shown as a formula I: li a Mn 2‑ b Al b F c O 4‑c Formula I; wherein a is more than or equal to 1.05 and less than or equal to 1.12, b is more than or equal to 0.04 and less than or equal to 0.1, and c is more than or equal to 0.01 and less than or equal to 0.04. Aluminum and fluorine are doped in the lithium manganate, and the fluorine in the modified lithium manganate partially replaces oxygen, so that the strength of chemical bonds is improved, and the high-temperature performance of the modified lithium manganate is improved. Al in modified lithium manganate 3+ And F ‑ The binary ions make the main structure of lithium manganate keep stable, al 3+ Partially replacing Mn by entering modified lithium manganate crystal lattice 3+ The position reduces the crystal lattice parameter of the lithium manganate spinel and increases Mn in the lithium manganate crystal 4+ The relative content of the modified lithium manganate reduces the Jahn-Teller effect, effectively stabilizes the lithium manganate spinel structure and obviously improves the high-temperature cycle performance of the modified lithium manganate.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to modified lithium manganate and a preparation method and application thereof.
Background
Lithium ion batteries are a new generation of green, environment-friendly and renewable chemical energy with excellent performance, and currently, the lithium ion batteries rapidly occupy the application fields of mobile phones, notebook computers, small video cameras, digital cameras, electric tools, electric automobiles and the like with incomparable advantages of other batteries, and can possibly replace cadmium nickel and hydrogen nickel batteries for the aerospace field. The market of lithium batteries is going to grow explosively without doubt, and the demand of lithium battery materials is certainly driven by the rapid expansion of the yield of electric vehicles. The cathode material is one of the key materials for manufacturing lithium ion batteries. Currently, the anode materials of commercial lithium ion batteries mainly include lithium cobaltate, spinel lithium manganate, nickel-cobalt-manganese ternary composite materials and lithium iron phosphate. Lithium cobaltate is expensive, has poor safety performance and large environmental pollution, and cannot be applied to power batteries; the nickel-cobalt-manganese ternary composite material has poor cycle stability and unsatisfactory safety performance; the lithium iron phosphate has poor synthesis consistency, low volume specific capacity and poor conductivity; the spinel type lithium manganate has the advantages of rich resources, low price, high energy density, no pollution, easy recovery, good safety and the like, is considered to be the lithium ion battery anode material with the greatest development prospect, and has stronger advantages particularly in the aspect of power supply.
However, when a lithium ion battery using spinel lithium manganate as a positive electrode material is cycled, especially when electrochemical cycling is performed at a high temperature (above 55 ℃), jahn-Teller effect occurs, so that the crystal structure is distorted, and the high-temperature capacity of lithium manganate is rapidly attenuated, thereby reducing the cycle performance of the lithium battery.
Disclosure of Invention
In view of the above, the invention provides modified lithium manganate and a preparation method and application thereof.
In order to solve the technical problems, the invention provides modified lithium manganate, which has a molecular formula shown as a formula I:
Li a Mn 2-b Al b F c O 4-c formula I;
wherein a is more than or equal to 1.05 and less than or equal to 1.12, b is more than or equal to 0.04 and less than or equal to 0.1, and c is more than or equal to 0.01 and less than or equal to 0.04.
Preferably, the modified lithium manganate has a molecular formula shown in any one of formulas 1 to 3:
Li 1.11 Mn 1.947 Al 0.053 F 0.018 O 3.982 formula 1,Li 1.1 Mn 1.946 Al 0.054 F 0.024 O 3.976 Formula 2,Li 1.08 Mn 1.945 Al 0.055 F 0.03 O 3.97 And (4) formula 3.
The invention also provides a preparation method of the modified lithium manganate in the technical scheme, which comprises the following steps:
mixing electrolytic manganese dioxide, lithium carbonate, cone cryolite and an aluminum source to obtain a mixed material;
and sintering the mixed material to obtain the modified lithium manganate.
Preferably, the molar ratio of the electrolytic manganese dioxide to the tapered cryolite is 100 (0.075-0.25).
Preferably, the aluminum source comprises one or more of boehmite, pseudoboehmite, aluminum hydroxide, and alumina.
Preferably, the molar ratio of the manganese element in the electrolytic manganese dioxide to the aluminum element in the aluminum source is 40 (0.5-1.2).
Preferably, the molar ratio of the electrolytic manganese dioxide to the lithium carbonate is 4 (1.05-1.15).
Preferably, the mixing is carried out in an inclined ball mill, the rotating speed of the mixing is 18-25 r/min, the ball-material ratio of the mixing is (1.3-2): 1, and the mixing time is 90-180 min.
Preferably, the sintering temperature is 700-750 ℃; the sintering heat preservation time is 10-15 h.
The invention also provides application of the modified lithium manganate prepared by the technical scheme or the preparation method in the technical scheme in a battery anode material.
The invention provides modified lithium manganate, which has a molecular formula shown as a formula I: li a Mn 2-b Al b F c O 4-c Formula I; wherein a is more than or equal to 1.05 and less than or equal to 1.12, b is more than or equal to 0.04 and less than or equal to 0.1, and c is more than or equal to 0.01 and less than or equal to 0.04. According to the invention, aluminum and fluorine are doped in the lithium manganate, and the fluorine in the modified lithium manganate partially replaces oxygen, so that the strength of chemical bonds is improved, and the high-temperature performance of the modified lithium manganate is improved. Al in modified lithium manganate 3+ And F - The binary ions make the main structure of lithium manganate keep stable, al 3+ Entering into modified lithium manganate crystal lattice to partially replace Mn 3+ The lattice parameter of the lithium manganate spinel is reduced, and Mn in the lithium manganate crystal is increased 4+ The relative content of the modified lithium manganate reduces the Jahn-Teller effect, effectively stabilizes the lithium manganate spinel structure and obviously improves the high-temperature cycle performance of the modified lithium manganate.
The invention provides a preparation method of modified lithium manganate according to the technical scheme, which comprises the following steps: mixing electrolytic manganese dioxide, lithium carbonate, cone cryolite and an aluminum source to obtain a mixed material; and sintering the mixed material to obtain the modified lithium manganate. The invention takes the electrolytic manganese dioxide and lithium carbonate with low price as main raw materials and the chiolite as a sintering aid, thus reducing the energy required by solid-phase synthesis of lithium manganate, further reducing the sintering temperature and the sintering time and further reducing the production cost. Meanwhile, the chiolite provides a fluorine source for the modified lithium manganate and part of aluminum sources perform binary modified doping on the lithium manganate, so that the high-temperature cycle performance of the modified lithium manganate is improved.
Detailed Description
The invention provides modified lithium manganate, which has a molecular formula shown as a formula I:
Li a Mn 2-b Al b F c O 4-c a formula I;
wherein a is more than or equal to 1.05 and less than or equal to 1.12, b is more than or equal to 0.04 and less than or equal to 0.1, and c is more than or equal to 0.01 and less than or equal to 0.04; preferably 1.08-a 1.11, 0.05-b 0.07, 0.015-c 0.03.
In the invention, the molecular formula of the modified lithium manganate is preferably as shown in any one of formulas 1 to 3:
Li 1.11 Mn 1.947 Al 0.053 F 0.018 O 3.982 formula 1,Li 1.1 Mn 1.946 Al 0.054 F 0.024 O 3.976 Formula 2,Li 1.08 Mn 1.945 Al 0.055 F 0.03 O 3.97 And (3) formula.
The invention utilizes Al 3+ And F - The binary ions carry out double doping modification on lithium manganate, and Al 3+ Entering into modified lithium manganate crystal lattice to partially replace Mn 3+ The crystal lattice parameter of spinel is reduced, and Mn in lithium manganate crystal is increased 4+ The relative content of the lithium manganate improves the stability of the structure of the modified lithium manganate, so that the modified lithium manganate has good cycling stability at high temperature.
The invention also provides a preparation method of the modified lithium manganate in the technical scheme, which comprises the following steps:
mixing electrolytic manganese dioxide, lithium carbonate, chiolite and an aluminum source to obtain a mixed material;
and sintering the mixed material to obtain the modified lithium manganate.
The method comprises the step of mixing electrolytic manganese dioxide, lithium carbonate, chiolite and an aluminum source to obtain a mixed material. In the invention, the molecular formula of the conoid cryolite is shown asNa 3 AlF 6 . In the present invention, the aluminum source preferably comprises one or more of boehmite, pseudoboehmite, aluminum hydroxide and alumina, more preferably aluminum hydroxide or alumina. In the present invention, when the aluminum source is two or more of the above-mentioned specific substances, the ratio of the specific substances in the present invention is not particularly limited, and any ratio may be used.
In the present invention, the molar ratio of the electrolytic manganese dioxide to the lithium carbonate is preferably 4 (1.05 to 1.15), and more preferably 4 (1.08 to 1.12). In the present invention, the molar ratio of the electrolytic manganese dioxide to the chiolite is preferably (0.075 to 0.25) 100, and more preferably (0.1 to 0.125) 100. In the present invention, the molar ratio of the manganese element in the electrolytic manganese dioxide to the aluminum element in the aluminum source is preferably (40) (0.5 to 1.2), and more preferably 40.
In the present invention, the mixing is preferably carried out in an inclined ball mill, and the rotation speed of the mixing is preferably 18 to 25r/min, more preferably 20 to 22r/min; the mixed ball-material ratio is preferably (1.3-2) to 1, more preferably (1.5-1.8) to 1; the mixing time is preferably 90 to 180min, more preferably 100 to 120min. In the present invention, the milling balls for mixing are preferably agate balls.
The invention takes the electrolytic manganese dioxide as the raw material, and the electrolytic manganese dioxide has low price and can reduce the production cost. The invention takes the tapered cryolite as the sintering aid, which can reduce the subsequent sintering time and the subsequent sintering temperature, thereby improving the production efficiency and reducing the processing cost; meanwhile, the conoid cryolite is used as a sintering aid, and a fluorine source and a part of an aluminum source are provided, so that the production cost is further saved.
After the mixed material is obtained, sintering the mixed material to obtain the modified lithium manganate. In the invention, the sintering temperature is preferably 700-750 ℃, and more preferably 710-740 ℃; the heat preservation time for sintering is preferably 10 to 15 hours, and more preferably 11 to 14 hours.
In the invention, high-temperature solid-phase synthesis reaction can occur in the sintering process to generate lithium manganate.
In the present invention, the sintered material preferably further comprises: and sieving the sintered product, and taking the undersize product. In the present invention, the mesh size of the sieving screen is preferably 200 to 400 mesh, and more preferably 280 to 300 mesh.
The invention also provides application of the modified lithium manganate prepared by the technical scheme or the modified lithium manganate prepared by the preparation method of the technical scheme in battery positive electrode materials. The application mode of the invention is not particularly limited, and the battery anode material can be prepared according to the conventional method in the field.
In order to further illustrate the present invention, the following technical solutions provided by the present invention are described in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Placing 4mol of electrolytic manganese dioxide, 1.11mol of lithium carbonate, 0.003mol of conical cryolite and 0.05mol of aluminum hydroxide in an inclined ball mill, and mixing (taking agate balls as grinding balls, and the ball-to-material ratio is 1.5) for 120min at the rotating speed of 18r/min to obtain a mixed material;
sintering the mixed material at 740 ℃ for 10h, sieving by using a mesh sieve with the aperture of 300 meshes, and taking undersize to obtain modified lithium manganate with the molecular formula of Li 1.11 Mn 1.947 Al 0.053 F 0.018 O 3.982 。
Example 2
Placing 4mol of electrolytic manganese dioxide, 1.1mol of lithium carbonate, 0.004mol of cone cryolite and 0.05mol of alumina in an inclined ball mill, and mixing (taking agate balls as grinding balls and the ball-to-material ratio of 1.5: 1) at the rotating speed of 20r/min for 100min to obtain a mixed material;
sintering the mixed material at 720 ℃ for 12h, sieving by using a mesh sieve with the aperture of 300, and taking undersize to obtain modified lithium manganate with the molecular formula of Li 1.1 Mn 1.946 Al 0.054 F 0.024 O 3.976 。
Example 3
Placing 4mol of electrolytic manganese dioxide, 1.08mol of lithium carbonate, 0.005mol of conical cryolite and 0.05mol of aluminum hydroxide in a high-speed mixer, and mixing (taking agate balls as grinding balls, and the ball-to-material ratio is 1.5) for 110min at the rotating speed of 20r/min to obtain a mixed material;
sintering the mixed material at 700 ℃ for 14h, sieving by using a mesh sieve with the aperture of 280 ℃, and taking undersize to obtain modified lithium manganate with the molecular formula of Li 1.08 Mn 1.945 Al 0.055 F 0.03 O 3.97 。
Comparative example 1
Putting electrolytic manganese dioxide and lithium carbonate into an inclined ball mill according to the molar ratio of manganese element in the electrolytic manganese dioxide to lithium element in the lithium carbonate being 2; and sintering the mixed material obtained by ball milling and mixing at 800 ℃ for 20h in an air atmosphere, and cooling and discharging to obtain the lithium manganate.
Test example
18650 lithium batteries were prepared according to a conventional method using the lithium manganate obtained in examples 1 to 3 and comparative example 1 as a positive electrode material.
The gram capacity and 55 ℃ 1C cycle performance of the cell after assembly were tested and the results are shown in table 1. TABLE 1 high temperature cycle performance of batteries manufactured using lithium manganate manufactured in examples 1 to 3 and comparative example
| Examples | Gram capacity (mAh/g) | Cycle number (times) at 55 DEG C |
| Example 1 | 120 | 300 |
| Example 2 | 123 | 285 |
| Example 3 | 126 | 270 |
| Comparative example 1 | 116 | 200 |
As can be seen from Table 1, the modified lithium manganate provided by the invention has good high-temperature cycle performance.
The quality and power consumption of lithium carbonate used for preparing 1 ton of modified lithium manganate was calculated by preparing modified lithium manganate by the preparation methods of examples 1 to 3, and the results are shown in Table 2.
Table 2 lithium carbonate usage and power consumption of examples 1 to 3 and comparative example 1
As can be seen from table 2, the preparation method provided by the invention can reduce the lithium carbonate dosage by 1.8-5.4%, and reduce the power consumption by 25% (the sintering temperature can be reduced by 7.5-12.5%, and the sintering time can be reduced by 30-50%) compared with the lithium carbonate dosage of the traditional lithium manganate preparation method; greatly reducing the production cost.
The power consumption is saved, and the modified lithium manganate prepared by the preparation method provided by the invention has lower production cost.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (9)
1. A modified lithium manganate has a molecular formula shown as a formula I:
Li a Mn 2-b Al b F c O 4-c a formula I;
wherein a is more than or equal to 1.05 and less than or equal to 1.12, b is more than or equal to 0.04 and less than or equal to 0.1, and c is more than or equal to 0.01 and less than or equal to 0.04;
the preparation method of the modified lithium manganate comprises the following steps:
electrolyzing manganese dioxide, lithium carbonate and Na 3 AlF 6 Mixing the aluminum source and the mixture to obtain a mixed material; the aluminum source comprises one or more of boehmite, pseudo-boehmite, aluminum hydroxide and alumina;
and sintering the mixed material to obtain the modified lithium manganate.
2. The modified lithium manganate of claim 1, wherein said modified lithium manganate has a molecular formula as shown in any one of formulas 1 to 3:
Li 1.11 Mn 1.947 Al 0.053 F 0.018 O 3.982 in the formula 1, the compound is shown in the specification,
Li 1.1 Mn 1.946 Al 0.054 F 0.024 O 3.976 in the formula (2), the first and second groups,
Li 1.08 Mn 1.945 Al 0.055 F 0.03 O 3.97 and (3) formula.
3. The process for producing modified lithium manganate according to claim 1 or 2, comprising the steps of:
electrolyzing manganese dioxide, lithium carbonate and Na 3 AlF 6 Mixing the aluminum source and the aluminum source to obtain a mixed material; the aluminum source comprises one or more of boehmite, pseudo-boehmite, aluminum hydroxide and alumina;
and sintering the mixed material to obtain the modified lithium manganate.
4. According toThe method according to claim 3, wherein said electrolytic manganese dioxide and Na 3 AlF 6 The molar ratio of (2) to (2) is 100 (0.075-0.25).
5. The method according to claim 3, wherein the molar ratio of the manganese element in the electrolytic manganese dioxide to the aluminum element in the aluminum source is 40 (0.5 to 1.2).
6. The production method according to claim 3, wherein the molar ratio of the electrolytic manganese dioxide to the lithium carbonate is 4 (1.05 to 1.15).
7. The preparation method according to claim 3, characterized in that the mixing is carried out in a slant ball mill, the rotation speed of the mixing is 18-25 r/min, the ball material ratio of the mixing is (1.3-2): 1, and the mixing time is 90-180 min.
8. The method according to claim 3, wherein the sintering temperature is 700-750 ℃; the sintering heat preservation time is 10-15 h.
9. Use of the modified lithium manganate according to claim 1 or 2 or prepared by the method according to any one of claims 3 to 8 in a battery positive electrode material.
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