CN113307309A - Method for improving cycle performance of ternary cathode material of lithium ion battery through conversion of lithium fluoride coating layer - Google Patents
Method for improving cycle performance of ternary cathode material of lithium ion battery through conversion of lithium fluoride coating layer Download PDFInfo
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Abstract
The invention discloses a method for improving the cycle performance of a ternary cathode material of a lithium ion battery by converting a lithium fluoride coating layer. Mixing a fluoride ethanol solution, a lithium salt ethanol solution and a lithium ion battery ternary positive electrode material, reacting at a constant temperature, filtering, washing to obtain filter residues, drying the filter residues, carrying out low-temperature heat treatment, and isolating the ternary positive electrode material from an electrolyte by using a composite coating layer, so that corrosion and dissolution of HF possibly existing in the electrolyte to the electrode material are avoided, and the cycle performance of the ternary positive electrode material is improved. The doping of fluorine increases the unit cell volume of the ternary material, provides a larger diffusion channel for the diffusion of lithium ions, is beneficial to improving the rate capability and the crystal structure stability of the ternary material, and the conversion of lithium fluoride into the ternary material provides two functions of coating and doping, thereby improving the electrochemical performance of the ternary anode material. The preparation method is simple in preparation process, environment-friendly, simple in operation method and high in application value.
Description
Technical Field
The invention belongs to the technical field of new energy materials, and particularly relates to a method for improving the cycle performance of a ternary cathode material of a lithium ion battery by realizing surface coating and doping synergistic functions through lithium fluoride conversion.
Background
LiCoO which is widely used as the anode material of the lithium ion battery at present2Compared with the prior art, the ternary cathode material has the obvious advantages of high capacity and low cost, is the development key point of the current lithium ion battery cathode material, and the cycle performance of the ternary cathode material still needs to be improved continuously. The poor cycle performance of the ternary positive electrode material mainly falls into the following two aspects: (1) electrolyte LiPF6HF generated by decomposition corrodes the electrode material, so that the active material is dissolved or falls off, and the cycle performance of the ternary cathode material is continuously deteriorated; (2) the instability of the crystal structure of the active material leads to a decrease in the cycling performance of the electrode material. For the reasons, a great deal of research shows that the surface coating, doping and the combination of the surface coating and the doping can improve the cycle performance of the ternary cathode material, but the single surface coating or doping method cannot obviously improve the cycle performance of the ternary cathode material, and the existing surface coating and doping combination method is too complex and needs to be completed through the steps of doping and surface coating in sequence. The invention simultaneously realizes two functions of surface coating and doping through a single step, and the ternary cathode material is isolated from the electrolyte by the surface coating layer, so that the corrosion and the dissolution of HF possibly generated in the electrolyte to the active material are avoided, and the cycle performance of the ternary cathode material is improved. The fluorine doping of the ternary cathode material improves the stability of the crystal structure of the ternary cathode material, widens the diffusion channel of lithium ions, improves the diffusion dynamic performance of the lithium ions, improves the rate capability and the cycle performance of the material, and obviously improves the cycle performance of the ternary cathode material.
Disclosure of Invention
The invention aims to provide a method for improving the cycle performance of a ternary cathode material of a lithium ion battery by converting a lithium fluoride coating layer, aiming at the defect of poor cycle performance of the ternary cathode material, the lithium fluoride coating layer coated on the surface of the ternary cathode material is subjected to heat treatment, so that lithium fluoride is partially converted into lithium oxide and fluorine doped into the ternary cathode material, the ternary cathode material coated with the lithium fluoride is converted into the fluorine doped ternary cathode material coated with a lithium fluoride/lithium oxide compound, and the ternary cathode material has excellent cycle performance and rate capability.
The method comprises the following specific steps:
(1) dissolving 0.0029-0.0119 g of fluoride in 20-30 mL of absolute ethanol to form a fluoride ethanol solution; dissolving 0.007 to 0.043g of lithium salt in 20 to 30mL of absolute ethanol to form a lithium salt ethanol solution.
(2) Uniformly mixing the fluoride ethanol solution and the lithium salt ethanol solution obtained in the step (1) with 1.000-2.000 g of ternary cathode material powder, placing the mixed solution in a constant temperature device, reacting for 0.5-3 hours while stirring, filtering the mixed solution, washing with ethanol and distilled water to obtain filter residue, and drying the filter residue.
(3) And (3) placing the filter residue dried in the step (2) in an air atmosphere or an oxygen atmosphere, heating to 350-500 ℃, keeping the temperature for 2-8 hours, and cooling to obtain the fluorine-doped ternary cathode material coated with the lithium fluoride/lithium oxide compound.
The fluoride is one or more of ammonium fluoride, ammonium bifluoride, sodium fluoride, potassium fluoride and potassium bifluoride.
The lithium salt is one or more of lithium nitrate, lithium acetate, lithium chloride, lithium bromide and lithium sulfate.
The ternary positive electrode material is LiNi1-x-yCoxAlyO2(x>0，y>0 and x + y<1) And LiNi1-x-yCoxMnyO2(x>0，y>0 and x + y<1) One or two of them.
The method realizes two functions of surface coating and doping by using a single heat treatment step at a lower temperature, obviously improves the cycle performance and the rate capability of the ternary cathode material, and has the advantages of simple process, environmental protection and great application value.
Drawings
FIG. 1 shows LiF/Li obtained in example 1 of the present invention2O-coated fluorine-doped LiNi0.8Co0.1Al0.1O2XRD pattern of the material.
FIG. 2 shows LiF/Li obtained in example 2 of the present invention2O-coated fluorine-doped LiNi0.9Co0.05Al0.05O2XRD pattern of the material.
FIG. 3 shows LiF/Li obtained in example 2 of the present invention2O-coated fluorine-doped LiNi0.9Co0.05Al0.05O2SEM image of material.
FIG. 4 shows LiF/Li obtained in example 2 of the present invention2O-coated fluorine-doped LiNi0.9Co0.05Al0.05O2First charge and discharge curves for material 0.5C.
FIG. 5 shows LiF/Li obtained in example 2 of the present invention2O-coated fluorine-doped LiNi0.9Co0.05Al0.05O2And (3) an electrochemical cycle performance diagram of the material at a current density of 0.5C.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Example 1:
(1) 0.0038g of ammonium fluoride was dissolved in 20mL of anhydrous ethanol to form an ethanol solution of ammonium fluoride. 0.007g of lithium nitrate was dissolved in 20mL of anhydrous ethanol to form an ethanol solution of lithium nitrate.
(2) Mixing the ammonium fluoride ethanol solution, the lithium nitrate ethanol solution and 1.000g LiNi obtained in the step (1)0.8Co0.1Al0.1O2Adding into 100mL volumetric flask, dispersing and mixing by ultrasonic wave, transferring the mixed solution into 40 deg.C constant temperature water bath, reacting for 2 hr while stirring, filtering, washing with anhydrous ethanol and distilled water, and oven drying the filter residueAnd (5) drying.
(3) And (3) placing the filter residue dried in the step (2) in a tubular furnace, introducing nitrogen, heating to 350 ℃, keeping the temperature for 4 hours, and cooling to obtain the fluorine-doped LiNi coated with the lithium fluoride/lithium oxide compound0.8Co0.1Al0.1O2. FIG. 1 is a fluorine-doped LiNi coated lithium fluoride/lithium oxide composite0.8Co0.1Al0.1O2XRD pattern of (a).
Fluorine-doped LiNi coated with lithium fluoride/lithium oxide composite as positive electrode material of lithium ion battery0.8Co0.1Al0.1O2The acetylene black and the PVDF are ground and mixed uniformly according to the mass ratio of 8:1:1, a proper amount of NMP is dripped to prepare electrode slurry, then the electrode slurry is coated on an aluminum foil uniformly, the aluminum foil is placed in a vacuum drying box at 120 ℃ for full drying, and a roll machine is used for compacting and cutting the aluminum foil into a wafer electrode with the diameter of 15 mm. The obtained wafer electrode was used as a positive electrode, a lithium metal plate was used as a negative electrode, and 1mol/L LiPF was used6The polycarbonate solution of (2) was used as an electrolyte, and the separator was a PVDF separator, which was assembled into a CR2016 type button cell in a glove box filled with dry, high-purity argon gas (both moisture and oxygen contents were less than 0.1 ppm). The button cell is placed on a cell test system to test the charge and discharge performance at room temperature, when the current density is 0.2C (44mA/g) and the charge and discharge voltage range is 2.8-4.3V (vs. Li)+Li), the first reversible discharge capacity is 198mAh/g, and after 50 times of circulation, the capacity is 190 mAh/g. And under the same charging and discharging test conditions, the LiNi which is not coated and treated0.8Co0.1Al0.1O2The discharge capacity of (2) is 200mAh/g, and after 50 times of circulation, the capacity is only 180 mAh/g.
Example 2:
(1) 0.0029g of ammonium bifluoride was dissolved in 20mL of absolute ethanol to form an ethanol solution of ammonium bifluoride. 0.0043g of lithium chloride was weighed out and dissolved in 20mL of absolute ethanol to form an ethanol solution of lithium chloride.
(2) Mixing the ammonium bifluoride ethanol solution, the chlorine lithium ethanol solution and 2.000g LiNi obtained in the step (1)0.9Co0.05Al0.05O2Into a 100mL volumetric flask and byUltrasonically dispersing, uniformly mixing, transferring the mixed solution into a constant-temperature water bath kettle at 40 ℃, reacting for 1 hour while stirring, carrying out suction filtration on the mixed solution, washing with absolute ethyl alcohol and distilled water respectively, and drying filter residues.
(3) And (3) placing the filter residue dried in the step (2) in a tubular furnace, introducing nitrogen, heating to 400 ℃, keeping the temperature for 4 hours, and cooling to obtain the fluorine-doped LiNi coated with the lithium fluoride/lithium oxide compound0.9Co0.05Al0.05O2. FIG. 2 is a fluorine-doped LiNi coated lithium fluoride/lithium oxide composite0.9Co0.05Al0.05O2FIG. 3 is a diagram showing a lithium fluoride/lithium oxide composite-coated fluorine-doped LiNi0.9Co0.05Al0.05O2SEM image of (d).
Fluorine-doped LiNi coated with the prepared lithium fluoride/lithium oxide composite of the lithium ion battery anode material0.9Co0.05Al0.05O2The acetylene black and the PVDF are ground and mixed uniformly according to the mass ratio of 8:1:1, a proper amount of NMP is dripped to prepare electrode slurry, then the electrode slurry is uniformly coated on an aluminum foil, the aluminum foil is placed in a vacuum drying box at 120 ℃ for full drying, and a roll machine is used for compacting and cutting the electrode into a wafer electrode with the diameter of 15 mm. The prepared positive plate is used as a positive electrode, a lithium metal plate is used as a negative electrode, and 1mol/L LiPF6The polycarbonate solution of (2) was used as an electrolyte, and the separator was a PVDF separator, and a CR2016 type button cell was mounted in a glove box (both moisture and oxygen contents were less than 0.1ppm) filled with dry, high-purity argon gas. The button cell is placed on a cell test system to test the charge and discharge performance at room temperature, when the current density is 0.2C (44mA/g) and the charge and discharge voltage range is 2.8-4.3V (vs. Li)+Li), the first reversible discharge capacity is 204 mAh/g, and after 50 times of circulation, the capacity is 198 mAh/g. FIGS. 4 and 5 are respectively a lithium fluoride/lithium oxide composite-coated fluorine-doped LiNi0.9Co0.05Al0.05O2Corresponding first charge-discharge curve and cycle performance curve. And LiNi0.9Co0.05Al0.05O2Under the same condition, the first discharge capacity is 206mAh/g, and the cycle isAfter 50 times, the capacity is only 180 mAh/g.
Example 3:
(1) 0.0119g of sodium fluoride was dissolved in 30mL of anhydrous ethanol to form an ethanol solution of sodium fluoride. 0.0224g of lithium sulfate was dissolved in 30mL of anhydrous ethanol to form a lithium chloride ethanol solution.
(2) The ammonium bifluoride ethanol solution, the chlorine lithium ethanol solution and 1.000g LiNi which are obtained in the step (1)0.8Co0.1Mn0.1O2Adding into a 100mL volumetric flask, dispersing by ultrasonic wave, mixing uniformly, transferring the mixed solution into a 50 ℃ constant-temperature water bath kettle, reacting for 2 hours while stirring, filtering the mixed solution, washing with absolute ethyl alcohol and distilled water respectively, and drying the filter residue.
(3) And (3) placing the filter residue dried in the step (2) in a tubular furnace, introducing nitrogen, heating to 450 ℃, keeping the temperature for 3 hours, and cooling to obtain the fluorine-doped LiNi coated with the lithium fluoride/lithium oxide compound0.8Co0.1Mn0.1O2。
Fluorine-doped LiNi coated with the obtained lithium fluoride/lithium oxide composite for the positive electrode material of the lithium ion battery0.8Co0.1Mn0.1O2The acetylene black and the PVDF are ground and mixed uniformly according to the mass ratio of 8:1:1, a proper amount of NMP is dripped to prepare electrode slurry, then the electrode slurry is coated on an aluminum foil uniformly, the aluminum foil is placed in a vacuum drying box at 120 ℃ for full drying, and a roll machine is used for compacting and cutting the aluminum foil into a wafer electrode with the diameter of 15 mm. The obtained disk electrode was used as a positive electrode, a metal lithium plate was used as a negative electrode, and 1mol/L LiPF was used6The polycarbonate solution of (2) was used as an electrolyte, and the separator was a PVDF separator, and a CR2016 type button cell was mounted in a glove box (both moisture and oxygen contents were less than 0.1ppm) filled with dry, high-purity argon gas. The button cell is placed on a cell test system to test the charge and discharge performance at room temperature, when the current density is 0.2C (44mA/g) and the charge and discharge voltage range is 2.8-4.3V (vs. Li)+Li), the first reversible discharge capacity is 184mAh/g, and after 50 times of circulation, the capacity is 179 mAh/g. And under the same charging and discharging test conditions, the LiNi which is not coated and treated0.8Co0.1Mn0.1O2The discharge capacity of (2) is 186mAh/g, and after 50 times of circulation, the capacity is only 170 mAh/g.
Since many embodiments of the invention are possible, it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (1)
1. A method for improving the cycle performance of a ternary cathode material of a lithium ion battery through conversion of a lithium fluoride coating layer is characterized by comprising the following specific steps:
(1) dissolving 0.0029-0.0119 g of fluoride in 20-30 mL of absolute ethanol to form a fluoride ethanol solution; dissolving 0.007-0.043 g of lithium salt in 20-30 mL of absolute ethanol to form a lithium salt ethanol solution;
(2) uniformly mixing the fluoride ethanol solution and the lithium salt ethanol solution obtained in the step (1) with 1.000-2.000 g of ternary cathode material powder, placing the mixed solution in a constant temperature device, reacting for 0.5-3 hours while stirring, filtering the mixed solution, washing with ethanol and distilled water to obtain filter residue, and drying the filter residue;
(3) placing the filter residue dried in the step (2) in an air atmosphere or an oxygen atmosphere, heating to 350-500 ℃, keeping the temperature for 2-8 hours, and cooling to obtain a fluorine-doped ternary cathode material coated with a lithium fluoride/lithium oxide compound;
the fluoride is one or more of ammonium fluoride, ammonium bifluoride, sodium fluoride, potassium fluoride and potassium bifluoride;
the lithium salt is one or more of lithium nitrate, lithium acetate, lithium chloride, lithium bromide and lithium sulfate;
the ternary positive electrode material is LiNi1-x-yCox Al yO2Wherein: x is the number of>0，y>0 and x + y<1 and LiNi1-x-yCoxMnyO2Wherein x is>0，y>0 and x + y<1 or two of them.
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| CN114373902A (en) * | 2021-11-25 | 2022-04-19 | 西安交通大学 | Method for preparing ternary NCM with fluoride-coated surface, NCM and electrode |
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Application publication date: 20210827 |