CN113130867A - Preparation method of lithium ion battery cathode material and material thereof - Google Patents
Preparation method of lithium ion battery cathode material and material thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
The invention relates to the technical field of lithium battery materials, in particular to a preparation method of a lithium ion battery cathode material and a material thereof, the lithium ion battery cathode material is transition metal oxide intercalated graphite, and the transition metal oxide is positioned between layers of the graphite, so that the transition metal oxide has larger interlayer spacing, relatively higher lithium intercalation potential and gram capacity compared with the graphite, and lithium ions can be better de-intercalated at low temperature; the preparation method adopts an in-situ synthesis method, the organic salt of the transition metal reacts with the graphite, the transition metal is introduced between graphite layers and is converted into metal oxide through oxidation and calcination, and the transition metal oxide intercalated graphite composite material is successfully prepared.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a preparation method of a lithium ion battery cathode material and a material thereof.
Background
People have higher and higher requirements on electronic products. Because of the advantages of high energy density, higher voltage platform, longer service life cycle, environmental friendliness and the like, the lithium ion battery is widely applied to more and more electronic products at present and is used as a main energy supply for the portable equipment, besides, the lithium ion battery is also applied to special fields such as aerospace, national defense and military industry, submarines, electric automobiles and the like, but due to poor low-temperature performance, the application of the lithium ion battery in the special fields and even in cold regions is limited, and the performance of the lithium ion battery becomes poor even and the lithium ion battery cannot work normally if the lithium ion battery is below-30 ℃.
The factors for limiting the use of the lithium ion battery at low temperature mainly comprise electrolyte, anode and cathode materials and a diaphragm, while graphite is used as a main cathode material of the lithium ion battery, and the lower lithium intercalation potential is an important factor for influencing the low-temperature charging and lithium precipitation of the lithium ion battery.
The graphite has a stable layered structure and good chemical stability, when the graphite is used as the cathode of a lithium ion battery, side reaction hardly occurs, the interlayer spacing is very close to the diameter of Li +, smooth intercalation can be realized, the stable layered structure can be always maintained in the de-intercalation process, a stable SEI film is formed during the first lithium intercalation, the graphite electrode can be protected, the electrode and electrolyte are isolated, and the loss of the battery capacity is prevented. However, when the battery is charged at a low temperature, the internal polarization of the battery is increased due to the reduction of the ion diffusion rate in the electrolyte, the lithium intercalation potential of the graphite is relatively low, and the interlayer spacing is not changed, so that lithium ions are easily separated from the surface of the graphite to form lithium dendrites, and thus the capacity of the battery is rapidly reduced, the cycle performance is poor, and even potential safety hazards are caused.
At present, the method for modifying low-temperature graphite mainly comprises surface coating and improvement of the interface performance. However, the method cannot fundamentally change the lithium ion intercalation problem of the graphite material at the temperature of-40 ℃ or even lower.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a lithium ion battery cathode material and a material thereof, and the preparation method has the advantages of simple process and easy preparation, and meets the requirement of industrialized production and manufacturing; the cathode material has good low-temperature charge and discharge performance and is safe to use.
The technical scheme adopted by the invention is as follows:
a preparation method of a lithium ion battery negative electrode material comprises the following steps:
s1, performing high-temperature treatment on the expandable graphite, and then placing the expandable graphite in ethanol for ultrasonic dispersion;
s2, mixing the graphite treated by the S1 and the organic salt of the transition metal in an organic solution, stirring and drying;
s3, placing the mixture processed by the S2 in a reaction kettle, replacing the mixture with high-purity inert gas, then filling the high-purity inert gas, sealing, heating and preserving heat, naturally cooling, releasing pressure, taking out, cleaning with organic solution, and drying to obtain the transition metal organic salt intercalated graphite material;
s4, adding the transition metal organic salt intercalated graphite material treated by the S3 into H2O2Heating and preserving heat, naturally cooling, filtering, and drying in a vacuum environment;
and S5, calcining the material treated by the S4 in inert gas to obtain the cathode material.
Further, in S1, heat preservation is carried out for 30-45 min at 900-950 ℃ for high-temperature treatment; the ultrasonic dispersion time is 8-10 h.
Further, in S2, the transition metal organic salt is any one of an organic nickel salt, an organic manganese salt, an organic cobalt salt, and an organic iron salt; the organic solvent is any one or more of acetone, benzene, ether and toluene solution; the stirring time is 5-6 h.
Further, the organic nickel salt is nickel dicyclopentadienyl or nickel diacetone; the organic manganese salt is manganese acetylacetonate or 2-methylcyclopentadienyl tricarboxymanganese; the organic cobalt salt is cobalt acetylacetonate or cobalt acetate tetrahydrate; the organic ferric salt is ferrocene or ferric citrate.
Further, in S3, the high-purity inert gas is any one of nitrogen, argon and neon; the organic cleaning solution is ethanol and/or acetone.
Further, in S3, the number of times of replacement is 3-5 times; filling high-purity inert gas at 2-4 MPa and then sealing; during heating, the heating rate is 3-5 ℃/min, the heating temperature is 100-160 ℃, and the heat preservation time is 8-10 h; the number of cleaning times is 3-5.
Further, in S4, the heating temperature is 100-160 ℃, and the heat preservation time is 8-12 h; the drying temperature is not more than 50 ℃, and the drying time is 6-8 h.
Further, in S5, the inert gas is any one of nitrogen, argon and neon; the calcination temperature is 400-450 ℃, and the calcination time is 1-2 h.
The lithium ion battery cathode material prepared by the preparation method is transition metal oxide intercalated graphite, and the transition metal oxide is positioned between layers of the graphite.
Further, the mass fraction of the metal oxide is 3% to 10%.
The invention has the following beneficial effects:
1. the preparation method has simple process and easy operation, adopts an in-situ synthesis method, and reacts the transition metal organic salt with graphite, introduces transition metal between graphite layers, converts the transition metal into metal oxide through oxidation and calcination, successfully prepares the transition metal oxide intercalated graphite composite material, the prepared material has a stable crystal structure, obtains a composite in which the transition metal organic salt is intercalated between the graphite layers through reaction, and oxidizes the composite to ensure that the composite has larger interlayer spacing, relatively higher lithium intercalation potential and gram capacity compared with the graphite, and the graphite structure does not change greatly, so that the composite can better de-intercalate lithium ions at low temperature, improve the diffusion problem and the low-temperature charging lithium precipitation problem of the lithium ions at low temperature, and can be widely applied.
2. The lithium ion battery cathode material is transition metal oxide intercalated graphite, and the transition metal oxide is positioned between layers of the graphite, so that the graphite has larger interlayer spacing, relatively higher lithium intercalation potential and gram capacity compared with the graphite, and lithium ions can be better de-intercalated at low temperature.
Drawings
Fig. 1 is a schematic structural view of a negative electrode material in example 1 of the present invention;
FIG. 2 is ZCV curves and impedance plots of a lithium battery using the material of example 1 of the present invention as a negative electrode material and a conventional graphite negative electrode lithium battery on the market during charging and discharging;
wherein the content of the first and second substances,
a. ZCV curve when charged at-20 ℃;
b. ZCV curve at-20 ℃ discharge;
c. -a map of total charging impedance at 20 ℃ versus the temperature remaining state of charge SOC;
d. -a plot of total discharge impedance at 20 ℃ versus the temperature remaining state of charge SOC;
FIG. 3 is a graph showing the discharge curves of a lithium battery using the material of example 1 of the present invention as a negative electrode material and a commercially available conventional graphite negative electrode lithium battery at different temperatures,
wherein the content of the first and second substances,
a. the discharge curve diagrams of the lithium battery taking the material in the embodiment 1 as the negative electrode material at different temperatures are shown;
b. the lithium cell (L6) with the material of example 1 of the invention as the negative electrode material is compared to a conventional graphite negative electrode lithium cell (L1) with 0.2C discharge curves at 25 deg.C and-40 deg.C.
Detailed Description
The invention will be further described with reference to the following figures and examples.
The lithium ion battery cathode material is transition metal oxide intercalated graphite, the transition metal oxide is positioned between layers of the graphite, the mass fraction of the metal oxide is 3% -10%, the material has a stable crystal structure, and a transition metal organic salt compound is embedded between the layers of the graphite and then oxidized, so that the material has larger interlayer spacing, relatively higher lithium intercalation potential and gram capacity compared with the graphite, and the graphite structure is not changed greatly, so that the material can better de-intercalate lithium ions at a low temperature, improve the diffusion problem and the low-temperature charging lithium precipitation problem of the lithium ions at the low temperature, and can be widely applied.
Example 1
S1, weighing 12g of expandable graphite, placing the expandable graphite in a high-temperature muffle furnace, treating for 45min at 900 ℃ to obtain expanded graphite, then placing the expanded graphite in ethanol, dispersing for 8h by using ultrasonic waves, and then filtering and drying;
s2, weighing 2.5g of ferrocene, putting the ferrocene and the expanded graphite dispersed in the S1 into 200mL of acetone, stirring for 6 hours to fully mix the ferrocene and the expanded graphite, and then filtering and drying the mixture;
s3, placing the mixture obtained in the step S2 in a 200mL reaction kettle, replacing 5 times with high-purity nitrogen, filling 2MPa of nitrogen, sealing, heating to 120 ℃ at a heating rate of 3 ℃/min, preserving heat for 8 hours, naturally cooling, releasing pressure, taking out, cleaning 3 times with acetone solution, and drying to obtain the ferrocene intercalated graphite material;
s4, adding the ferrocene intercalation graphite material obtained in the S3 into 100mL of H2O2Heating to 150 ℃, keeping the temperature for 10 hours, naturally cooling to room temperature, filtering, and drying in a vacuum environment at the drying temperature of 45 ℃ for 6 hours.
And S5, calcining the material obtained in the step S4 in a nitrogen environment at the temperature of 450 ℃ for 1h to obtain the ferric oxide intercalated graphite material.
Example 2
S1, weighing 12g of expandable graphite, placing the expandable graphite in a high-temperature muffle furnace, treating at 930 ℃ for 40min to obtain expanded graphite, then placing the expanded graphite in ethanol, dispersing for 8h by using ultrasonic waves, and then filtering and drying;
s2, weighing 2.8g of nickelocene, putting the nickelocene and the expanded graphite dispersed in the S1 into 200mL of acetone, stirring for 5 hours to fully mix, and then filtering and drying;
s3, placing the mixture obtained in S2 in a 200mL reaction kettle, replacing 4 times with high-purity nitrogen, filling 4MPa of nitrogen, sealing, heating to 160 ℃ at a heating rate of 5 ℃/min, preserving heat for 9 hours, naturally cooling, releasing pressure, taking out, cleaning 3 times with acetone solution, and drying to obtain the nickelocene intercalation graphite material;
s4, adding the nickelocene intercalation graphite material obtained in S3 into 100mL of H2O2Heating to 150 ℃, keeping the temperature for 12 hours, naturally cooling to room temperature, filtering, and drying in a vacuum environment at the drying temperature of 50 ℃ for 6 hours.
And S5, calcining the material obtained in the step S4 in a nitrogen environment at the temperature of 420 ℃ for 2 hours to obtain the nickel oxide intercalated graphite material.
Example 3
S1, weighing 12g of expandable graphite, placing the expandable graphite in a high-temperature muffle furnace, treating at 930 ℃ for 35min to obtain expanded graphite, then placing the expanded graphite in ethanol, dispersing for 8h by using ultrasonic waves, and then filtering and drying;
s2, weighing 1.2g of cobalt acetylacetonate, placing the cobalt acetylacetonate and the expanded graphite dispersed in the S1 into 200mL of toluene, stirring for 6 hours to fully mix the cobalt acetylacetonate and the expanded graphite, and filtering and drying the mixture;
s3, placing the mixture obtained in the step S2 in a 200mL reaction kettle, replacing the mixture with high-purity nitrogen for 5 times, filling 4MPa of nitrogen, sealing, heating to 150 ℃ at a heating rate of 4 ℃/min, preserving heat for 10 hours, naturally cooling, releasing pressure, taking out, cleaning for 5 times by using an ethanol solution, and drying to obtain the cobalt acetylacetonate intercalated graphite material;
s4, adding the cobalt acetylacetonate intercalated graphite material obtained in the S3 into 100mL of H2O2Heating to 120 ℃, keeping the temperature for 12 hours, naturally cooling to room temperature, filtering, and drying in a vacuum environment at 40 ℃ for 8 hours.
And S5, calcining the material obtained in the step S4 in a nitrogen environment at the temperature of 430 ℃ for 1.5 hours to obtain the cobaltosic oxide intercalated graphite material.
The microstructure test of the material prepared in example 1 is performed, and as a result, referring to fig. 1, it can be seen that the material is a particle intercalation structure, so that the material has larger interlayer spacing, relatively higher lithium intercalation potential and gram capacity compared with graphite, and the material can better de-intercalate lithium ions at low temperature, and is more suitable for being applied in low-temperature special fields compared with the graphite cathode which is commercially available at present.
The negative electrode material prepared in the above example 1 is used as a negative electrode material of a lithium battery to prepare a lithium battery, and compared with a lithium battery using conventional graphite as a negative electrode material, the low-temperature charge and discharge performance test is performed, and the test items and results are shown in fig. 2 to 3.
The preparation method adopts an in-situ synthesis method, the organic salt of the transition metal reacts with the graphite, the transition metal is introduced between graphite layers and is converted into metal oxide through oxidation and calcination, and the transition metal oxide intercalated graphite composite material is successfully prepared. Firstly, after the transition metal is oxidized to generate the transition metal oxide, the interlayer spacing between the graphite is opened, so that the interlayer spacing is increased, and the lithium ion is favorably embedded; and secondly, the transition metal oxide has higher lithium storage capacity, the interlayer distance of graphite which does not form a compound with the transition metal oxide is very close to the diameter of Li < + >, and the interlayer distance of the intercalated graphite increases the interlayer distance of the graphite to a great extent, so that the graphite can more smoothly de-intercalate Li < + >, and especially can better show the effect under the low temperature condition.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a lithium ion battery cathode material is characterized by comprising the following steps:
s1, performing high-temperature treatment on the expandable graphite, and then placing the expandable graphite in ethanol for ultrasonic dispersion;
s2, mixing the graphite treated by the S1 and the organic salt of the transition metal in an organic solution, stirring and drying;
s3, placing the mixture processed by the S2 in a reaction kettle, replacing the mixture with high-purity inert gas, then filling the high-purity inert gas, sealing, heating and preserving heat, naturally cooling, releasing pressure, taking out, cleaning with organic solution, and drying to obtain the transition metal organic salt intercalated graphite material;
s4, adding the transition metal organic salt intercalated graphite material treated by the S3 into H2O2Heating and preserving heat, naturally cooling, filtering, and drying in a vacuum environment;
and S5, calcining the material treated by the S4 in inert gas to obtain the cathode material.
2. The preparation method of the lithium ion battery anode material according to claim 1, characterized in that in S1, heat preservation is carried out at 900-950 ℃ for 30-45 min for high temperature treatment; the ultrasonic dispersion time is 8-10 h.
3. The method according to claim 1, wherein in S2, the transition metal organic salt is any one of an organic nickel salt, an organic manganese salt, an organic cobalt salt, and an organic iron salt; the organic solvent is any one or more of acetone, benzene, ether and toluene solution; the stirring time is 5-6 h.
4. The preparation method of the lithium ion battery anode material according to claim 3, wherein the organic nickel salt is nickelocene or nickel diacetoneacetonate; the organic manganese salt is manganese acetylacetonate or 2-methylcyclopentadienyl tricarboxymanganese; the organic cobalt salt is cobalt acetylacetonate or cobalt acetate tetrahydrate; the organic ferric salt is ferrocene or ferric citrate.
5. The method for preparing the negative electrode material of the lithium ion battery according to claim 1, wherein in S3, the high-purity inert gas is any one of nitrogen, argon and neon; the organic cleaning solution is ethanol and/or acetone.
6. The method for preparing the negative electrode material of the lithium ion battery according to claim 1, wherein in S3, the number of times of replacement is 3-5 times; filling high-purity inert gas at 2-4 MPa and then sealing; during heating, the heating rate is 3-5 ℃/min, the heating temperature is 100-160 ℃, and the heat preservation time is 8-10 h; the number of cleaning times is 3-5.
7. The preparation method of the lithium ion battery anode material according to claim 1, wherein in S4, the heating temperature is 100-160 ℃, and the heat preservation time is 8-12 h; the drying temperature is not more than 50 ℃, and the drying time is 6-8 h.
8. The method for preparing the negative electrode material of the lithium ion battery according to claim 1, wherein in S5, the inert gas is any one of nitrogen, argon and neon; the calcination temperature is 400-450 ℃, and the calcination time is 1-2 h.
9. The lithium ion battery negative electrode material prepared by the preparation method of any one of claims 1 to 8, wherein the negative electrode material is transition metal oxide intercalated graphite, and the transition metal oxide is positioned between layers of the graphite.
10. The lithium ion battery negative electrode material of claim 9, wherein the mass fraction of the metal oxide is 3% to 10%.
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| CN114975926A (en) * | 2022-05-24 | 2022-08-30 | 东莞理工学院 | Double-active-site Prussian blue type sodium ion negative electrode material and preparation method thereof |
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| CN114975926A (en) * | 2022-05-24 | 2022-08-30 | 东莞理工学院 | Double-active-site Prussian blue type sodium ion negative electrode material and preparation method thereof |
| CN114975926B (en) * | 2022-05-24 | 2024-01-26 | 东莞理工学院 | Prussian blue sodium ion negative electrode material with double active sites and preparation method thereof |
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