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CN114142033A - Modified graphite negative electrode material for lithium ion battery - Google Patents

Modified graphite negative electrode material for lithium ion battery Download PDF

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Publication number
CN114142033A
CN114142033A CN202111275162.2A CN202111275162A CN114142033A CN 114142033 A CN114142033 A CN 114142033A CN 202111275162 A CN202111275162 A CN 202111275162A CN 114142033 A CN114142033 A CN 114142033A
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lithium ion
lithium
graphite
ion battery
solid powder
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Inventor
吴正明
胡淑婉
张峥
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Gotion High Tech Co Ltd
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Gotion High Tech Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a modified graphite cathode material for a lithium ion battery, which comprises the following process steps: dissolving a zirconium source and polyvinyl alcohol in deionized water to obtain a solution A; dispersing a certain amount of graphite in the solution A; filtering and collecting solid powder in the solution, and washing until the pH value is neutral; drying the solid powder to obtain the product with ZrO coated on the surface2The graphite solid powder of (4); coating the surface with ZrO2The graphite solid powder is uniformly mixed with a lithium source and sintered to form ZrO2Reacting with lithium salt to form a lithium ion conductor layer and ZrO2Lithium salt enters the graphite laminated structure to form doping; washing with water, and drying. The modified graphite cathode material for the lithium ion battery prepared by the invention has excellent performance, the electrolyte wettability on the surface of the material is high, the first effect of the battery is improved, and the preparation method is prolongedThe cycle life of the battery is prolonged.

Description

Modified graphite negative electrode material for lithium ion battery
Technical Field
The invention relates to the field of new energy materials and lithium ion batteries, in particular to a modified graphite cathode material for a lithium ion battery.
Background
The lithium ion battery has the characteristics of long cycle life, strong cruising ability, high green environmental protection performance and the like, and is one of the most popular secondary batteries in portable electronic products. At present, graphite is the most widely used negative electrode material of lithium ion batteries, and has the advantages of rich resources, stable electrochemical performance, low price, high reversible capacity and the like. But it also has obvious defects, such as poor hydrophilicity of graphite cathode, incomplete wetting of electrolyte; the graphite layers are connected by weak van der waals force, so that the layer structure is easy to damage in the charging and discharging process, graphite is pulverized, falls off and the like, and the cycle performance of the battery is reduced; in the charging and discharging process, the graphite cathode reacts with the electrolyte to generate an SEI film, so that the first coulombic efficiency of the battery is reduced, and the like. Aiming at the problems, the graphite is mainly coated and modified at present.
At present, graphite is coated with metal oxide, and the main methods include atomic layer deposition, hydrolysis, and the like. Hydrolysis is preferred in view of the fact that atomic layer deposition is too costly and does not provide conditions for large scale production. The hydrolysis method has mild conditions, does not need any treatment equipment and has the condition of mass production.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a modified graphite lithium ion battery cathode material which has a remarkable effect of improving various performances of a lithium ion battery.
The invention provides a preparation method of a modified graphite cathode material for a lithium ion battery, which comprises the following steps:
s1, dissolving a certain amount of zirconium source and polyvinyl alcohol in deionized water to obtain a solution A;
s2, dispersing a certain amount of graphite in the solution A, heating at a certain temperature and continuously stirring for a period of time;
s3, filtering and collecting solid powder in the solution A, and washing with hot deionized water until the pH value is neutral;
s4, drying the washed solid powder at a certain temperature for a period of time to obtain the solid powder with the surface coated with ZrO2The graphite solid powder of (4);
s5 coating the surface with ZrO2The graphite solid powder and a lithium source are uniformly mixed according to a certain proportion and are put in an inert gas atmosphereSintering at 700 ℃ for 10 h;
and S6, washing and drying the sintered solid to finally obtain the modified graphite negative electrode material which is coated with the lithium ion conductor layer and is doped with zirconium ions and lithium ions.
Preferably, in S1, the zirconium source is ZrOCl2.8(H2O), preferably ZrOCl in solution A2.8(H2O) concentration was 0.2 mol/L.
Preferably, in S2, the heating temperature is 100 ℃, the stirring speed is 300-500 rpm, and the stirring time is 24-48 h.
Preferably, in S2, the graphite powder has a mass of 4g to 16 g.
Preferably, in S4, the drying temperature is 120 ℃ and the drying time is 24 h.
Preferably, in S5, the lithium source is at least one of lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate and lithium phosphate; the inert gas is at least one of nitrogen and argon; preferably, is coated with ZrO2The mixing mass ratio of the graphite solid powder to the lithium source is 1: 0.5-1.
The invention also provides the modified graphite cathode material for the lithium ion battery, which is prepared by the preparation method.
The invention also provides a lithium ion battery which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the negative electrode adopts the modified graphite negative electrode material for the lithium ion battery as a negative electrode active substance.
Has the advantages that: forming a layer of ZrO on the surface of graphite by hydrolysis2The operation is simple, and then the graphite is mixed with a lithium source and calcined at high temperature to form Li on the surface of the graphite2ZrO3Lithium ion conductor layer while Zr4+And Li+Doped into the graphite layer. Li as above2ZrO3The lithium ion conductor layer improves the wettability of the graphite surface to the electrolyte on one hand and improves the transmission efficiency of lithium ions on the other hand; in addition, zirconium ions are doped into the graphite laminated structure, so that the graphite layer spacing is increased, and the lithium ion transmission speed is favorably improved, so that the rate performance is improved; doping of lithium ions into graphite to form Li6C, additionally adding a lithium source to improveFirst-order and cycle life of the battery. The method is simple to operate, can be used for preparing a large amount of lithium ion batteries, and has a remarkable effect of improving the performance of the lithium ion batteries in all aspects.
Drawings
FIG. 1 is a photograph showing contact angles between graphite (a) before modification and graphite (b) after modification, which were prepared in example 1.
FIG. 2 is a graph showing the normal temperature cycle performance of examples 1, 2, 3 and 4.
Detailed Description
The present invention will be further illustrated with reference to the following specific embodiments, however, the scope of the present invention is not limited to the following examples.
Example 1
The invention provides a preparation method of a modified graphite cathode material for a lithium ion battery, which comprises the following steps:
s1: 0.02mol of ZrOCl28(H2O) in 100mL of deionized water to give solution A;
s2: dispersing 16g of graphite powder in the solution A, then heating at 100 ℃ and continuously stirring at a stirring speed of 400rpm for 24 h;
s3: the solid powder in solution a was collected by filtration and washed with hot deionized water until the pH was neutral;
s4: drying the washed solid powder at 120 deg.C for 24h to obtain the final product with ZrO coated surface2The graphite solid powder of (4);
s5: coating the surface with ZrO2Uniformly mixing the graphite solid powder with lithium carbonate according to the proportion of 1:1, and sintering for 10 hours at 700 ℃ in an argon atmosphere;
s6: and (3) after cooling, washing with water to remove redundant lithium carbonate, and drying to obtain the modified graphite cathode material which is coated with the lithium ion conductor layer and doped with zirconium ions and lithium ions.
The modified graphite negative electrode material prepared in the example 1 is mixed with conductive carbon black and sodium carboxymethylcellulose according to the mass ratio of 8:1:1, then a proper amount of N-methyl pyrrolidone is added, the mixture is uniformly mixed, coated on a copper foil, and dried in a vacuum oven at 80 ℃. Rolling and cutting to obtain electrode plate, using Li plate as counter electrode and electrolyteTo contain 1M LiPF6And (EC + DMC) (volume ratio of 1:1) mixed system, wherein the diaphragm is a microporous polyethylene film, and the button cell is assembled and formed in a glove box filled with argon gas, and then the performance of the button cell is tested.
Example 2
The invention provides a preparation method of a modified graphite cathode material for a lithium ion battery, which comprises the following steps:
s1: 0.02mol of ZrOCl28(H2O) in 100mL of deionized water to give solution A;
s2: dispersing 12g of graphite powder in the solution A, then heating at 100 ℃ and continuously stirring at a stirring speed of 400rpm for 24 h;
s3: the solid powder in solution a was collected by filtration and washed with hot deionized water until the pH was neutral;
s4: drying the washed solid powder at 120 deg.C for 24h to obtain the final product with ZrO coated surface2The graphite solid powder of (4);
s5: coating the surface with ZrO2Uniformly mixing the graphite solid powder with lithium hydroxide according to the proportion of 1:1, and sintering for 10 hours at 700 ℃ in an argon atmosphere;
s6: and (3) cooling, washing with water to remove redundant lithium hydroxide, and drying to obtain the modified graphite cathode material which is coated with the lithium ion conductor layer and is doped with zirconium ions and lithium ions.
The modified graphite negative electrode material prepared in the example 2 is mixed with conductive carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, then a proper amount of N-methyl pyrrolidone is added, the mixture is uniformly mixed, coated on a copper foil, and dried in a vacuum oven at 80 ℃. Rolling and cutting to obtain electrode plate, using Li plate as counter electrode, and using electrolyte containing 1M LiPF6/And (EC + DMC) (volume ratio of 1:1) mixed system, wherein the diaphragm is a microporous polyethylene film, assembling and forming the button cell in an argon-filled glove box, and then testing the performance of the button cell.
Example 3
The invention provides a preparation method of a modified graphite cathode material for a lithium ion battery, which comprises the following steps:
s1: 0.02mol of ZrOCl28(H2O) in 100mL of deionized water to give solution A;
s2: dispersing 8g of graphite powder in the solution A, then heating at 100 ℃ and continuously stirring at a stirring speed of 400rpm for 24 h;
s3: the solid powder in solution a was collected by filtration and washed with hot deionized water until the pH was neutral;
s4: drying the washed solid powder at 120 deg.C for 24h to obtain the final product with ZrO coated surface2The graphite solid powder of (4);
s5: coating the surface with ZrO2Uniformly mixing the graphite solid powder with lithium hydroxide according to the proportion of 1:1, and sintering for 10 hours at 700 ℃ in an argon atmosphere;
s6: and (3) cooling, washing with water to remove redundant lithium hydroxide, and drying to obtain the modified graphite cathode material which is coated with the lithium ion conductor layer and is doped with zirconium ions and lithium ions.
The modified graphite negative electrode material prepared in example 3 was mixed with conductive graphite and polyvinylidene fluoride in a mass ratio of 8:1:1, and then an appropriate amount of N-methylpyrrolidone was added, mixed uniformly, coated on a copper foil, and dried in a vacuum oven at 80 ℃. Rolling and cutting to obtain electrode plate, using Li plate as counter electrode, and using electrolyte containing 1M LiPF6And (EC + DMC) (volume ratio of 1:1) mixed system, wherein the diaphragm is a microporous polypropylene film, assembling and forming the button cell in an argon-filled glove box, and then testing the performance of the button cell.
Example 4
The invention provides a preparation method of a modified graphite cathode material for a lithium ion battery, which comprises the following steps:
s1: 0.02mol of ZrOCl28(H2O) in 100mL of deionized water to give solution A;
s2: dispersing 4g of graphite powder in the solution A, then heating at 100 ℃ and continuously stirring at a stirring speed of 400rpm for 24 h;
s3: the solid powder in solution a was collected by filtration and washed with hot deionized water until the pH was neutral;
s4: drying the washed solid powder at 120 deg.C for 24h to obtain the final product with ZrO coated surface2The graphite solid powder of (4);
s5: coating the surface with ZrO2Uniformly mixing the graphite solid powder with lithium hydroxide according to the proportion of 1:1, and sintering for 10 hours at 700 ℃ in an argon atmosphere;
s6: and (3) cooling, washing with water to remove redundant lithium hydroxide, and drying to obtain the modified graphite cathode material which is coated with the lithium ion conductor layer and is doped with zirconium ions and lithium ions.
The modified graphite negative electrode material prepared in example 4 was mixed with carbon nanotubes and polyvinylidene fluoride in a mass ratio of 8:1:1, and then an appropriate amount of N-methylpyrrolidone was added, mixed uniformly, coated on a copper foil, and dried in a vacuum oven at 80 ℃. Rolling and cutting to obtain electrode plate, using Li plate as counter electrode, and using electrolyte containing 1M LiPF6And (EC + DMC) (volume ratio of 1:1) mixed system, wherein the diaphragm is a microporous polypropylene film, assembling and forming the button cell in an argon-filled glove box, and then testing the performance of the button cell.
Test examples
The modified graphite cathode material prepared by the method of the invention in the embodiment 1-4 and the common unmodified graphite cathode material are respectively assembled to form a button cell, and the performance of the button cell is tested. The specific experimental settings are as follows: the electrical property test data of the button cell assembled by the modified graphite cathode material prepared by the method of the embodiment 1-4 of the invention is recorded as an experimental group 1-4; the electrical performance test data of button cells assembled by common unmodified graphite cathode materials are recorded as a reference group, and the test results are shown in the following table:
item First effect of battery (%) Capacity after 1000 cyclesRetention (%)
Experimental group 1 95.4 91.6
Experimental group 2 96.8 92.2
Experimental group 3 97.5 92.8
Experimental group 4 98.2 94.1
Reference group 91.3 88.6
The data in the table show that the electrical performance data of the button cell batteries of the experimental groups 1 to 4 are superior to those of the reference group, which shows that the modified graphite cathode material prepared by the invention can obviously improve various electrical properties of the lithium ion battery, and the ratio of the zirconium source to the graphite is gradually increased along with the gradual reduction of the graphite dosage, so that the coating effect is better and better, and the electrical performance of the button cell batteries is also gradually improved.

Claims (8)

1. A preparation method of a modified graphite negative electrode material for a lithium ion battery is characterized by comprising the following steps:
s1, dissolving a certain amount of zirconium source and polyvinyl alcohol in deionized water to obtain a solution A;
s2, dispersing a certain amount of graphite in the solution A, heating at a certain temperature and continuously stirring for a period of time;
s3, filtering and collecting solid powder in the solution A, and washing with hot deionized water until the pH value is neutral;
s4, drying the washed solid powder at a certain temperature for a period of time to obtain the solid powder with the surface coated with ZrO2The graphite solid powder of (4);
s5 coating the surface with ZrO2Uniformly mixing the graphite solid powder with a lithium source according to a certain proportion, and sintering for 10 hours at 700 ℃ in an inert gas atmosphere;
and S6, washing and drying the sintered solid to finally obtain the modified graphite negative electrode material which is coated with the lithium ion conductor layer and is doped with zirconium ions and lithium ions.
2. The method for preparing the modified graphite anode material for the lithium ion battery as claimed in claim 1, wherein in S1, the zirconium source is ZrOCl2.8(H2O), ZrOCl in the liquid A2.8(H2O) concentration was 0.2 mol/L.
3. The preparation method of the modified graphite anode material for the lithium ion battery according to claim 1, wherein in S2, the heating temperature is 100 ℃, the stirring speed is 300-500 rpm, and the stirring time is 24-48 h.
4. The method for preparing a modified graphite anode material for a lithium ion battery according to claim 1, wherein the mass of the graphite powder in S2 is 4g to 16 g.
5. The method for preparing the modified graphite anode material for the lithium ion battery according to claim 1, wherein in S4, the drying temperature is 120 ℃ and the drying time is 24 h.
6. The method for preparing the modified graphite anode material for the lithium ion battery according to claim 1, wherein in S5, the lithium source is at least one of lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate and lithium phosphate; inert gasIs one or more of nitrogen and argon; cladding with ZrO2The mixing mass ratio of the graphite solid powder to the lithium source is 1: 0.5-1.
7. The modified graphite anode material for the lithium ion battery, which is obtained by the preparation method of any one of claims 1 to 6.
8. The utility model provides a lithium ion battery, includes positive pole, negative pole, diaphragm and electrolyte, its characterized in that: the negative electrode uses the modified graphite negative electrode material for lithium ion batteries according to claim 7 as a negative electrode active material.
CN202111275162.2A 2021-10-29 2021-10-29 Modified graphite negative electrode material for lithium ion battery Pending CN114142033A (en)

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CN114613963A (en) * 2022-03-21 2022-06-10 惠州锂威新能源科技有限公司 Negative electrode material, preparation method thereof, negative electrode plate and secondary battery
CN114613963B (en) * 2022-03-21 2023-07-04 惠州锂威新能源科技有限公司 Negative electrode material, preparation method thereof, negative electrode sheet and secondary battery

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Application publication date: 20220304