CN109524631B - Preparation method of high-capacity composite negative electrode material - Google Patents
Preparation method of high-capacity composite negative electrode material Download PDFInfo
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- CN109524631B CN109524631B CN201710853169.5A CN201710853169A CN109524631B CN 109524631 B CN109524631 B CN 109524631B CN 201710853169 A CN201710853169 A CN 201710853169A CN 109524631 B CN109524631 B CN 109524631B
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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
- H01M4/362—Composites
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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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- 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
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a high-capacity composite negative electrode material, which comprises the steps of calcining sucrose and water-soluble phenolic resin for 5-10 hours at the temperature of 550-850 ℃ in a protective atmosphere, and cooling to obtain amorphous carbon; placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 8-120: 0.1-50, and mixing for 1-8h to obtain a mixture A; calcining the mixture A in a protective atmosphere at the temperature of 2200-; filling the mixture B pressed powder into a mold, carrying out high-frequency electromagnetic vibration to compact the mixture B, sealing the mold, vacuumizing the mold, then putting the mold into a high-pressure container filled with water or oil, pressurizing the container to 80-250MPa, heating the container to 120 ℃ and 250 ℃, maintaining the pressure and the temperature for 8-30h, cooling the container to obtain a mixture C, and then putting the mixture C into a crusher for crushing and spheroidizing to obtain spherical powder D50 which is 10-80 mu m. The composite negative electrode material prepared by the invention has high tap density, can reduce side reaction, is beneficial to improving the battery capacity and improving the low-temperature charging performance of the battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a high-capacity composite negative electrode material.
Background
The carbon material has the advantages of low chemical potential, good cycle performance, low price, environmental protection and the like, and is the most ideal and commonly used lithium ion battery cathode material at present. In the carbon material, compared with soft carbon and hard carbon, the graphite material has obvious advantages in the aspects of specific capacity, discharge platform, cost and the like. The natural graphite has the advantages of high specific capacity, low price and the like, but has large first irreversible capacity, poor cycle performance and poor rate performance. In order to overcome the defects of natural graphite, the electrochemical performance of the carbon negative electrode material is improved, and the production and manufacturing cost is reduced. The carbon/graphite material has high theoretical specific energy, low cost, easy obtaining and mature preparation process, thereby being widely used as the cathode material of the lithium ion battery. However, carbon/graphite anodes have problems: the first charge forms a Solid Electrolyte Interface (SEI) on the surface of carbon particles, which causes the capacity loss of the battery, and the SEI generation amount increases with the increase of the number of charge and discharge cycles, and simultaneously, the internal resistance of the battery increases, and the specific energy and power performance decrease.
Disclosure of Invention
The invention aims to provide a preparation method of a high-capacity composite negative electrode material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-capacity composite anode material comprises the following steps:
1) calcining sucrose and water-soluble phenolic resin in protective atmosphere at the temperature of 550-850 ℃ for 5-10h, and cooling to obtain amorphous carbon;
2) lithium titanate, natural graphite and amorphous carbon are mixed according to the mass ratio of 1: 8-120: 0.1-50, placing the mixture into a high-speed stirrer, and mixing for 1-8h at the rotation speed of 400-;
3) calcining the mixture A in a protective atmosphere at the temperature of 2200-;
4) filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 80-250MPa, heating to 120-250 ℃, maintaining the pressure and the temperature for 8-30h, and cooling to room temperature to obtain a mixture C;
5) and (3) putting the mixture C into a pulverizer for pulverizing and spheroidizing, wherein the rotating speed of the pulverizer is 1500-.
As a further scheme of the invention: in the step 1), the protective atmosphere is at least one selected from helium, nitrogen, argon and carbon dioxide.
As a further scheme of the invention: in the step 1), calcining is carried out for 5-9h at the temperature of 600-800 ℃.
As a further scheme of the invention: in the step 2), the purity of the lithium titanate is more than 99.0 percent, and the particle size is 1000 nm.
As a further scheme of the invention: in the step 2), the mass ratio of lithium titanate, natural graphite and amorphous carbon is 1: 10-100: 0.1-20.
As a further scheme of the invention: in the step 2), the rotation speed of the high-speed stirrer is 500-.
As a further scheme of the invention: in the step 3), the protective atmosphere is selected from one of helium, nitrogen and argon.
As a further scheme of the invention: in step 3), calcining at the temperature of 2500 ℃ and 2800 ℃ for 4-6 h.
As a further scheme of the invention: in the step 4), pressurizing to 100-.
As a further scheme of the invention: in step 5), the rotation speed of the pulverizer is 1800-.
Compared with the prior art, the invention has the beneficial effects that:
the composite negative electrode material prepared by the steps has high tap density, can reduce side reaction, is beneficial to improving the battery capacity, avoids the anisotropy of a graphite structure and improves the low-temperature charging performance of the battery.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In the embodiment of the invention, the preparation method of the high-capacity composite negative electrode material comprises the following steps:
1) and (3) calcining the sucrose and the water-soluble phenolic resin for 5 hours at the temperature of 550 ℃ in a helium atmosphere, and cooling to obtain the amorphous carbon.
2) Placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 8: 0.1, and mixing for 1h at the rotating speed of 400r/min to obtain a mixture A; the purity of the lithium titanate is more than 99.0 percent, and the particle size is 100-1000 nm.
3) Calcining the mixture A in a helium atmosphere at the temperature of 2200 ℃ for 3h, and cooling to obtain a mixture B.
4) Filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 80MPa, heating to 120 ℃, maintaining the pressure and the temperature for 8 hours, and cooling to room temperature to obtain a mixture C.
5) And (3) putting the mixture C into a grinder for grinding and spheroidizing, wherein the rotation speed of the grinder is 1500r/min, and obtaining spherical powder with the D50 being 10-80 mu m.
Example 2
In the embodiment of the invention, the preparation method of the high-capacity composite negative electrode material comprises the following steps:
1) and (3) calcining the sucrose and the water-soluble phenolic resin for 10 hours at the temperature of 850 ℃ in a nitrogen atmosphere, and cooling to obtain the amorphous carbon.
2) Placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 120: 50, and mixing for 8 hours at the rotating speed of 5500r/min to obtain a mixture A; the purity of the lithium titanate is more than 99.0 percent, and the particle size is 100-1000 nm.
3) Calcining the mixture A at the temperature of 2900 ℃ for 10h in a nitrogen atmosphere, and cooling to obtain a mixture B.
4) Filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 250MPa, heating to 250 ℃, maintaining the pressure and the temperature for 30h, and cooling to room temperature to obtain a mixture C.
5) And (3) putting the mixture C into a grinder for grinding and spheroidizing, wherein the rotation speed of the grinder is 2500r/min, and obtaining spherical powder with the D50 being 10-80 mu m.
Example 3
In the embodiment of the invention, the preparation method of the high-capacity composite negative electrode material comprises the following steps:
1) and (3) calcining the sucrose and the water-soluble phenolic resin for 5 hours at the temperature of 600 ℃ in an argon atmosphere, and cooling to obtain the amorphous carbon.
2) Placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 10: 0.1, and mixing for 2 hours at the rotating speed of 500r/min to obtain a mixture A; the purity of the lithium titanate is more than 99.0 percent, and the particle size is 100-1000 nm.
3) Calcining the mixture A for 4-6h at 2500 ℃ in an argon atmosphere, and cooling to obtain a mixture B.
4) Filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 100MPa, heating to 150 ℃, maintaining the pressure and the temperature for 10 hours, and cooling to room temperature to obtain a mixture C.
5) And (3) putting the mixture C into a grinder for grinding and spheroidizing, wherein the rotation speed of the grinder is 1800r/min, and obtaining spherical powder with D50 being 10-80 mu m.
Example 4
In the embodiment of the invention, the preparation method of the high-capacity composite negative electrode material comprises the following steps:
1) and (3) calcining the sucrose and the water-soluble phenolic resin for 9 hours at the temperature of 800 ℃ in the atmosphere of carbon dioxide, and cooling to obtain the amorphous carbon.
2) Placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 100: 20, and mixing for 6 hours at the rotating speed of 5200r/min to obtain a mixture A; the purity of the lithium titanate is more than 99.0 percent, and the particle size is 100-1000 nm.
3) The mixture A was calcined at 2800 ℃ for 6h under nitrogen atmosphere and cooled to give mixture B.
4) Filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 200MPa, heating to 200 ℃, maintaining the pressure and the temperature for 20 hours, and cooling to room temperature to obtain a mixture C.
5) And (3) putting the mixture C into a grinder for grinding and spheroidizing, wherein the rotation speed of the grinder is 2200r/min, and obtaining spherical powder with D50 being 10-80 mu m.
Example 5
In the embodiment of the invention, the preparation method of the high-capacity composite negative electrode material comprises the following steps:
1) and (3) calcining the sucrose and the water-soluble phenolic resin for 7 hours at the temperature of 700 ℃ in a nitrogen atmosphere, and cooling to obtain the amorphous carbon.
2) Placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 50: 10, and mixing for 5 hours at the rotating speed of 3000r/min to obtain a mixture A; the purity of the lithium titanate is more than 99.0 percent, and the particle size is 100-1000 nm.
3) Calcining the mixture A at 2600 ℃ for 5h in a nitrogen atmosphere, and cooling to obtain a mixture B.
4) Filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 150MPa, heating to 180 ℃, maintaining the pressure and the temperature for 15h, and cooling to room temperature to obtain a mixture C.
5) And (3) putting the mixture C into a grinder for grinding and spheroidizing, wherein the rotation speed of the grinder is 2000r/min, and obtaining spherical powder with the D50 being 10-80 mu m.
The high-capacity composite negative electrode material prepared in example 5 was used as a negative electrode material, and a conventional graphite negative electrode material was used as a reference; according to a conventional manufacturing method of the lithium ion battery, the positive electrode and the negative electrode adopt a winding structure to manufacture the 32650 type lithium ion battery with the rated voltage of 5.0Ah, and relevant parameters are shown in a table 1:
TABLE 1
| Internal resistance/omega | capacity/mAh | Mass/g | Gram play/mAh | Energy density/Wh/Kg | |
| Example 5 | 6.2 | 5569 | 139.2 | 345 | 129 |
| Reference to | 7.4 | 5305 | 142.8 | 325 | 119.5 |
From the above table, it can be seen that: the high-capacity composite negative electrode material prepared in example 5 has high tap density, and is beneficial to first effect and gram capacity exertion of the positive electrode material, the prepared lithium ion battery has large capacity, the whole battery has light weight and large energy density, and the internal resistance of the prepared lithium ion battery is small.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. A preparation method of a high-capacity composite anode material is characterized by comprising the following steps:
1) calcining sucrose and water-soluble phenolic resin in protective atmosphere at the temperature of 600-800 ℃ for 5-9h, and cooling to obtain amorphous carbon;
2) placing lithium titanate, natural graphite and amorphous carbon into a high-speed stirrer according to the mass ratio of 1: 8-120: 0.1-50, and mixing for 1-8h at the rotation speed of 400-5500r/min to obtain a mixture A;
3) calcining the mixture A in a protective atmosphere at the temperature of 2200-;
4) filling the obtained mixture B pressed powder into a mold, compacting the mixture B by high-frequency electromagnetic vibration in the filling process, vacuumizing the mold after sealing, then putting the mold into a high-pressure container filled with water or oil, pressurizing to 80-250MPa, heating to 120-250 ℃, maintaining the pressure and the temperature for 8-30h, and cooling to room temperature to obtain a mixture C;
5) and (3) putting the mixture C into a pulverizer for pulverizing and spheroidizing, wherein the rotating speed of the pulverizer is 1500-.
2. The method for preparing a high-capacity composite anode material according to claim 1, wherein in the step 1), the protective atmosphere is at least one selected from helium, nitrogen, argon and carbon dioxide.
3. The preparation method of the high-capacity composite anode material as claimed in claim 1, wherein in the step 2), the purity of the lithium titanate is greater than 99.0%, and the particle size is 100-1000 nm.
4. The preparation method of the high-capacity composite anode material according to claim 1, wherein in the step 2), the mass ratio of the lithium titanate, the natural graphite and the amorphous carbon is 1: 10-100: 0.1-20.
5. The method for preparing the high-capacity composite anode material as claimed in claim 1, wherein the rotation speed of the high-speed stirrer in the step 2) is 500-.
6. The method for preparing a high-capacity composite anode material according to claim 1, wherein in the step 3), the protective atmosphere is selected from one of helium, nitrogen and argon.
7. The method for preparing a high capacity composite anode material according to claim 1, wherein in the step 3), the calcination is performed at a temperature of 2500-2800 ℃ for 4-6 h.
8. The preparation method of the high-capacity composite anode material as claimed in claim 1, wherein in the step 4), the pressure is increased to 100-200MPa, the temperature is increased to 150-200 ℃, and the pressure and the temperature are maintained for 10-20 h.
9. The method for preparing the high-capacity composite anode material as claimed in claim 1, wherein the rotation speed of the pulverizer in the step 5) is 1800-.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001126727A (en) * | 1999-10-26 | 2001-05-11 | Toyota Motor Corp | Lithium ion secondary cell |
| CN102170018A (en) * | 2011-03-31 | 2011-08-31 | 东莞新能源科技有限公司 | Lithium-ion secondary battery |
| WO2013058566A1 (en) * | 2011-10-20 | 2013-04-25 | Sk Innovation Co.,Ltd. | Secondary battery |
| CN106876675A (en) * | 2017-03-23 | 2017-06-20 | 福建翔丰华新能源材料有限公司 | A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101155909B1 (en) * | 2010-01-07 | 2012-06-20 | 삼성에스디아이 주식회사 | Negative active material for rechargeable lithium battery, method of preparing same, and rechargeable lithium battery including same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001126727A (en) * | 1999-10-26 | 2001-05-11 | Toyota Motor Corp | Lithium ion secondary cell |
| CN102170018A (en) * | 2011-03-31 | 2011-08-31 | 东莞新能源科技有限公司 | Lithium-ion secondary battery |
| WO2013058566A1 (en) * | 2011-10-20 | 2013-04-25 | Sk Innovation Co.,Ltd. | Secondary battery |
| CN106876675A (en) * | 2017-03-23 | 2017-06-20 | 福建翔丰华新能源材料有限公司 | A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite |
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