CN111244398A - Composite graphite negative electrode material, lithium ion battery, preparation method and application - Google Patents
Composite graphite negative electrode material, lithium ion battery, preparation method and application Download PDFInfo
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- CN111244398A CN111244398A CN201811434778.8A CN201811434778A CN111244398A CN 111244398 A CN111244398 A CN 111244398A CN 201811434778 A CN201811434778 A CN 201811434778A CN 111244398 A CN111244398 A CN 111244398A
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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
- H01M4/366—Composites as layered products
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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 composite graphite negative electrode material, a lithium ion battery, a preparation method and application. The preparation method comprises the following steps: and (3) carrying out heat treatment on the mixture of the microcrystalline graphite, the mesocarbon microbeads and the asphalt at 300-700 ℃, cooling and then carrying out graphitization high-temperature treatment. The specific surface area of the composite graphite cathode material prepared by the preparation method is greatly reduced (less than 2.0 m)2(iv)/g); lithium ion prepared by using the sameThe discharge capacity of the sub-battery is more than 364.9mAh/g (up to 368.5mAh/g), the charge-discharge efficiency is more than 95 percent (up to 95.9 percent), the large multiplying power (5C/0.2C) is more than 90 percent (up to 94.5 percent), and the performance is good.
Description
Technical Field
The invention belongs to the field of lithium electronic batteries, and particularly relates to a composite graphite negative electrode material, a lithium ion battery, a preparation method and application.
Background
Compared with the original battery, the lithium ion battery has been rapidly popularized in the aspects of mobile phones, notebook computers, electric tools and the like due to the characteristics of high energy density, long cycle life, no memory effect and the like. With the increasing requirements of various products on small-size, light-weight, multifunction and long-time driving, the improvement of the capacity of the lithium ion battery mainly depends on the development and the perfection of a negative electrode material. Therefore, it has been a focus of research and development for a long time to improve the specific capacity of a negative electrode material of a lithium ion battery, reduce the first irreversible capacity, and improve the rate characteristics.
The natural graphite used by the lithium ion secondary battery cathode material has an ideal layered structure, has very high discharge capacity (close to theoretical capacity 372mAh/g), is low in cost but has an unstable structure, so that the co-intercalation of solvent molecules is easily caused, and the interlayer falls off in the charge and discharge process, so that the battery has poor cycle performance and poor safety.
Therefore, in order to overcome the performance deficiency of natural graphite, the prior art carries out modification treatment on the natural graphite. In japanese patent JP10294111, the graphite carbon material is coated with pitch at a low temperature, and after coating, non-melting treatment and light pulverization are required, which makes uniform coating difficult. Japanese patent JP11246209 discloses a method of impregnating graphite and hard carbon particles in pitch or tar at a temperature of 10-300 ℃, followed by solvent separation and heat treatment, which is difficult to form a highly polymerized pitch layer having a certain thickness on the surface of the graphite and hard carbon, and is limited in improvement of structural stability of natural graphite. JP2000003708 rounds graphite material mechanically, then impregnates it in heavy oil, tar or pitch, separates and washes it, just like JP11246209 in terms of coating method. Japanese patent JP2000182617 uses natural graphite and the like to carbonize together with asphalt or resin or a mixture thereof, and the method can reduce the specific surface area of the graphite material, but cannot achieve better control on the coating effect. JP2000243398 discloses a method for surface treatment of graphite material by utilizing the atmosphere generated by pyrolysis of pitch, which is unlikely to improve the morphology of the modified material, and thus the improvement of the electrical properties is limited. JP2002042816 uses aromatic hydrocarbon as raw material and uses CVD method to coat or uses pitch phenolic resin to coat, which is similar to JP2000182617 and JP2000283398 in effect.
In the prior art, patent application (CN104140093A) describes that natural graphite, needle coke green coke powder and asphalt are used to prepare a negative electrode material, however, the first efficiency of a lithium ion secondary battery prepared by using the negative electrode material is only 91.8% at most, which is difficult to further improve, and even if the efficiency is improved by 1%, the technical difficulty is very high; and the natural graphite has the defects of large expansion, poor circulation and the like.
Disclosure of Invention
The invention aims to solve the technical problems that the composite graphite cathode material in the prior art is low in first-time discharge efficiency, and the raw materials used for preparing the composite graphite cathode material are large in expansion, poor in circulation and the like when used for preparing a battery, and provides the composite graphite cathode material, the lithium ion battery, the preparation method and the application. The lithium ion battery has high first discharge efficiency and discharge capacity.
The invention solves the technical problems through the following technical scheme.
Because the microcrystalline graphite used as the lithium ion battery cathode material has the defects of low first charge-discharge efficiency, poor high-current charge-discharge performance and the like, the microcrystalline graphite is rarely applied to the preparation of the lithium ion battery cathode material in the actual operation process; the application of the material is described in that the surface of microcrystalline graphite is modified by ultrasonic waves, and the surface of graphite is coated by carbon nanotubes/urea resin carbon to improve the conductivity and discharge capacity of the negative electrode material (CN 107959028A). It is difficult to prepare the negative electrode material by directly using the microcrystalline graphite, and the microcrystalline graphite has many requirements for a raw material to be mixed with the microcrystalline graphite to prepare the negative electrode material. After creative labor is paid, the mesocarbon microbeads, the asphalt and the microcrystalline graphite are selected for combination for the first time, extra treatment on the microcrystalline graphite is not needed, the optimal ratio of the mesocarbon microbeads, the asphalt and the microcrystalline graphite is obtained through exploration, and the composite graphite cathode material with good performance is obtained after treatment.
One of the technical schemes provided by the invention is as follows: a preparation method of a composite graphite negative electrode material comprises the following steps: carrying out heat treatment on a mixture of microcrystalline graphite, mesocarbon microbeads and asphalt at 300-700 ℃, cooling and then carrying out graphitization high-temperature treatment;
wherein the mass ratio of the microcrystalline graphite to the mesocarbon microbeads is (1-9): 1; the mass ratio of the microcrystalline graphite to the asphalt is 10 (1-5); the average grain diameter D50 of the microcrystalline graphite is 5-20 mu m, and the average grain diameter D50 of the mesocarbon microbeads is 20-30 mu m.
In the present invention, the microcrystalline graphite may be commercially available microcrystalline graphite, such as microcrystalline graphite obtained from microcrystalline graphite product factories of Chenzhou, Hunan province.
In the invention, in order to effectively improve the product compaction density and easily prepare the high-compaction-density cathode material, the mesocarbon microbeads are preferably the mesocarbon microbeads subjected to crushing pretreatment, and the crushing pretreatment is preferably carried out by adopting a crushing classifier treatment method. The particle size D50 of the powder obtained after the grinding pretreatment is preferably 20.1-28.2 μm, more preferably 21.8-25.6 μm, such as 22.7 μm or 25.0 μm; the mesocarbon microbeads are preferably mesocarbon microbeads prepared by liquid phase polymerization of pitch, such as those prepared from coal (tar) pitch or petroleum pitch.
The mesocarbon microbeads can be obtained from Shanghai fir Techni, Inc.
The coal pitch can be medium temperature pitch produced by Henan Bohai chemical Co.
The petroleum asphalt can be MQ-100 medium temperature asphalt produced by Dalian reinforcement materials Co.
In the present invention, the mass ratio of the microcrystalline graphite to the mesocarbon microbeads is preferably (7:3) to (4: 1).
In the invention, the mass ratio of the microcrystalline graphite to the asphalt is preferably 10 (2-4), for example 10: 3.
The average particle size D50 of the microcrystalline graphite in the invention is preferably 10.4-18.1 μm, and more preferably 12.5-16.3 μm.
In the present invention, it is preferable that the microcrystalline graphite, the mesocarbon microbeads and the pitch are mixed by a mixer to obtain the mixture. The mixing time is preferably 1 to 5 hours, more preferably 2 to 4 hours, for example 2.5 or 3 hours.
In the present invention, the temperature of the heat treatment is preferably 400 to 600 ℃, for example, 500 ℃.
In the present invention, the heat treatment time is preferably 12 to 24 hours, for example, 16 hours.
The atmosphere of the heat treatment is an inert atmosphere, as is common in the art. The inert atmosphere refers to an atmosphere which does not participate in the reaction in the heat treatment, and is generally an inert atmosphere such as nitrogen or argon.
In the invention, the cooled temperature is preferably room temperature, and the room temperature is 5-40 ℃.
In the present invention, the method and conditions for the graphitization high temperature treatment may be those conventional in the art. The temperature of the graphitization high-temperature treatment is preferably 2500-2800 ℃, such as 2600 ℃ or 2700 ℃. The time for the graphitization high-temperature treatment is preferably 20-60 hours, and more preferably 48 hours. The atmosphere of the graphitization high temperature treatment is an inert atmosphere, as is common in the art.
The second technical scheme of the invention is as follows: the composite graphite cathode material prepared by the preparation method.
Preferably, the average particle size D50 of the composite graphite negative electrode material is 10-25 μm.
Preferably, the specific surface area of the composite graphite negative electrode material is 2.0m2The ratio of the carbon atoms to the carbon atoms is less than g.
More preferably, the composite graphite negative electrode materialThe average particle size D50 of the composite graphite anode material is 10-25 mu m, and the specific surface area of the composite graphite anode material is 2.0m2The ratio of the carbon atoms to the carbon atoms is less than g.
The performance parameters and the detection method thereof are shown in the following table 1.
TABLE 1
| Serial number | Item | Index (I) | Analytical method |
| 1 | Average particle diameter D50, μm | 10～25 | Laser method |
| 2 | Specific surface area, m2/g | ≤2.0 | Nitrogen adsorption process |
The average particle size D50 of the composite graphite negative electrode material is preferably 10.7-24.6 μm, such as 15.3, 15.8, 16.2, 16.3 or 20.1 μm.
The specific surface area of the composite graphite negative electrode material is preferably 1.5-1.8 μm, such as 1.6 or 1.7 μm.
Therefore, the specific surface area of the composite graphite cathode material prepared by the preparation method is effectively reduced.
The third technical scheme of the invention is as follows: the composite graphite cathode material is applied to lithium ion batteries.
The fourth technical scheme of the invention is as follows: a lithium ion battery containing the composite graphite negative electrode material.
Wherein the discharge capacity of the lithium ion battery is more than or equal to 360mAh/g (measured by a multichannel battery test Bt2000 type), such as 364.9, 363.7, 360.2, 360.5, 362.2, 360.8 or 361.2 mAh/g.
Wherein the first discharge efficiency of the lithium ion battery is more than or equal to 95 (measured by a multichannel battery test Bt2000 type), such as 95.1%, 95.6%, 95.2%, 95.9%, 95.7%, 95.4% or 95.3%.
Wherein the discharge rate (5C/0.2C) of the lithium ion battery is greater than 90%, such as 93.8%, 94.5%, 93.5%, 91.4%, 95.1%, 94.2%, or 94.1%.
Therefore, the composite graphite cathode material effectively reduces the specific surface area, improves the gram capacity and the discharge efficiency, has good large-current charge and discharge performance, and can be used for preparing a lithium ion battery with excellent comprehensive performance.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
the specific surface area of the composite graphite cathode material prepared by the preparation method is greatly reduced (less than 2.0 m)2(iv)/g); the discharge capacity of the lithium ion battery prepared by the lithium ion battery is more than 364.9mAh/g (up to 368.5mAh/g), the charge-discharge efficiency is more than 95 percent (up to 95.9 percent), the high multiplying power (5C/0.2C) is more than 90 percent (up to 94.5 percent), and the high-current charge-discharge performance is good.
Drawings
Fig. 1 is a first charge-discharge curve of the composite graphite negative electrode material of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples:
the microcrystalline graphite is purchased from microcrystalline graphite product factories in Chenzhou city, Hunan province;
the petroleum asphalt is MQ-100 medium temperature asphalt produced by Dalian reinforcement industrial materials GmbH;
the coal pitch is medium temperature pitch produced by Henan Bohai chemical Co., Ltd;
mesocarbon microbeads were purchased from shanghai fir tech ltd.
The button cell testing method used by the invention comprises the following steps: adding conductive carbon black into a carboxymethyl cellulose (CMC) aqueous solution, then adding a graphite sample, finally adding Styrene Butadiene Rubber (SBR), uniformly stirring, and uniformly coating the slurry on a copper foil on a coating machine to prepare a pole piece. And (3) putting the coated pole piece into a vacuum drying oven at the temperature of 110 ℃ for vacuum drying for 4 hours, taking out the pole piece, and rolling the pole piece on a roller press for later use. The simulated cell was assembled in an argon-filled German Braun glove box with an electrolyte of 1MLiPF6+ EC: DEC: DMC 1: 1 (volume ratio) and a metallic lithium plate as counter electrode. The capacity test was carried out on an ArbinBT2000 model U.S. Battery tester, with a charge-discharge voltage range of 0.005 to 2.0V and a charge-discharge rate of 0.1C.
The discharge multiplying power test method used by the invention comprises the following steps: the graphite of the embodiment or the comparative example of the invention is used as a negative electrode, lithium cobaltate is used as a positive electrode, 1M-LiPF6EC, DMC, EMC (volume ratio) is 1: 1 is used as electrolyte to assemble a full cell, and the discharge rate (5C/0.2C) is tested to be more than 90%.
The process parameters for each example and comparative example are shown in table 2 below:
TABLE 2
The following is specifically illustrated by example 2:
example 2
The intermediate phase carbon microsphere green ball is crushed and graded in a crushing and grading machine to obtain an F1 material (D50 is 25.6 mu m), 80kg of microcrystalline graphite (D50 is 10.4 mu m), 20kg of F1 material and 30kg of coal tar pitch are alternately added into a mixer to be mixed for 2 hours, heat treatment is carried out under the protection of nitrogen, after the final temperature is 500 ℃, a reaction product is cooled to the room temperature and then graphitized at high temperature (2500 ℃ for 48 hours) to obtain the composite graphite cathode material, the half cell capacity is 363.7mAh/g, the first efficiency is 95.6%, and the discharge rate (5C/0.2C) is 94.5%.
The performance parameters of each example and comparative example are shown in table 3 below:
TABLE 3
As can be seen from the above data, the discharge capacity, the charge-discharge efficiency and the first efficiency in the comparative example were low, in which the charge-discharge efficiency of the non-pitch-coated graphite was the lowest, 88.5%, and the discharge rate (5C/0.2C) reached only 75.2%; in comparative examples 2 to 11, when the particle size of the microcrystalline graphite, the mass ratio of the microcrystalline graphite to the pitch, the mass ratio of the microcrystalline graphite to the mesocarbon microbeads and the heat treatment temperature of the mixture are out of the ranges of the present invention, the discharge capacity, the first efficiency, the discharge rate, the specific surface area, etc. of the prepared composite graphite negative electrode material do not reach the standards.
Claims (10)
1. The preparation method of the composite graphite negative electrode material is characterized by comprising the following steps of: carrying out heat treatment on a mixture of microcrystalline graphite, mesocarbon microbeads and asphalt at 300-700 ℃, cooling and then carrying out graphitization high-temperature treatment;
wherein the mass ratio of the microcrystalline graphite to the mesocarbon microbeads is (1-9): 1; the mass ratio of the microcrystalline graphite to the asphalt is 10 (1-5); the average grain diameter D50 of the microcrystalline graphite is 5-20 mu m, and the average grain diameter D50 of the mesocarbon microbeads is 20-30 mu m.
2. The preparation method according to claim 1, wherein the mesocarbon microbeads are the mesocarbon microbeads obtained by the pulverization pretreatment, and the mesocarbon microbeads have an average particle size D50 of preferably 20.1 to 28.2 μm, more preferably 21.8 to 25.6 μm, such as 22.7 μm or 25.0 μm;
and/or the mesocarbon microbeads are prepared by liquid phase polymerization of asphalt, wherein the asphalt is preferably coal tar pitch or petroleum asphalt.
3. The method according to claim 1, wherein the asphalt is petroleum asphalt or coal asphalt.
4. The preparation method according to claim 1, wherein the mass ratio of the microcrystalline graphite to the pitch is 10 (2-4), such as 10: 3;
and/or the mass ratio of the microcrystalline graphite to the mesocarbon microbeads is (7:3) - (4: 1);
and/or the average grain diameter D50 of the microcrystalline graphite is 10.4-18.1 μm, and more preferably 12.5-16.3 μm.
5. The preparation method of the composite graphite anode material as claimed in claim 1, wherein the temperature of the heat treatment is 400-600 ℃, such as 500 ℃;
and/or the time of the heat treatment is 12-24 hours, such as 16 hours;
and/or the temperature after cooling is room temperature.
6. The method of claim 1, wherein the mixture is obtained by mixing the microcrystalline graphite with the mesocarbon microbeads and the pitch using a mixer, preferably for 1 to 5 hours, more preferably for 2 to 4 hours, such as for 2.5 or 3 hours.
7. The method according to any one of claims 1 to 6, wherein the temperature of the graphitization high temperature treatment is 2500 to 2800 ℃, such as 2600 ℃ or 2700 ℃;
and/or the time of the graphitization high-temperature treatment is 20-60 hours, preferably 48 hours.
8. The composite graphite anode material prepared by the preparation method of any one of claims 1 to 7.
9. Use of the composite graphite anode material of claim 8 in a lithium ion battery.
10. A lithium ion battery comprising the composite graphite anode material of claim 8.
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