CN112938959B - Preparation method of power battery negative electrode material - Google Patents
Preparation method of power battery negative electrode material Download PDFInfo
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- CN112938959B CN112938959B CN202110125405.8A CN202110125405A CN112938959B CN 112938959 B CN112938959 B CN 112938959B CN 202110125405 A CN202110125405 A CN 202110125405A CN 112938959 B CN112938959 B CN 112938959B
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000010426 asphalt Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 102220043159 rs587780996 Human genes 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000010406 cathode material Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000571 coke Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005087 graphitization Methods 0.000 claims description 5
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052744 lithium Inorganic materials 0.000 abstract description 14
- 229910021383 artificial graphite Inorganic materials 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000010405 anode material Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 239000011331 needle coke Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012257 stirred material Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- 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
-
- 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
-
- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 application discloses a preparation method of a power battery cathode material, which comprises the steps of firstly mixing needle Jiao Fenmo (D50=8-10 mu m) and 5% -20% of intermediate asphalt powder (D50=4-5 mu m) with a softening point of more than or equal to 350 ℃ for 30min at normal temperature. The uniformly mixed materials were put into a reaction kettle and heated to 360 ℃ and stirred at this temperature for 1 hour. Then cooling to 200 ℃, adding high-temperature asphalt with a softening point of 240 ℃ into the reaction kettle, and slowly heating to 250 ℃; and finally, graphitizing the granulated material at high temperature to obtain the negative electrode material. The application improves the cycling stability of the lithium battery, improves the quick charge performance, improves the capacity of the artificial graphite of the negative electrode material, and finally prepares the negative electrode material of the power battery with high capacity.
Description
Technical Field
The application relates to a preparation method of a power battery negative electrode material, and belongs to the technical field of preparation methods of power lithium battery negative electrode materials.
Background
In recent years, with the rapid development of electronic devices, the demands of large-scale energy storage, electric tools, portable devices, hybrid power and pure electric vehicles are rapidly increasing, and the in-depth research of convenient high-performance energy storage battery systems is more and more urgent. Currently, power lithium ion batteries are classified into two types, namely high-capacity and high-power. The high-capacity battery can be used for electric tools, bicycles, scooters, miner lamps, medical appliances and the like; the high-power battery is mainly used for hybrid electric vehicles and other occasions requiring high-current charge and discharge. Although graphite is currently the main stream as the negative electrode material, it has the disadvantages of insufficient gram capacity, poor satisfaction of the requirements of the power battery, and the stability of the layered structure is still to be improved.
Disclosure of Invention
According to the application, needle coke raw materials are coated with one high-softening-point asphalt, the coated materials are granulated by using the other high-softening-point asphalt after temperature treatment, and finally, the high-capacity power battery anode material is obtained by high-temperature graphitization. The specific technical scheme is as follows:
step 1: mixing needle coke with the D50 of 8-10 mu m and intermediate asphalt with the D50 of 4-5 mu m for 30min at normal temperature, wherein the softening point of the intermediate asphalt is more than or equal to 350 ℃ and the content of the intermediate asphalt is 5-20 wt%,
step 2: heating the uniformly mixed materials in the step 1 to 360 ℃, stirring for 30min at the temperature, cooling the heated and stirred materials to 200 ℃,
step 3: adding high-temperature asphalt with a softening point of 240 ℃ into the material after the reaction in the step 2, heating the material to 250 ℃,
step 4: granulating the material treated in the step 3, and then carrying out high-temperature graphitization to obtain a finished product.
Further, the specific operation process of the step 1 is as follows: crushing needle Jiao Shengjiao to obtain a material with the particle size less than or equal to 10mm, grinding the material to obtain raw coke with the particle size D50=8-10 mu m, grinding asphalt with the softening point at 350 ℃ to obtain powder with the particle size D50=4-5 mu m, and putting the raw coke and 5-20wt% of the intermediate asphalt powder into a VC mixer to be mixed for 30min at normal temperature under the rotating speed of 700rpm.
Further, the materials uniformly mixed in the step 1 are put into a reaction kettle, the materials are stirred at a low speed while being heated in the heating process, when the temperature of the reaction kettle reaches 360 ℃, the materials are stirred and mixed at a high speed for 1 hour, and then the temperature of the reaction kettle is reduced to 200 ℃.
Further, the low-speed stirring rotation speed was 40rpm, and the high-speed stirring rotation speed was 700rpm.
Further, in the step 3, the materials are heated to 250 ℃ and then stirred for 30min.
Further, the high temperature graphitization temperature in the step 4 is 2900-3000 ℃.
The beneficial effects are that: according to the application, 5-20wt% of intermediate asphalt powder with a softening point of 350 ℃ is used for coating the coke powder to fill the cavity on the surface of the coke powder, a lithium transmission channel is provided, peeling caused by expansion of graphite volume due to co-intercalation of solvent molecules is avoided, the cycling stability of a lithium battery is improved, and then high-temperature asphalt with a softening point of 240 ℃ is used for granulation bonding so as to improve isotropy, so that lithium ions are intercalated from multiple directions in the charge and discharge process, the quick charge performance is improved, more lithium intercalation points are provided, the expansion of a pole piece is reduced, the capacity of artificial graphite of a negative electrode material is improved, and finally the negative electrode material of the high-capacity power battery is prepared.
Drawings
FIG. 1 is a surface image of a high capacity lithium battery anode material prepared in an embodiment of the present application under a Scanning Electron Microscope (SEM) of 10um,
figure 2 is a surface image of the high capacity lithium battery anode material prepared in the example of the present application observed under a Scanning Electron Microscope (SEM) of 50um,
fig. 3 is a schematic view showing the surface particle size distribution of the high-capacity lithium battery anode material prepared in the embodiment of the application, which is observed by using a malvern laser particle sizer (MASTERSIZER 3000).
Detailed Description
The present application is further illustrated in the accompanying drawings and detailed description which are to be understood as being merely illustrative of the application and not limiting of its scope, and various modifications of the application, which are equivalent to those skilled in the art upon reading the application, will fall within the scope of the application as defined in the appended claims.
The application relates to a preparation method of a power battery anode material, which specifically comprises the following steps:
step 1: crushing needle Jiao Shengjiao to obtain a material with particle size less than or equal to 10mm, grinding to obtain raw coke with particle size D50=8-10 um, grinding asphalt with softening point of 350 ℃ to powder with particle size D50=4-5 μm, adding the raw coke and 5-20wt% of the intermediate asphalt powder into a VC mixer, mixing for 30min at normal temperature and rotating speed of 700rpm,
step 2: putting the materials uniformly mixed in the step 1 into a reaction kettle, heating and stirring at a low speed of 40rpm in the heating process, when the temperature of the reaction kettle reaches 360 ℃, stirring and mixing at a high speed of 700rpm for 1 hour, then cooling the temperature of the reaction kettle to 200 ℃,
step 3: adding high-temperature asphalt with a softening point of 240 ℃ into the material after the reaction in the step 2, heating the material to 250 ℃ and then continuously stirring for 30min,
step 4: granulating the material treated in the step 3, and then carrying out high-temperature graphitization at 2900-3000 ℃ to obtain a finished product.
Examples
The artificial graphite anode material of the power battery is prepared by the following steps:
step 1: grinding needle Jiao Shengjiao to obtain powder with particle diameter d50=8um, and grinding asphalt with softening point of 350deg.C into raw material powder with particle diameter d50=4um; charging raw coke D50=8um and 8wt% of intermediate asphalt powder (D50=4μm) with softening point of 350 ℃ into VC mixer at mass ratio of 10:0.8, mixing at normal temperature for 30min, rotating at about 700rpm,
step 2: putting the evenly mixed materials into a reaction kettle, heating and stirring slowly (rotating speed is 40 rpm) in the heating process, when the temperature of the reaction kettle reaches 360 ℃, then increasing the rotating speed to mix for 1 hour at the speed of 700rpm, then reducing the temperature of the reaction kettle to 200 ℃,
step 3: adding high-temperature asphalt with a softening point of 240 ℃ into the reaction kettle according to a ratio of 10:0.6, then raising the temperature of the reaction kettle to 250 ℃ and continuously stirring for 30min,
step 4: and (3) graphitizing the coated and granulated material at a high temperature (the temperature is 3000 ℃) to obtain the high-capacity power battery.
The lithium ion battery of the embodiment is prepared by mixing the artificial graphite anode material of the embodiment and the conductive agent SP, CMC, SBR (content 45%) according to a mass ratio of 92:3:2:3, preparing into slurry, coating the slurry on copper foil, and drying the slurry in a vacuum drying oven for 12 hours to prepare the anode sheet; and cutting the dried film on a manual sheet punching device into a round electrode sheet with the diameter of 14mm, and finally assembling the battery in a glove box filled with argon. The counter electrode adopted in the embodiment is a metal lithium sheet, the diaphragm is a Celgard 2300 polypropylene film, the electrolyte system is a national standard electrolyte EC: DEC: DMC=1:1:1 LiPF6 1mol/L of Hua Rong LB303, and the button cell of CR2016 type is assembled.
This example characterizes the test: observing the appearance form of the anode material by adopting a Japan electron (Jieulu) Jeol Scanning Electron Microscope (SEM); observing the particle size of the anode material by using a Markov laser particle sizer (MASTERSIZER 3000); the charging and discharging cycle and the capacity test are carried out by adopting a Wuhan blue electric test system CT 2001A.
The high-capacity lithium battery cathode material prepared in the embodiment adopts a Scanning Electron Microscope (SEM) to observe the surface of the material, obviously small particles are all adhered to form large particles, and the particles are relatively uniform and smooth after being adhered; as shown in fig. 1 and 2.
The high-capacity lithium battery anode material prepared by the method of the embodiment adopts a malvern laser particle sizer (MASTERSIZER 3000) to observe the particle size distribution of the anode material, and after small particles are bonded into large particles, the average particle size d50=16.9 μm is reasonable, and the particle size is shown in fig. 3.
The high-capacity lithium battery cathode material prepared by the method of the embodiment adopts a Wuhan blue electric test system CT2001A to test the multiplying power performance and capacity, and the charge capacity retention rate of the button battery after 0.2C is circularly changed for 100 weeks is more than 98%, so that the material has good cycle life; the capacity can still reach 178mAh/g above at different multiplying powers (0.1C, 0.2C, 0.5C, 1C and 2C), the data are shown in table 2, the specific capacity can be maintained above 365, and the first efficiency is above 95%. As shown in table 1 below.
Table 1 test of first cycle efficiency and first discharge specific Capacity Performance of high Capacity lithium Battery cathode Material prepared by the method of this example
Table 2 test data of the rate and capacity performance of the high capacity lithium battery anode material prepared by the method of this example
| Multiplying power | 0.1C | 0.2C | 0.5C | 1C | 2C |
| Capacity (mAh/g) | 368±10 | 350.9±3 | 339±4 | 245±2 | 178±2 |
It will be evident to those skilled in the art that the application is not limited to the details of the foregoing illustrative embodiments, and that the present application may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the application 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. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (2)
1. The preparation method of the power battery cathode material is characterized by comprising the following steps of:
step 1: crushing needle Jiao Shengjiao to obtain material with particle size less than or equal to 10mm, grinding to obtain raw coke with particle size D50=8-10 um, pulverizing asphalt with softening point of 350 deg.C to obtain powder with particle size D50=4-5 μm, mixing the raw coke with 5-20wt% of intermediate asphalt powder in VC mixer at normal temperature of 700rpm for 30min,
step 2: putting the materials uniformly mixed in the step 1 into a reaction kettle, heating and stirring at a low speed in the heating process, when the temperature of the reaction kettle reaches 360 ℃, stirring and mixing at a high speed for 1 hour, then reducing the temperature of the reaction kettle to 200 ℃,
step 3: adding high-temperature asphalt with a softening point of 240 ℃ into the material after the reaction in the step 2, heating the material to 250 ℃ and then continuously stirring for 30min,
step 4: granulating the material treated in the step 3, and then carrying out high-temperature graphitization at 2900-3000 ℃ to obtain a finished product.
2. The method for producing a negative electrode material for a power battery according to claim 1, wherein the low-speed stirring rotation speed is 40rpm and the high-speed stirring rotation speed is 700rpm.
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