CN112938958A - Surface modification method of negative electrode material - Google Patents
Surface modification method of negative electrode material Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a surface modification method of a negative electrode material, which is implemented by the step of modifying the particle diameter D50: mixing 8-10 μm coke powder and 2 wt% 10-200nm silicon carbide (SiC) powder, and blending in a blending machine for surface modification, wherein the surface modified coke powder and 5-10 wt% high-softening-point asphalt powder (D)50: 2-3 mu m) and then put into a reaction kettle for granulation and coating to obtain a coated raw material, and the raw material is graphitized to obtain the highly conductive graphite @ amorphous carbon and graphene composite negative electrode material. The invention is innovative in graphite negativeSilicon carbide (SiC) is added into the cathode material, so that the effects of dual increase of the conductivity and the rate quick charging performance of the cathode material are achieved.
Description
Technical Field
The invention relates to a surface modification method of a negative electrode material, and belongs to the technical field of a process method for modifying the surface of the negative electrode material in the field of negative electrode materials of lithium batteries.
Background
In recent years, with the rapid development of power supply technology and the rapid increase of hybrid power and pure electric vehicle requirements, people are more and more urgent to deeply research a convenient high-performance energy storage battery system, and the surface modification means of the lithium battery material can effectively improve the conductivity of the material and can bring more improvements to other properties of the material. To meet the requirement of high performance batteries, further improvement and innovation in improving the conductivity and rate capability of the batteries are still needed.
Disclosure of Invention
In order to solve the technical problem, the invention discloses a surface modification method of a negative electrode material, which comprises the following steps:
step 1: taking raw coke, crushing the raw coke until the particle size is less than or equal to 10mm, and grinding and shaping the crushed raw coke to obtain the coke with the particle size of D50The raw coke with the thickness of 8-10um,
step 2: taking silicon carbide (SiC), grinding the SiC to the particle size of 10-200nm,
and step 3: subjecting D in step 1 to50Mixing the raw coke with the diameter of 8-10um with the silicon carbide (SiC) with the diameter of 10-200nm in the step 2 for 30-50 minutes, then fusing for 40-60 minutes to obtain a mixture,
and 4, step 4: taking high-softening-point asphalt raw material, and crushing the high-softening-point asphalt raw material into D50＝2-3um，
And 5: the mixture obtained in the step (3) and the high-softening-point asphalt raw material obtained in the step (4) are mixed according to the proportion of 5 wt% -10 wt% (particle diameter D)502-3um) is granulated and then is continuously fused for 20-40 minutes to obtain a coating material,
step 6: and graphitizing the coating material to obtain a finished product, namely the high-conductivity graphite @ amorphous carbon and graphene composite negative electrode material.
Further, step (ii)1 the raw coke is crushed by a coarse crusher, and is milled and shaped by a mechanical mill and a shaping machine to obtain the coke with the particle size of D508-10um coke.
Further, the silicon carbide (SiC) in step 2 is ground by a high-energy ball mill.
Further, the mixing proportion of the silicon carbide (SiC) in the step 3 is 2 wt% -10 wt%, the mixing time is 40 minutes, and the fusion time is 60 minutes.
Further, the high-softening-point asphalt raw material in the step 4 is crushed by an asphalt crusher.
Further, the fusion time in step 5 is 30 minutes.
Further, in the step 6, the cladding material is graphitized through a graphitization furnace.
Has the advantages that: according to the invention, silicon carbide (SiC) is innovatively added into the graphite cathode material, and because the hardness of the silicon carbide is very high, the silicon carbide has the effect of grinding the surface of the raw material coke to be smoother, and part of the silicon carbide can be embedded into the surface of the raw material after long-time grinding; in addition, Si is evaporated after high-temperature graphitization, the remaining C atoms are reconstructed in a self-assembly form to obtain graphene, the generated graphene is left in graphite, a large amount of graphene is left on the outer surface of amorphous carbon, and a fine seam is left between a core and a shell after the Si is evaporated, so that more channels can be provided for the insertion of lithium ions, and the effects of doubly increasing the conductivity and multiplying power quick charge performance of the negative electrode material are achieved.
Drawings
FIG. 1 is a schematic structural diagram of a graphite @ amorphous carbon and graphene composite anode material of the invention,
FIG. 2-1 is a SEM schematic diagram of the graphite @ amorphous carbon and graphene composite anode material of the invention,
FIG. 2-2 is a SEM schematic diagram of the graphite @ amorphous carbon and graphene composite anode material of the invention,
FIG. 3 is a graph of the cycle performance of the graphite @ amorphous carbon and graphene composite anode material,
FIG. 4 is a graph of the rate capability of a graphite @ amorphous carbon and graphene composite anode material,
description of the drawings: 1-amorphous carbon shell, 2-Si evaporated fine seam, 3-graphene and 4-graphite.
Detailed Description
The present invention is further illustrated by the following figures and specific examples, which are to be understood as illustrative only and not as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
The invention discloses a surface modification method of a negative electrode material, which comprises the following steps:
step 1: taking raw coke, crushing the raw coke by a coarse crusher until the particle size is less than or equal to 10mm, and grinding and shaping the raw coke by a mechanical mill and a shaping machine to obtain the coke with the particle size D50The raw coke with the thickness of 8-10um,
step 2: taking silicon carbide (SiC), grinding the SiC to the particle size of 10-200nm by a high-energy ball mill,
and step 3: subjecting D in step 1 to50Mixing the raw coke with the size of 8-10um with the silicon carbide (SiC) with the size of 10-200nm in the step 2 for 30-50 minutes, and then fusing for 40-60 minutes to obtain a mixture, wherein the mixing ratio of the silicon carbide (SiC) is 2-10 wt%, the mixing time is preferably 40 minutes, the fusing time is preferably 60 minutes,
and 4, step 4: taking high-softening-point asphalt raw material, and crushing the high-softening-point asphalt raw material into D powder by an asphalt crusher50＝2-3um，
And 5: the mixture obtained in the step (3) and the high-softening-point asphalt raw material obtained in the step (4) are mixed according to the proportion of 5 wt% -10 wt% (particle diameter D)50: 2-3um) for 20-40 minutes, preferably for 30 minutes, to obtain a coating material,
step 6: graphitizing the coating material through a graphitizing furnace to obtain a finished product, namely the high-conductivity graphite @ amorphous carbon and graphene composite negative electrode material, wherein the structural schematic diagram is shown in fig. 1, an amorphous carbon shell 1, a fine seam 2 after Si evaporation, graphene 3 and graphite 4.
Examples
Preparing a negative electrode material:
1) taking raw coke, crushing the raw coke by a coarse crusher until the particle size is less than or equal to 10mm, and grinding and shaping the raw coke by a mechanical mill and a shaping machine to obtain the coke with the particle size D50The coke is a raw material coke with the thickness of 10um,
2) taking silicon carbide (SiC), grinding the SiC to the particle size of 100nm by a high-energy ball mill,
3) subjecting D described in step 1) to50Mixing the raw coke with the raw material coke of 10um and the silicon carbide (SiC) with the particle size of 100nm in the step 2) for 40 minutes, then fusing for 60 minutes to obtain a mixture, wherein the mixing proportion of the silicon carbide (SiC) is 2 wt%,
4) taking high-softening-point asphalt raw material, and crushing the high-softening-point asphalt raw material into D powder by an asphalt crusher50＝2-3um，
5) Mixing the mixture obtained in the step 3) and the high-softening-point asphalt raw material obtained in the step 4) according to the proportion of the high-softening-point asphalt raw material of 10 wt% (particle diameter D)50: 2-3um) for further fusion for 30 minutes to obtain a coating material,
6) graphitizing the coating material through a graphitizing furnace to obtain a finished product, namely the high-conductivity graphite @ amorphous carbon and graphene composite negative electrode material.
Preparing an electrode:
mixing the artificial graphite negative electrode material prepared in the embodiment, a conductive agent SP, a CMC (content of 1.2%) and an SBR (content of 45%) according to a mass ratio of 92:3:2:3 to prepare slurry, coating the slurry on a copper foil, and drying the copper foil in a vacuum drying oven for 12 hours to prepare a negative electrode sheet; and cutting the dried negative plate into a 14mm circular electrode plate on a manual sheet punching device, and finally assembling the battery in a glove box filled with argon. The counter electrode adopted in the experiment is a metal lithium sheet, the diaphragm is a Celgard 2300 polypropylene film, and the electrolytic liquid is a standard electrolyte EC of the Taihuarong LB303, DEC and DMC are 1:1:1LiPF61mol/L, and assembling into a button cell battery of CR2016 type.
And (3) material structure characterization:
the appearance of the negative electrode material was observed by a Jeol Scanning Electron Microscope (SEM) using a Jeol electron microscope (jiehuo), as shown in fig. 2-1 and 2-2, which are SEM schematic diagrams of the graphite @ amorphous carbon and graphene composite negative electrode material at different magnifications, and the particle size of the negative electrode material was measured by a malvern laser particle sizer (MASTERSIZER 3000).
Electrochemical testing:
the charging and discharging cycle and the rate capability test of the assembled charging are carried out by adopting a Wuhan blue electricity test system CT2001A, and the conductivity of the artificial graphite cathode material prepared in the embodiment is tested by adopting a four-probe method.
Data and effect:
table 1: the performance parameters of the graphite cathode material tested in this example
| Electrical conductivity of | s/cm | 18.6 |
| Particle size | μm | 17.5 |
| Specific capacity of initial discharge | mAh/g | 360 |
| First cycle efficiency | ％ | 95.01 |
As can be seen from the data in Table 1, the conductivity of the negative electrode material prepared by the method is 3 times that of common artificial graphite at 18.6s/cm, the material can greatly improve the conductivity of the battery, the first discharge specific capacity can reach more than 360mAh/g, the first cycle efficiency is more than 95%, and the granularity of 17.5 microns is kept within a qualified range. From FIG. 3, it can be seen that the cycle performance of the negative electrode material is still above 300mAh/g after 2000 cycles, and the negative electrode material has excellent cycle performance. From fig. 4, it can be known that the rate capability of the negative electrode material is more than 350mAh/g after 40 cycles from 0.1C, 0.2C, 0.5C, 1C, 1.5C, 2C, 2.5C to 3C, so the negative electrode material prepared by the method disclosed by the patent has high rate capability.
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. Any reference sign in a claim should not be construed as limiting the claim concerned.
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 (7)
1. A surface modification method of a negative electrode material is characterized by comprising the following steps:
step 1: taking raw coke, crushing the raw coke until the particle size is less than or equal to 10mm, and grinding and shaping the crushed raw coke to obtain the coke with the particle size of D50The raw coke with the thickness of 8-10um,
step 2: taking silicon carbide (SiC), grinding the SiC to the particle size of 10-200nm,
and step 3: subjecting D in step 1 to50Raw coke of 8-10um and 10-200nm as described in step 2Mixing silicon carbide (SiC) for 30-50 minutes, then fusing for 40-60 minutes to obtain a mixture,
and 4, step 4: taking high-softening-point asphalt raw material, and crushing the high-softening-point asphalt raw material into D50＝2-3um，
And 5: granulating the mixture obtained in the step 3 and the high-softening-point asphalt raw material obtained in the step 4 according to the proportion of 5-10 wt% (particle size D50: 2-3um) of the high-softening-point asphalt raw material, then continuously fusing for 20-40 minutes to obtain a coating material,
step 6: and graphitizing the coating material to obtain a finished product, namely the high-conductivity graphite @ amorphous carbon and graphene composite negative electrode material.
2. The method for modifying the surface of the negative electrode material according to claim 1, wherein the raw coke obtained in the step 1 is crushed by a coarse crusher, ground by a mechanical mill and a shaper to obtain a particle size D508-10um coke.
3. The method for modifying the surface of the anode material according to claim 1, wherein the silicon carbide (SiC) in the step 2 is ground by a high-energy ball mill.
4. The method for modifying the surface of the anode material according to claim 1, wherein the silicon carbide (SiC) is mixed in the step 3 at a ratio of 2 wt% to 10 wt%, and the mixing time is 40 minutes and the fusion time is 60 minutes.
5. The method for modifying the surface of the negative electrode material according to claim 1, wherein the high-softening-point asphalt material obtained in the step 4 is pulverized by an asphalt pulverizer.
6. The method for modifying the surface of the anode material according to claim 1, wherein the fusing time in the step 5 is 30 minutes.
7. The method for modifying the surface of the negative electrode material according to claim 1, wherein the coating material in step 6 is graphitized at a high temperature by a graphitization furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113422030A (en) * | 2021-06-29 | 2021-09-21 | 贝特瑞新材料集团股份有限公司 | Negative electrode material and preparation method thereof, battery negative electrode and lithium ion battery |
| RU2797909C1 (en) * | 2022-11-22 | 2023-06-13 | Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Anode material of a lithium-ion current source and method for its manufacture |
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