CN106532051B - Method for preparing power lithium ion battery cathode material by using natural graphite - Google Patents
Method for preparing power lithium ion battery cathode material by using natural graphite Download PDFInfo
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- CN106532051B CN106532051B CN201510631290.4A CN201510631290A CN106532051B CN 106532051 B CN106532051 B CN 106532051B CN 201510631290 A CN201510631290 A CN 201510631290A CN 106532051 B CN106532051 B CN 106532051B
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- 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
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- 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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Abstract
The invention discloses a method for preparing a power lithium ion battery cathode material by utilizing natural graphite, which comprises the steps of mixing microcrystalline graphite and flaky graphite, mixing the mixture with binder asphalt, carrying out compound granulation, carrying out graphitization purification, iron removal, shaping and grading to prepare graphite powder; coating and modifying the obtained graphite powder by using phenolic resin to prepare the negative electrode material of the power lithium ion battery, wherein the particle size distribution of the negative electrode material is that D10 is 0-10 mu m, D50 is 11-25 mu m, D90 is 26-60 mu m, and the tap density is 0.9-1.2 g/cm 3The content of the fixed carbon is 99.0-99.9%, and the graphitization degree is 90-96%. The power lithium ion battery cathode material prepared by the invention has the characteristics of high capacity, small expansion and good rate capability.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a method for preparing a power lithium ion battery cathode material by using natural graphite.
Background
The graphite material for the lithium ion battery negative electrode has the advantages of low discharge platform, high true density, high lithium insertion capacity, high first charge and discharge efficiency and the like. The negative electrode material widely used at present is mostly a graphite carbon negative electrode, and mainly comprises the following components: natural graphite and artificial graphite.
The natural graphite refers to a natural graphite material obtained by mining, flotation, screening and purifying natural graphite ores. Graphite particles can be classified into foliated graphite, flaky graphite and microcrystalline graphite according to their shapes and crystallite sizes. At present, the practical natural graphite is mainly flaky graphite, but the flaky graphite is poor in compatibility with electrolyte, an organic solvent and lithium ions are jointly embedded into a graphite sheet layer to be reduced to generate gas, and part of lithium is consumed, so that the first efficiency is low; in the process of charging and discharging, the graphite sheet layer repeatedly expands and contracts, so that the graphite layer is peeled off and pulverized, and the cycle stability is influenced. To obtain a carbon material for a high-performance negative electrode, U.S. patent nos.: 5908715, 1999, 6.1, discloses a method for coating hard carbon on the surface of graphite, which is characterized in that the synthetic process of resin and coating are carried out simultaneously, but the method is difficult to implement. In addition, the patent numbers of China: CN1129194C, 11/26/2003 discloses a preparation method of a carbon/carbon composite material. These methods are all aimed at improving certain drawbacks of natural graphite.
The macroscopic isotropy of the microcrystalline graphite enables the cycle stability of the microcrystalline graphite to be superior to that of the flaky graphite, the c-axis expansion amount of the flaky graphite in the lithium ion intercalation process can reach 10%, and the unidirectional expansion amount of the microcrystalline graphite is about 3% due to the isotropic property, so that the structure is not easy to damage. But the microcrystalline graphite has lower mechanical strength and is very easy to pulverize in the traditional crushing, shaping and other processes, so that a large amount of fine powder is generated to reduce the yield of the final product.
Disclosure of Invention
The invention aims to provide a method for preparing a power lithium ion battery cathode material by using natural graphite, which has high capacity, small expansion, good rate capability and good cycle stability, and solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
A method for preparing a power lithium ion battery cathode material by using natural graphite comprises the following steps:
Firstly, taking microcrystalline graphite with the fixed carbon content of 60-99% and crushing the microcrystalline graphite into powder A with the D10 of 0-4 microns, the D50 of 4-8 microns and the D90 of 10-60 microns through a jet mill; taking scaly graphite with the fixed carbon content of 99 percent, crushing the scaly graphite into powder B with the D10 of 0-4 mu m, the D50 of 4-8 mu m and the D90 of 10-60 mu m by using a jet mill, and mixing the two kinds of powder in a high-speed mixer to obtain mixed natural graphite;
Step two, mixing the mixed natural graphite obtained in the step one with binder asphalt to obtain a mixture, wherein the binder asphalt accounts for 10-50% of the mixture by mass; carrying out compound granulation on the mixture in mixed granulation equipment to obtain powder C with the particle size distribution of D10 being 0-10 mu m, D50 being 11-25 mu m and D90 being 26-60 mu m;
Step three, carrying out graphitization purification on the powder C obtained in the step two, wherein the graphitization temperature is 2000-3500 ℃, carrying out constant temperature reaction for 0-12 hours, then carrying out iron removal, and sieving with a 200-325-mesh sieve to obtain a material;
Shaping the materials by using a ball mill, and then grading to prepare graphite powder; and coating and modifying the obtained graphite powder by using phenolic resin to obtain the negative electrode material of the power lithium ion battery.
As a further scheme of the invention: the addition amount of the phenolic resin is 0-15% of the total mass of the phenolic resin and the graphite powder.
Compared with the prior art, the invention has the beneficial effects that: the power lithium ion battery cathode material prepared by the invention has the particle size distribution of D10 of 0-10 mu m, D50 of 11-25 mu m, D90 of 26-60 mu m and the tap density of 0.9-1.2 g/cm 3The content of fixed carbon is 99.0-99.9%, and the graphitization degree is 90-96%; has the characteristics of high capacity, small expansion, good rate capability, good cycle stability and the like.
Drawings
FIG. 1 is a micro-topography of a conventional graphite anode material;
FIG. 2 is a microscopic morphology of the prepared negative electrode material of the power lithium ion 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, a method for preparing a power lithium ion battery cathode material by using natural graphite comprises the following implementation steps:
Step 1, selecting aphanitic graphite with fixed carbon content of 80%, crushing and grading to obtain powder A with particle size distribution of D10 of 1.2 microns, D50 of 8 microns and D90 of 25 microns.
And 2, selecting spherical flaky graphite with the fixed carbon content of 99.9%, crushing and grading to obtain powder B with the particle size distribution of D10 of 2.5 microns, D50 of 8 microns and D90 of 43 microns.
And 3, fully mixing the powder A and the powder B in a mixer, wherein the proportion of the powder A in the mixed material is 40%, and the added asphalt accounts for 12% of the mass of the mixture. Carrying out compound granulation in a mixing granulation device, wherein the granulation temperature is 500 ℃, and finally obtaining powder C with the particle size distribution of D10 of 3.8 μm, D50 of 16 μm and D90 of 45 μm.
And 4, heating the powder C obtained in the step 3 to 3000 ℃ for constant-temperature reaction for 12 hours to discharge high-boiling-point impurities.
Step 5, crushing and grading the purified graphite powder obtained in the step 4, and sieving the crushed graphite powder with a 250-mesh sieve to obtain the graphite powder with the D10 of 3.6 microns, the D50 of 16.2 microns, the D90 of 46.3 microns, and the tap density of 1.0g/cm 3The cathode material of the power lithium ion battery has the fixed carbon content of 99.99 percent and the graphitization degree of 92 percent.
Example 2
In the embodiment of the invention, a method for preparing a power lithium ion battery cathode material by using natural graphite comprises the following implementation steps:
Step 1, selecting aphanitic graphite with fixed carbon content of 60%, crushing and grading to obtain powder A with particle size distribution of D10 of 0.5 μm, D50 of 4 μm and D90 of 10 μm.
And 2, selecting spherical flaky graphite with the fixed carbon content of 99.9%, crushing and grading to obtain powder B with the particle size distribution of D10 of 0.5 mu m, D50 of 4 mu m and D90 of 10 mu m.
And 3, fully mixing the powder A and the powder B in a mixer, wherein the proportion of the powder A in the mixed material is 40%, and the added asphalt accounts for 10% of the mass of the mixture. Carrying out compound granulation in a mixing granulation device, wherein the granulation temperature is 500 ℃, and finally obtaining powder C with the particle size distribution of D10 of 1.2 μm, D50 of 11 μm and D90 of 26 μm.
And 4, heating the powder C obtained in the step 3 to 2000 ℃, reacting for 2 hours at a constant temperature to discharge high-boiling-point impurities, and sieving with a 200-mesh sieve.
Step 5, crushing and grading the purified material obtained in the step 4 to prepare graphite powder, and obtaining the graphite powder by using phenolic resin with the total mass of 15 percent of the phenolic resin and the graphite powder The obtained graphite powder is coated and modified to obtain the graphite powder with the D10 of 3.6 mu m, the D50 of 16.2 mu m, the D90 of 46.3 mu m, and the tap density of 1.2g/cm 3The cathode material of the power lithium ion battery has the fixed carbon content of 99.99 percent and the graphitization degree of 96 percent.
Example 3
In the embodiment of the invention, a method for preparing a power lithium ion battery cathode material by using natural graphite comprises the following implementation steps:
Step 1, selecting aphanitic graphite with fixed carbon content of 80%, crushing and grading to obtain powder A with particle size distribution of D10 of 4 microns, D50 of 6 microns and D90 of 60 microns.
And 2, selecting spherical flaky graphite with the fixed carbon content of 99.9%, crushing and grading to obtain powder B with the particle size distribution of 4 microns D10, 6 microns D50 and 60 microns D90.
And 3, fully mixing the powder A and the powder B in a mixer, wherein the proportion of the powder A in the mixed material is 40%, and the added asphalt accounts for 30% of the mass of the mixture. Carrying out compound granulation in a mixing granulation device, wherein the granulation temperature is 500 ℃, and finally obtaining powder C with the particle size distribution of 10 μm D10, 25 μm D50 and 60 μm D90.
And 4, heating the powder C obtained in the step 3 to 3000 ℃ for constant-temperature reaction for 12 hours to discharge high-boiling-point impurities, and sieving with a 325-mesh sieve.
Step 5, crushing and grading the purified material obtained in the step 4 to obtain graphite powder, coating and modifying the obtained graphite powder by using phenolic resin accounting for 7% of the total mass of the phenolic resin and the graphite powder to obtain the graphite powder with the D10 of 3.6 microns, the D50 of 16.2 microns, the D90 of 46.3 microns and the tap density of 1.1g/cm 3The cathode material of the power lithium ion battery has the fixed carbon content of 99.99 percent and the graphitization degree of 94.24 percent.
The comprehensive performance parameters of the power lithium ion battery negative electrode material obtained in the above embodiment are shown in table 1. The micro-topography of the prepared negative electrode material of the power lithium ion battery is shown in fig. 2, and is compared with the micro-topography of the conventional graphite negative electrode material in fig. 1.
TABLE 1
| Particle size | Tap density | Ash content | Discharge capacity | Efficiency of discharge | Degree of graphitization |
| 15.6μm | 1.1g/cm3 | ≤0.1％ | 347.8mAh/g | ≥90％ | 94.08％ |
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 (2)
1. A method for preparing a power lithium ion battery cathode material by using natural graphite is characterized by comprising the following steps:
Firstly, taking microcrystalline graphite with the fixed carbon content of 60-99% and crushing the microcrystalline graphite into powder A with the D10 of 0-4 microns, the D50 of 4-8 microns and the D90 of 10-60 microns through a jet mill; taking scaly graphite with the fixed carbon content of 99 percent, crushing the scaly graphite into powder B with the D10 of 0-4 mu m, the D50 of 4-8 mu m and the D90 of 10-60 mu m by using a jet mill, and mixing the two kinds of powder in a high-speed mixer to obtain mixed natural graphite;
Step two, mixing the mixed natural graphite obtained in the step one with binder asphalt to obtain a mixture, wherein the binder asphalt accounts for 10-50% of the mixture by mass; carrying out compound granulation on the mixture in mixed granulation equipment to obtain powder C with the particle size distribution of D10 being 0-10 mu m, D50 being 11-25 mu m and D90 being 26-60 mu m;
Step three, carrying out graphitization purification on the powder C obtained in the step two, wherein the graphitization temperature is 2000-3500 ℃, carrying out constant temperature reaction for 0-12 hours, then carrying out iron removal, and sieving with a 200-325-mesh sieve to obtain a material;
Shaping the materials by using a ball mill, and then grading to prepare graphite powder; and coating and modifying the obtained graphite powder by using phenolic resin to obtain the negative electrode material of the power lithium ion battery.
2. The method for preparing the negative electrode material of the power lithium ion battery by using the natural graphite as claimed in claim 1, wherein the addition amount of the phenolic resin is 0-15% of the total mass of the phenolic resin and the graphite powder.
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| CN107146880A (en) * | 2017-03-24 | 2017-09-08 | 宁波杉杉新材料科技有限公司 | A kind of high magnification fills the preparation method of graphite soon |
| CN107522197A (en) * | 2017-09-15 | 2017-12-29 | 福建翔丰华新能源材料有限公司 | The method of the preparation high-purity of economy, the micro crystal graphite of high graphitization degree |
| KR102277734B1 (en) * | 2018-02-26 | 2021-07-16 | 주식회사 엘지에너지솔루션 | Negative electrode active material for lithium secondary battery, negative electrode for lithium secondry battery and lithium secondary battery comprising the same |
| CN109346707A (en) * | 2018-11-15 | 2019-02-15 | 桑顿新能源科技有限公司 | A kind of cathode material of lithium ion battery and preparation method thereof and lithium ion battery |
| CN109599546B (en) * | 2018-12-05 | 2020-12-04 | 中南大学 | Asphalt carbon-coated natural mixed graphite material and method for preparing lithium ion battery cathode by using same |
| CN112201776B (en) * | 2019-07-08 | 2022-02-08 | 宁波杉杉新材料科技有限公司 | Natural graphite negative electrode material, preparation method thereof and lithium ion battery |
| CN111072012B (en) * | 2019-12-14 | 2023-05-23 | 内蒙古杉杉科技有限公司 | Microcrystalline graphite graphene-doped negative electrode material of lithium ion battery and preparation method thereof |
| CN112670461B (en) * | 2019-12-31 | 2022-11-29 | 宁波杉杉新材料科技有限公司 | Natural graphite carbon coated negative electrode material, preparation method thereof and lithium ion battery |
| CN111232971B (en) * | 2020-01-17 | 2021-10-15 | 广东东岛新能源股份有限公司 | Long-circulation natural graphite-based modified composite material and preparation method and application thereof |
| CN112670464B (en) * | 2020-04-21 | 2022-02-18 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material, lithium ion battery and preparation method and application of graphite negative electrode material |
| CN112366315A (en) * | 2020-11-30 | 2021-02-12 | 河南开炭新材料设计研究院有限公司 | Production method of lithium battery negative electrode material |
| CN113800912A (en) * | 2021-11-04 | 2021-12-17 | 大连宏光锂业股份有限公司 | High compaction rate type lithium ion battery cathode material and preparation method thereof |
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| CN1851963A (en) * | 2006-05-19 | 2006-10-25 | 湛江市聚鑫电子材料有限公司 | Lithium-ion cell composite carbon negative polar material and preparing method |
| CN102148355A (en) * | 2011-03-03 | 2011-08-10 | 江西正拓新能源科技有限公司 | Cathode material for lithium-ion power battery and preparation method thereof |
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