CN115275154A - Method for preparing high-performance silicon-carbon negative electrode from natural graphite spherical tailings - Google Patents

Method for preparing high-performance silicon-carbon negative electrode from natural graphite spherical tailings Download PDF

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CN115275154A
CN115275154A CN202211006974.1A CN202211006974A CN115275154A CN 115275154 A CN115275154 A CN 115275154A CN 202211006974 A CN202211006974 A CN 202211006974A CN 115275154 A CN115275154 A CN 115275154A
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tailings
spherical
natural graphite
silicon
ball milling
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公旭中
李佳丽
付雨龙
孟悦
王志
刘俊昊
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Institute of Process Engineering of CAS
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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
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • 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
    • 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a method for preparing a high-performance silicon-carbon cathode by using high-performance natural graphite spherical tailings, belonging to the field of secondary resource utilization. The method takes natural graphite small-size sheet spherical tailings combined with micron waste silicon powder as a raw material, and comprises the following steps: firstly, oxidizing natural spherical graphite tailings, washing, drying, putting the oxidized natural spherical graphite tailings and waste silicon powder into a mechanical ball mill for high-speed mixing, and finally, coating and carbonizing the composite material to obtain a final product. When the modified material is used as a lithium battery negative electrode material, the capacity is high and the stability is good. The invention takes natural graphite spheroidization tailing and waste silicon powder as raw materials, obtains the high-performance silicon-carbon cathode by modification, realizes high-value utilization of waste materials, has simple and controllable production process, and is suitable for large-scale industrial production.

Description

Method for preparing high-performance silicon-carbon negative electrode from natural graphite spherical tailings
Technical Field
The invention belongs to the technical field of lithium ion batteries, and discloses a method for preparing a high-performance silicon-carbon negative electrode material from natural graphite spherical tailings.
Background
With the increase of the market demand for high specific energy density lithium ion batteries, the lithium ion batteries are required to have high energy density and safety performance, and the negative electrode is a key material influencing the energy density and safety performance of the lithium ion batteries. The current commercialized negative electrode material mainly takes a high-capacity graphite material as a main material, has advantages in the aspects of cycle performance, price, material source and the like, but has low specific capacity (the theoretical specific capacity is 372mA h/g), and is difficult to meet the storage requirement of a battery with higher capacity. So that a high capacity silicon negative electrode is used.
Silicon has attracted most of the research interest over the past decades and is considered to be the most attractive and promising high performance anode material to replace the traditional graphite anode material. Due to its highest theoretical specific capacity (about 4200mA h/g), the capacity of silicon is approximately 10 times higher than that of the graphite anode. In addition, other advantages of Si include low discharge potential (about 0.5V), high natural abundance, safety, and environmental friendliness. However, the large volume change (about 300%) of silicon-based anodes during cycling limits their practical applications. The critical mechanical strain of the silicon particles leads to electrode pulverization, instability of the solid electrolyte interface film (SEI), and electrical disconnection of the silicon electrode from the current collector, resulting in rapid decay of the silicon-based anode capacity. In addition, silicon has poor intrinsic conductivity, limiting transport at fast Li + high current densities.
For silicon-carbon composite materials, silicon can improve the specific capacity of the materials, but the biggest problem is that the formation of silicon-lithium alloy is accompanied by huge volume change in the using process, the addition of graphite can buffer the breakage of the silicon-lithium alloy, in addition, the low-mass load (generally lower than 0.5mg/cm < 2 >) of the silicon-based active material is caused to have lower area capacity and energy density although the specific capacity is very high, the addition of graphite is also one of the methods for solving the low-mass load, and simultaneously, the problem of poor silicon conductivity is solved, namely, the graphite increases the lithium intercalation speed of silicon in both the transverse direction and the longitudinal direction. The main means for solving the problem at present is to utilize the fluidity of other carbon sources at high temperature for coating and granulation.
In the process of spheroidization of natural crystalline flake graphite, the effective utilization rate is only 50%, and the amount of spherical tailings generated in China every year can reach 20 ten thousand tons. The spherical tailing is solid waste generated in the spheroidization process of natural flake graphite, is characterized by small and nonuniform size, but has high fixed carbon proportion (more than 95 percent) and is still high-purity natural flake graphite, has high conductivity and good lithium ion transmission capability, has small size, belongs to lamellar graphite and has certain flexibility. Meanwhile, due to the rapid development of the photovoltaic industry, the yield of the solar-grade crystalline silicon is gradually increased year by year. In the production of these crystalline silicon plates, the waste silicon powder produced by cutting accounts for 40% of the total silicon mass. Therefore, the silicon-carbon solid waste has high yield, low resource utilization rate and great recycling space, and is a cathode material capable of being industrially utilized.
Disclosure of Invention
In order to solve the problem of poor stability of natural graphite spherical tailings and waste silicon powder, the invention provides a lithium ion battery silicon-carbon composite negative electrode material and a preparation method thereof, wherein a stable silicon-carbon negative electrode structure is constructed by coating after mechanical ball milling, and the preparation method comprises the following specific steps:
step 1: weighing a certain mass of purified natural graphite spherical tailings, adding a certain amount of oxidant, stirring at room temperature, and carrying out oxidation treatment to obtain a product 1;
and 2, step: performing ball milling granulation on the product 1 and the purified waste silicon powder according to a certain proportion to obtain a target material;
and 3, step 3: and coating the target material, and carbonizing at a specific temperature to obtain a final product.
Further, in the step 1, the particle size D50 of the spherical tailings is 100 nm-20 μm, and the content of the purified fixed carbon is more than 99%. The particle diameter D50 of the waste silicon powder is 1-200 mu m, and the purity of the acid-washed waste silicon powder is more than 99 percent.
Further, the oxidant in the step 1 can be one or a plurality of the following reagents, concentrated sulfuric acid, concentrated hydrochloric acid, hydrogen peroxide, potassium permanganate and sodium hydroxide, the effective content of the oxidant accounts for 2-200% of the mass fraction of the graphite spherical tailings, and the reaction time is 1-48 h;
further, ball milling is carried out on the natural graphite spherical tailings and the waste silicon powder after mixing in the step 2, wherein the proportion of graphite is 95% -70%, the ball milling speed is 200 rpm-700 rpm, and the ball milling time is 1 h-10 h;
further, the coating agent in the step 3 can be one or more of the following mixtures: citric acid, coal tar, glucose, phenolic resin, polyvinylpyrrolidone and biomass tar, wherein the carbonization temperature is 100-1200 ℃, the heat preservation time is 10-600 min, and the carbonization is argon atmosphere, nitrogen atmosphere or hydrogen-argon mixed atmosphere (wherein the hydrogen ratio is 5%).
The invention aims to combine the characteristics of natural graphite spherical tailings and waste silicon powder raw materials, modify the structures of the natural graphite spherical tailings and the waste silicon powder through ball milling, and combine a carbon material for coating to finally obtain the graphite silicon carbon composite material with good cycle stability. The natural graphite spherical tailing and the waste silicon powder are both flaky and have fine particles. The graphite and silicon ball milling and the heat curing bonding can realize the reconstruction of the nano-micro structure of the composite material and reduce the specific surface area of the negative electrode.
The method disclosed by the invention is simple to operate, the required modifiers are all conventional cheap reagents, and the raw materials and the synthesis process are suitable for large-scale production, so that the prepared cathode material has a great application prospect in lithium ion batteries.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is an SEM image of natural graphite spherical tailings and waste silicon powder before and after ball milling in the specific example 1 of the present invention: a) Purifying the natural graphite spherical tailing SEM picture; b) SEM image of purified waste silicon powder; c) SEM images of ball-milled natural graphite spherical tailings and waste silicon powder; d) SEM image of the composite after carbonization.
Fig. 3 is a blue test cycle stability chart of natural graphite spherical tailings and waste silicon powder before and after ball milling and after coating in embodiment 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
Placing the purified natural graphite spherical tailings with a certain mass and H2O2 accounting for 30% of the mass fraction of the graphite tailings into a beaker to form a mixture, wherein the solid-to-liquid ratio of graphite to H2O2 is 1: and 50, stirring at room temperature for 6 hours, washing the suspension after reaction with a large amount of deionized water, performing suction filtration and drying to obtain a product 1. And mixing the product 1 with the purified waste silicon powder, and putting the mixture into a ball milling tank, wherein the mass ratio of the waste silicon powder to the ball tail is 1:4, the rotating speed of the ball mill is 400rpm, the ball milling time is 10 hours, the composite material is obtained by sieving the composite material with a 200-mesh sieve and carrying out magnetic removal treatment, and then the composite material is compounded with glucose, wherein the mass ratio of the composite material to the glucose is 97: and 3, fully mixing the two, and then coating the target product by using glucose, wherein the carbonization temperature is 900 ℃, the time is 180min, and the protective atmosphere is argon.
A scanning electron microscope (JSM-7800) is used for observing the morphology of the modified natural graphite spherical tailing negative electrode material under the conditions, and is shown in figure 2.
The silicon-carbon negative electrode material prepared in example 1 was directly used as a negative electrode material of a lithium ion battery, and a button cell was assembled in an argon-protected glove box by using a metal lithium sheet as a counter electrode, celgard2325 as a diaphragm, and 1mol/L LiPF6 (a solvent is a mixed solution of ethylene carbonate and dimethyl carbonate at a volume ratio of 1:1) as an electrolyte, and a CR2032 type button cell case. And (3) a charge-discharge test, wherein the charge-discharge current density is 0.1A/g and the voltage charge-discharge interval is 0.01-3V in the program. The charge and discharge cycle performance of the battery is shown in fig. 3, the specific capacity of the silicon-carbon negative electrode before ball milling is 172mA h/g, the specific capacity of the silicon-carbon negative electrode after ball milling is 1208mA h/g, the silicon-carbon negative electrode is carbonized after ball milling, the specific capacity of the silicon-carbon negative electrode is 1246mA h/g, and the modified negative electrode material shows higher capacity and cycle stability.
Example 2
Placing a certain mass of purified natural graphite spherical tailings, sulfuric acid (with the concentration of 98.8 wt.%), which accounts for 5% of the mass fraction of the graphite tailings, and 30% of H2O2 in a beaker to form a mixture, using deionized water to perform constant volume according to a solid-to-liquid ratio of 1: 95, the rotating speed of the ball mill is 700rmp, the ball milling time is 5 hours, the composite material is obtained by sieving the mixture through a 200-mesh sieve and carrying out magnetic removal treatment, and then the composite material is compounded with polyvinylpyrrolidone, wherein the mass ratio of the composite material to the polyvinylpyrrolidone is 97: and 3, fully mixing the two, and then coating and carbonizing the mixture, wherein the carbonizing temperature is 800 ℃, the carbonizing time is 180min, and the protective atmosphere is argon. And (3) assembling the final material into a half-button cell to carry out charge and discharge performance test, wherein the specific capacity of the silicon-carbon cathode is 168mA h/g before ball milling, the specific capacity of the silicon-carbon cathode is 1200mA h/g after ball milling, carbonization is carried out after ball milling, the specific capacity of the silicon-carbon cathode is 1250mA h/g, and the modified cathode material shows higher capacity and cycling stability.
Example 3
Putting the purified natural graphite spherical tailings with a certain mass and sodium hydroxide accounting for 50% of the mass of the graphite tailings into a beaker, and adding deionized water into the beaker according to a solid-to-liquid ratio of 1:50, fixing the volume, stirring at room temperature for 1h, then increasing the temperature of the mixture to 90 ℃, stirring for 5h, then cooling the reaction mixture to room temperature, neutralizing with HCl (0.1M) until the pH is =7, performing suction filtration, cleaning and drying on the suspension after reaction to obtain a product 1, putting the product 1 and purified waste silicon powder into ethanol, and performing ultrasonic treatment for 1h, wherein the solid-to-liquid ratio of silicon graphite to ethanol is 1:200, drying, putting into a ball milling tank, ball milling for 10h, sieving by a 200-mesh sieve, and carrying out demagnetization treatment to obtain the composite material, dissolving the coal tar pitch in a certain amount of tetrahydrofuran, wherein the solid-to-liquid ratio is 1:200, and then compounding the composite material and tetrahydrofuran-dissolved coal tar pitch, wherein the mass ratio of the composite material to the coal tar pitch is 98:2, mixing the two solutions thoroughly to obtain a viscous liquid mixture, and then subjecting the mixture to 900 deg.C for 180min under a hydrogen-argon atmosphere (wherein hydrogen is 5%). And (3) assembling the final material into a half-button cell to carry out charge and discharge performance test, wherein the specific capacity of the silicon-carbon cathode is 171mA h/g before ball milling, the specific capacity of the silicon-carbon cathode is 1205mA h/g after ball milling, carbonization is carried out after ball milling, the specific capacity of the silicon-carbon cathode is 1258mA h/g, and the modified cathode material has higher capacity and cycling stability.
Example 4
Placing the purified natural graphite spherical tailings with a certain mass, potassium permanganate solid powder accounting for 5% of the mass fraction of the graphite tailings and H2O2 (with the concentration of 30 wt.%) accounting for 5% of the mass fraction in a beaker to form a mixture, using deionized water to perform constant volume according to a solid-to-liquid ratio of 1. And mixing the product 1 with the purified waste silicon powder, and putting the mixture into a ball milling tank, wherein the mass ratio of the waste silicon powder to the ball tail is 3:7, ball milling at 700rmp for 5h, sieving with a 200-mesh sieve to obtain a composite material, dissolving phenolic resin in a proper amount of absolute ethanol, adding the composite material, mixing and coating, wherein the carbonization temperature is 700 ℃, the time is 360min, and the protective atmosphere is nitrogen. And (3) assembling the final material into a half-button cell for carrying out charge and discharge performance test, wherein the specific capacity of the silicon-carbon cathode is 172mA h/g before ball milling, the specific capacity of the silicon-carbon cathode is 1212mA h/g after ball milling, carbonization is carried out after ball milling, the specific capacity of the silicon-carbon cathode is 1240mA h/g, and the modified cathode material has higher capacity and cycling stability.
Example 5
Placing a certain mass of purified natural graphite spherical tailings and nitric acid (with the concentration of 68 wt.%), which accounts for 50% of the mass fraction of the graphite tailings, in a beaker to form a mixture, performing constant volume by using deionized water according to a solid-to-liquid ratio of 1: and 9, the rotating speed of the ball mill is 500rmp, the ball milling time is 5 hours, the composite material is obtained by sieving the composite material through a 200-mesh sieve and carrying out demagnetization treatment, citric acid is adopted to carry out coating treatment on the composite material, the carbonization temperature is 700 ℃, the time is 180min, and the protective atmosphere is nitrogen. And (3) assembling the final material into a half-button cell for carrying out charge and discharge performance test, wherein the specific capacity of the silicon-carbon cathode is 174mA h/g before ball milling, the specific capacity of the silicon-carbon cathode is 1203mA h/g after ball milling, carbonization is carried out after ball milling, the specific capacity of the silicon-carbon cathode is 1248mA h/g, and the modified cathode material shows higher capacity and cycling stability.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.

Claims (5)

1. A method for preparing a high-performance silicon-carbon negative electrode by using natural graphite spherical tailings is characterized by comprising the following steps:
step 1: weighing a certain mass of purified natural graphite spherical tailings, adding a certain amount of oxidant, stirring at room temperature for oxidation treatment, washing the oxidized graphite with deionized water for multiple times, and then performing suction filtration and drying to obtain a product 1;
and 2, step: mixing the product 1 with silicon powder according to a certain proportion, and then carrying out ball milling to obtain a product 2;
and step 3: and coating the product 2, and carbonizing at a specific temperature to obtain a final product.
2. The method for preparing the high-performance silicon-carbon cathode by using the natural graphite spherical tailings as the raw material in the step 1 is characterized in that the particle size D50 of the spherical tailings in the step 1 is 100 nm-20 microns, and the content of the purified fixed carbon is more than 99%. The particle diameter D50 of the waste silicon powder is 1-200 μm, and the purity of the acid-washed waste silicon powder is more than 99 percent.
3. The method for preparing the high-performance silicon-carbon cathode by using the natural graphite spherical tailings as claimed in claim 1, wherein the oxidant in the step 1 can be one or a combination of concentrated sulfuric acid, concentrated hydrochloric acid, hydrogen peroxide, potassium permanganate and sodium hydroxide, the effective content of the oxidant accounts for 2% -200% of the mass of the graphite spherical tailings, and the reaction time is 1-48 h.
4. The method for preparing the high-performance silicon-carbon cathode by using the natural graphite spherical tailings as the raw material in the step 2 is characterized in that the natural graphite spherical tailings and the waste silicon powder are mixed and then subjected to ball milling, wherein the proportion of graphite is 95-70%, the ball milling speed is 200-700 rpm, and the ball milling time is 1-10 h.
5. The method for preparing the high-performance silicon-carbon negative electrode by using the natural graphite spherical tailings as claimed in claim 1, wherein the coating agent in the step 3 can be one or more of the following mixtures: citric acid, coal tar, glucose, phenolic resin, polyvinylpyrrolidone and biomass tar, wherein the carbonization temperature is 100-1200 ℃, the heat preservation time is 10-600 min, and the carbonization is argon atmosphere, nitrogen atmosphere or hydrogen-argon mixed atmosphere (wherein the hydrogen ratio is 5%).
CN202211006974.1A 2022-08-22 2022-08-22 Method for preparing high-performance silicon-carbon negative electrode from natural graphite spherical tailings Pending CN115275154A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116598465A (en) * 2023-06-19 2023-08-15 深圳光风新能源科技创新中心有限公司 High-rate lithium battery negative electrode material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116598465A (en) * 2023-06-19 2023-08-15 深圳光风新能源科技创新中心有限公司 High-rate lithium battery negative electrode material and preparation method thereof
CN116598465B (en) * 2023-06-19 2024-04-05 深圳光风新能源科技创新中心有限公司 High-rate lithium battery negative electrode material and preparation method thereof

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