CN107180958B - Anthracite/silicon monoxide/amorphous carbon negative electrode material and preparation method thereof - Google Patents

Anthracite/silicon monoxide/amorphous carbon negative electrode material and preparation method thereof Download PDF

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CN107180958B
CN107180958B CN201710414858.6A CN201710414858A CN107180958B CN 107180958 B CN107180958 B CN 107180958B CN 201710414858 A CN201710414858 A CN 201710414858A CN 107180958 B CN107180958 B CN 107180958B
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anthracite
sio
negative electrode
electrode material
amorphous carbon
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CN107180958A (en
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杨学林
宋凡
张斐
吴璇
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O'cell New Energy Technology Co ltd
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China Three Gorges University CTGU
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • 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
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    • 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 provides an anthracite/silicon monoxide/amorphous carbon composite negative electrode material and a preparation method thereof. The composite negative electrode material is prepared by dispersing amorphous SiO, anthracite and citric acid through mechanical ball milling, and then sintering to obtain a powdery lithium ion battery negative electrode material with the particle size of about 13-15 microns. The preparation method of the anthracite/silicon monoxide/amorphous carbon composite negative electrode material comprises the following steps: the preparation method comprises the steps of crushing anthracite coal, removing impurities, performing high-temperature treatment, mixing the anthracite coal with SiO, adding citric acid for coating, performing mechanical ball milling and compounding to obtain a precursor, and performing high-temperature treatment to obtain the high-specific-capacity lithium ion battery negative electrode material. The composite material effectively combines the good conductivity of the carbon material and the high lithium storage capacity of SiO, shows excellent electrochemical performance, has the reversible capacity of 459.2 mAh/g after being circulated for 100 circles under the condition of 0.1A/g, and provides certain feasible selection for the practicability of the SiO negative electrode material.

Description

Anthracite/silicon monoxide/amorphous carbon negative electrode material and preparation method thereof
Technical Field
The invention relates to an anthracite/silicon monoxide/amorphous carbon composite negative electrode material of a lithium ion battery and a preparation method thereof, belonging to the field of electrochemistry.
Background
Lithium ion batteries have become the most important energy storage devices for various electronic products, wireless communication and transportation facilities, etc. due to their excellent properties (such as high working voltage, high specific energy, good cycle performance, long service life, wide working temperature range, no memory effect, small self-discharge, no pollution, etc.). At present, a graphite-type carbon material is mainly adopted by a commercial lithium ion battery as a negative active material, however, the carbon-type negative material cannot meet the requirements of miniaturization of electronic equipment and high power and high capacity of a lithium ion battery for a vehicle due to the low specific capacity (372 mAh/g) and the safety problem caused by lithium deposition, so that the research and development of a novel negative material which can replace a carbon material and has high energy density, high safety performance and long cycle life is an important factor for breakthrough of the lithium ion battery.
As a novel lithium ion battery cathode material, the silicon monoxide is a hotspot for research on the lithium ion battery cathode material due to high theoretical specific capacity (2400 mAh/g). But the volume expansion phenomenon exists in the charging and discharging process, which can cause active particles to be pulverized, and finally, the capacity is greatly reduced due to the reduction of electric contact among silicon particles and between the particles and a current collector, thereby hindering the commercialization process of the silicon-based lithium ion battery. To solve this problem, a number of exploratory tests have been conducted, including methods of reducing the particle size of silicon particles, preparing silicon thin films, and constructing silicon-based composites. Currently, most researches are made on silicon and graphite composite negative electrode materials, which make full use of the good conductivity and cycling stability of graphite and the high capacity performance of silicon negative electrodes.
Anthracite coal is a new class of carbon material that contains both soft carbon and a small amount of hard carbon. The invention uses anthracite as carbon source to perform graphitization treatment, which is an ideal lithium ion battery cathode material, but the specific capacity is lower.
The anthracite in the composite material can effectively relieve the volume expansion effect of SiO and provide a good conductive network, and because the SiO has higher theoretical specific capacity, the reversible capacity of the material can be greatly improved by introducing a small amount of the SiO into the anthracite carbon material, and the cycle stability of the SiO cathode material applied to a lithium ion battery is remarkably improved.
Disclosure of Invention
The invention provides a composite cathode material taking anthracite, SiO and citric acid as raw materials and a preparation method thereof, which effectively combine the good conductivity of a carbon material and the high lithium storage capacity (2400 mAh/g) of SiO, show excellent electrochemical performance, provide a certain feasible selection for the practicability of the SiO cathode material, and have a certain commercial popularization value.
The technical scheme adopted by the invention is as follows: the anthracite/silicon monoxide/amorphous carbon composite negative electrode material is prepared by selecting high-quality anthracite (the carbon content is more than 97%), purifying, carrying out high-temperature heat treatment, and then mechanically ball-milling and mixing the anthracite, the SiO and the citric acid according to a certain proportion, wherein the particle size of the material is 13-15 microns.
A specific preparation method of an anthracite/silicon monoxide/amorphous carbon composite negative electrode material comprises the following steps:
firstly, mechanically ball-milling anthracite coal with carbon content more than 97%, and controlling the average particle size of anthracite coal particles within 0.1-1 micron by adjusting ball-milling parameters to obtain anthracite micro powder;
and secondly, placing the ball-milled anthracite micro powder into 2 mol/L nitric acid, and stirring and reacting for 3-5 hours to remove metal impurities in the anthracite. After the reaction is finished, filtering and washing until the filtrate is neutral, and then carrying out high-temperature treatment at 2000-3000 ℃ to obtain graphitized anthracite;
thirdly, mechanically milling the obtained graphitized anthracite for 6-8h, adding SiO with the particle size of 0.6-1.1 μm, and continuing milling, wherein the addition amount of the SiO is 5-10% (more preferably 8%) of the mass of the graphitized anthracite, so as to obtain the anthracite and SiO composite material;
and fourthly, adding citric acid accounting for 10-30% of the mass fraction of the anthracite and SiO composite material, continuously ball-milling (preferably 20% further), drying, sintering for 2-6 hours at 800-1000 ℃ in a nitrogen atmosphere (preferably 4 hours at 900 ℃), and sieving the obtained material to obtain the anthracite/silicon monoxide/amorphous carbon composite material.
Compared with the existing carbon cathode material of the lithium ion battery, the anthracite, SiO and citric acid composite cathode material prepared by the invention has the following remarkable characteristics:
1. the prepared anthracite/silicon monoxide/amorphous carbon composite material is uniformly mixed, and the particle size is about 13-15 microns.
2. The anthracite in the composite material can effectively relieve the volume expansion effect of SiO and provide a good conductive network, and the cycle stability of the SiO cathode material applied to the lithium ion battery is obviously improved.
3. The material preparation cost is low, the preparation method is simple to operate, and the environment-friendly effect is achieved.
Drawings
FIG. 1 is an X-ray diffraction pattern of an anthracite/SiO/amorphous carbon composite anode material in example two.
FIG. 2 is a charge-discharge curve and cycle performance curve of the battery prepared from the anthracite/SiO/amorphous carbon composite material in the second example.
FIG. 3 is a graph of rate performance of a battery made of anthracite/SiO/amorphous carbon composite material in example two.
Detailed Description
Comparative example
Mechanically ball-milling anthracite coal with carbon content more than 97%, and controlling the average particle size of anthracite coal particles within 0.5 micron by adjusting ball-milling parameters; placing the ball-milled anthracite micro powder into 2400 ℃ high-temperature heat treatment; cooling and screening, taking 2.0 g of the obtained material, ball-milling for 8 hours by using a planetary ball mill, cooling and screening the material, and mixing with acetylene black and polyvinylidene fluoride (PVdF) according to the weight ratio of 8: 1: 1 in N-methyl pyrrolidone (NMP) medium, coating on copper foil, drying, punching and pressing to obtain working electrode. The metal lithium sheet is a counter electrode, the polypropylene is a diaphragm, the 1M LiPF6 is electrolyte, and a constant current charge and discharge test (0.1A/g) is carried out, wherein the voltage range is 0-3.0V. The first (lithium intercalation) specific capacity is 379 mAh/g, the first charging (lithium deintercalation) specific capacity is 265 mAh/g, the coulombic efficiency is 70%, the charging capacity is 295.9 mAh/g after 100 cycles, and the capacity retention rate is 112%. The method shows that the anthracite coal with the temperature of 2400 ℃ is only used as the cathode material of the lithium ion battery, and the reversible capacity of the anthracite coal is lower.
Example 1
Mechanically ball-milling anthracite coal with the carbon content of more than 97 percent, controlling the average particle size of anthracite coal particles within 0.1-1 micron by adjusting ball-milling parameters to obtain anthracite micro powder, mechanically crushing the anthracite micro powder, chemically removing impurities, treating at the high temperature of 2400 ℃, cooling and screening to obtain graphitized anthracite coal, ball-milling the graphitized anthracite coal and SiO (with the particle size of 0.6-1.1 mu m) accounting for 8 percent of the mass fraction of the graphitized anthracite coal for 8 hours, adding citric acid which accounts for 10 percent of the mass fraction of the graphitized anthracite and SiO composite material, ball-milling for 8 hours, the obtained material is put into a tubular furnace to be sintered for 4 hours at 900 ℃ in nitrogen atmosphere, and then is cooled and screened to obtain the anthracite/silicon monoxide/amorphous carbon composite negative electrode material, and the electrode preparation method, the battery assembly and the test conditions of the obtained product are the same as those of the comparative example. The first lithium intercalation capacity is 1093.0 mAh/g, and the first lithium deintercalation capacity is 432.0 mAh/g; after 100 cycles, the lithium insertion capacity is 416.3 mAh/g, the lithium removal capacity is 406.9 mAh/g, and the capacity retention rate is 97.7%. It is demonstrated that the reversible capacity of the material can be effectively increased by adding a certain amount of SiO.
Example 2
The method comprises the steps of carrying out mechanical ball milling treatment on anthracite coal with the carbon content of more than 97%, controlling the average particle size of anthracite coal particles within 0.1-1 micron by adjusting ball milling parameters to obtain anthracite coal micro powder, carrying out mechanical crushing and chemical impurity removal on the anthracite coal micro powder, carrying out high-temperature treatment at 2400 ℃, cooling and screening to obtain graphitized anthracite coal, carrying out ball milling on the graphitized anthracite coal and SiO (with the particle size of 0.6-1.1 mu m) accounting for 8% of the mass fraction of the graphitized anthracite coal for 8 hours, adding citric acid accounting for 20% of the mass fraction of the graphitized anthracite coal and SiO composite material for ball milling for 8 hours, sintering the obtained material at 900 ℃ for 4 hours in a tubular furnace under the nitrogen atmosphere, cooling and screening to obtain the anthracite/silicon monoxide/amorphous carbon composite negative electrode material. The electrode preparation method, battery assembly and test conditions of the obtained composite negative electrode material were the same as those of the comparative example. The first lithium intercalation capacity is 1297.4 mAh/g, and the first lithium deintercalation capacity is 604.7 mAh/g; after 100 cycles, the lithium insertion capacity is 466.4 mAh/g, the lithium removal capacity is 459.2 mAh/g, and the capacity retention rate is 98.5%. It is shown that by adjusting the amount of citric acid, the reversible capacity of the material can be effectively improved, and the cycle performance can be improved.
Example 3
Mechanically ball-milling anthracite coal with the carbon content of more than 97 percent, controlling the average particle size of anthracite coal particles within 0.1-1 micron by adjusting ball-milling parameters to obtain anthracite micro powder, mechanically crushing the anthracite micro powder, chemically removing impurities, treating at the high temperature of 2400 ℃, cooling and screening to obtain graphitized anthracite coal, ball-milling the graphitized anthracite coal and SiO (with the particle size of 0.6-1.1 mu m) accounting for 8 percent of the mass fraction of the graphitized anthracite coal for 8 hours, adding citric acid accounting for 30 percent of the mass fraction of the graphitized anthracite and SiO composite material, ball-milling for 8 hours, the obtained material is put into a tubular furnace to be sintered for 4 hours at 900 ℃ in nitrogen atmosphere, and then is cooled and sieved to obtain the anthracite/silicon monoxide/amorphous carbon composite negative electrode material, and the electrode preparation method, the battery assembly and the test conditions of the obtained composite negative electrode material are the same as those of the comparative example. The first lithium intercalation capacity is 976.3 mAh/g, and the first lithium deintercalation capacity is 450.1 mAh/g; the lithium insertion capacity is 427.0 mAh/g, the lithium removal capacity is 419.5 mAh/g and the capacity retention rate is 93.2% after 100 cycles. It is shown that when the amount of citric acid is increased to a certain amount, the reversible capacity of the material is rather decreased and the cycle stability is also decreased.
FIG. 1 is an X-ray diffraction pattern of an anthracite/SiO/amorphous carbon composite anode material in example two. As can be seen from the figure, the anthracite coal at 2400 ℃ has an obvious graphite peak, and SiO has no obvious characteristic peak on an X-ray diffraction pattern and is in an amorphous state.
FIG. 2 is a charge-discharge curve and cycle performance curve of the battery prepared from the anthracite/SiO/amorphous carbon composite material in the second example. It can be seen that the capacity of the anthracite, SiO and 20% citric acid composite negative electrode material is not obviously attenuated after 100 times of 0.1A/g circulation.
FIG. 3 is a graph of rate performance of a battery made of anthracite/SiO/amorphous carbon composite material in example two. As can be seen, the anthracite/silicon monoxide/amorphous carbon composite negative electrode material has almost no loss of capacity after being subjected to cycle tests under different currents of 0.1A/g, 0.3A/g, 0.5A/g and 1A/g. After charging and discharging back and forth at 0.1A/g and 1A/g, and then charging and discharging at the current density of 0.1A/g, the capacity can be recovered, and excellent rate performance is shown.

Claims (2)

1. An anthracite/silicon monoxide/amorphous carbon composite negative electrode material is characterized in that: the anthracite/silicon monoxide/amorphous carbon composite negative electrode material is a uniformly dispersed material obtained by mechanically ball-milling anthracite, SiO and citric acid and sintering at high temperature, the particle size of the composite negative electrode material is 13-15 microns, and the preparation method comprises the following steps:
firstly, mechanically ball-milling anthracite coal with carbon content more than 97%, and controlling the average particle size of anthracite coal particles within 0.1-1 micron by adjusting ball-milling parameters to obtain anthracite micro powder;
secondly, performing high-temperature treatment on the ball-milled anthracite micro powder at 2400 ℃ to obtain graphitized anthracite;
thirdly, mechanically ball-milling the obtained graphitized anthracite, adding SiO with the particle size of 0.6-1.1 mu m, and continuing ball milling, wherein the addition amount of the SiO is 5-10% of the mass of the graphitized anthracite, so as to obtain the anthracite and SiO composite material;
and fourthly, adding citric acid accounting for 20 percent of the mass fraction of the anthracite and SiO composite material, continuing ball milling, drying, sintering at 900 ℃ for 2-6 hours in a nitrogen atmosphere, and sieving the obtained material to obtain the anthracite/silicon monoxide/amorphous carbon composite material.
2. The anthracite/SiO/amorphous carbon composite anode material as set forth in claim 1, characterized in that: the ball milling time in the third step is 6-10 hours; in the third step, the addition amount of SiO is 8 percent of the mass of the graphitized anthracite.
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CN110061199B (en) * 2018-01-19 2023-08-01 湖南晋烨高科股份有限公司 Metal-carbon composite anode material and preparation method and application thereof
CN108777292B (en) * 2018-05-23 2021-05-18 三峡大学 Anthracite modified selenium/citric acid composite positive electrode material and preparation method thereof
CN111146418A (en) * 2019-12-24 2020-05-12 中国科学院山西煤炭化学研究所 High-energy-density lithium ion battery cathode material and preparation method thereof
CN114604847A (en) * 2022-02-28 2022-06-10 武汉理工大学 Method for preparing amorphous carbon through heterogeneous atom doping and application
CN117650245A (en) * 2024-01-29 2024-03-05 陕西晶泰新能源科技有限公司 Lithium battery anode material and preparation method and application thereof

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