CN103730644B - Silicon-silicon oxide-carbon composite negative pole material of lithium ion battery preparation method - Google Patents
Silicon-silicon oxide-carbon composite negative pole material of lithium ion battery preparation method Download PDFInfo
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- CN103730644B CN103730644B CN201310683767.4A CN201310683767A CN103730644B CN 103730644 B CN103730644 B CN 103730644B CN 201310683767 A CN201310683767 A CN 201310683767A CN 103730644 B CN103730644 B CN 103730644B
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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
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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
- 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
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- 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 invention discloses a kind of preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery, mix with pitch after Si oxide, silicon and graphite ball milling being mixed, high-temperature heat treatment i.e. obtained silicon-silicon oxide-carbon composite negative pole material of lithium ion battery again.The present invention adds silicon in Si oxide-material with carbon element, can improve reversible capacity and the coulombic efficiency first of material, makes silicon oxide composite material have high power capacity, the better excellent properties such as cycle performance and higher coulombic efficiency first concurrently.This method has that cost is low, equipment is simple, process conditions are simple and easy to control, productive rate advantages of higher, is very suitable for large-scale industrial and produces.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material preparation method, particularly a kind of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery preparation method.
Background technology
Si oxide (SiO
x, 0 < x≤2) and lithia (Li owing to being formed in first electrochemistry charge/discharge process
2and lithium metasilicate (Li O)
4siO
4) bulk effect of nano-silicon active material can be cushioned preferably, thus there is high specific capacity and excellent cycle performance, become the negative material of lithium electricity business circles hot research in recent years.But, Si oxide is still difficult to practical at present, because consume lithium in first electrochemistry charge/discharge process to generate irreversible lithia and lithium metasilicate, causes irreversible capacity first large, coulombic efficiency is less than 60% first, and coulombic efficiency increases along with oxygen content and reduces first.In order to solve the silicon oxide material problem that coulombic efficiency is low first, people have carried out a large amount of explorations, prepare the composite material of Si oxide mainly through methods such as the coated and metallic reducings of carbon.
In the patent of CN101752547B, once disclose one prepare Si-SiO
2-C material preparation method.This method for raw material, has prepared the nucleocapsid structure carbon coated Si oxide material of higher cycle performance and specific capacity with silicon monoxide (SiO), graphite and pitch.But the coulombic efficiency first of this material only has about 70%, cannot reach business-like requirement.
A kind of lithium ion battery silicon oxide/carbon negative material and preparation method thereof is disclosed in the patent of CN103022446A.This 3-layer composite material take graphite as kernel, and the porous silicon oxide of the active metal partial reductions such as lithium is intermediate layer, and organic RESEARCH OF PYROCARBON is outermost coating layer, has good cycle performance and specific capacity, and coulombic efficiency also can reach 88% first.But this complex process, cost is high, and three-layer composite structure is restive, heavy industrialization difficulty.
SiO is disclosed in the patent of CN102593426A
x/ C composite and preparation method thereof.This method containing the silicon dioxide microsphere of nano-silicon by sol-gel process synthesis, then is mixed coated rear carbonization and obtains composite material with cold primer-oil.This method can effectively extend silicon-carbon cathode material the rate of decay, improve silicon-carbon cathode material cycle performance, improve the cycle efficieny first of silicon-carbon cathode material.But this method complex process, cost is high, and sol-gel process preparation process controls difficulty, and industrial operability is poor.
Summary of the invention
Technical problem to be solved by this invention is, provides that a kind of capacity is high, good cycle and coulombic efficiency is higher first low cost, is applicable to the silicon-silicon oxide-carbon composite negative pole material of lithium ion battery preparation method of large-scale production.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery, comprises the following steps:
1) under argon gas atmosphere protection, Si oxide, silicon and graphite mix through mechanical ball milling, obtain mixed once material, then mix with pitch and organic solvent, obtain secondary composite material after dry process;
2) by above-mentioned secondary composite material high-temperature heat treatment under inert gas shielding, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
Described Si oxide is the one in silicon monoxide and silicon dioxide.
The weight ratio of described Si oxide, silicon and graphite is 1:0.01 ~ 10:0.5 ~ 50.
Described pitch is the one of petroleum asphalt, coal tar pitch and bitumen.
Described organic solvent is the one in acetone, ethanol, isopropyl alcohol, oxolane, cyclohexane, benzinum, toluene and solvent naphtha, and the weight ratio of mixed once material and organic solvent is 1:1 ~ 200.
The weight ratio of described mixed once material and pitch is 1:0.1 ~ 10.
The inert protective gas of described high-temperature heat treatment is the gaseous mixture of argon gas, nitrogen, hydrogen and argon gas.
Described high-temperature heat treatment temperature is 500 ~ 1100 DEG C; The high-temperature heat treatment time is 0.5 ~ 20h.
The invention has the beneficial effects as follows: device therefor is simple, be easy to operation, process conditions are simple and easy to control, are suitable for large-scale production; The silicon-silicon oxide-carbon composite negative pole material of lithium ion battery that the present invention obtains not only capacity is high, and have extended cycle life, simultaneously due to the interpolation of silicon, effectively can improve reversible specific capacity and the coulombic efficiency first of Si oxide-material with carbon element, meet the requirement of practical application.
Accompanying drawing explanation
X-ray diffraction (XRD) spectrogram of Fig. 1 material prepared by the embodiment of the present invention 1.
Surface sweeping Electronic Speculum (SEM) photo of Fig. 2 material prepared by the embodiment of the present invention 1.
The electrochemistry cyclic curve of Fig. 3 material prepared by the embodiment of the present invention 1 and coulombic efficiency curve.
Embodiment
The preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery of the present invention, comprises the steps:
Be that the Si oxide of 1:0.01 ~ 10:0.5 ~ 50, silicon and graphite are mixed by mechanical ball milling by weight ratio, obtain mixed once material.Mix with the pitch of 0.1 ~ 10 times of weight and the organic solvent of 1 ~ 200 times of weight, dry process, obtains secondary composite material again.By secondary composite material in inert protective atmosphere, 500 ~ 1100 DEG C of high-temperature process 0.5 ~ 20h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
In ball milling blend step described in said method, Si oxide is the one in silicon monoxide or silicon dioxide; In described secondary blend step, pitch is the one of petroleum asphalt, coal tar pitch or bitumen, and organic solvent is acetone, ethanol, isopropyl alcohol, oxolane, cyclohexane, benzinum, toluene, solvent naphtha; In described high temperature processing step, inert protective gas is argon gas, nitrogen or hydrogen-argon-mixed.
The mechanical ball milling that is mixed into of Si oxide of the present invention, silicon and graphite mixes, and object makes three kinds of raw materials reach nanoscale particle diameter and Homogeneous phase mixing, improves the conductivity of material and alleviates the bulk effect of silicon active material.Described pitch mixes with the liquid phase of mixed once material, object be realize pitch can clad nano yardstick mixture on a molecular scale.Described high-temperature process, object is the pitch pyrolysis carbonization in pyroprocess introducing in compound, carries out effective carbon coated, and then improve the chemical property of material to nanoscale mixture surface.
Below by specific embodiment, the present invention is described in further detail, but is not limited to protection scope of the present invention.
Embodiment 1
Under argon gas atmosphere protection, be the mixing of the silicon monoxide of 1:0.05:1, silicon and graphite machinery ball milling by weight ratio, obtain mixed once material.Mix with the petroleum asphalt of 2 times of weight and the oxolane of 10 times of weight, be uniformly mixed, dry process obtains secondary composite material.By secondary composite material in hydrogen 5%(volume ratio) hydrogen and argon gas mixed atmosphere in, 800 DEG C process 4h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
Fig. 1 is X-ray diffraction (XRD) spectrogram of the silicon-Si oxide-carbon compound cathode materials of above-mentioned preparation.As can be seen from this figure, diffraction maximum more sharp-pointed in figure is the diffraction maximum of graphite and elemental silicon, and the broad peak between 20 ~ 30 ° belongs to Si oxide.Fig. 2 is ESEM (SEM) photo of prepared silicon carbon material, can find out that sample is random micron particles.
With the silicon-silicon oxide-carbon composite negative pole material of lithium ion battery of above-mentioned preparation for active electrode material, test its cycle performance in 2032 type button cells.Electrode material consists of: active material: conductive agent: the weight ratio of PVdF is 8:1:1; Be lithium metal to electrode; Electrolyte is 1mol/LLiPF
6eC/DMC (volume ratio is 1:1) solution; Barrier film is Cellgard2400 micro-pore septum.Fig. 3 is electrochemistry cyclic curve when current density is 100mA/g of the silicon-silicon oxide-carbon composite negative pole material of lithium ion battery electrode of above-mentioned preparation and coulombic efficiency curve.Testing result is as can be seen from this figure: discharge capacity is 1012.2mAh/g first, and initial charge capacity is 822.7mAh/g, and namely coulombic efficiency is 81.2% first, and after circulating 50 weeks, capability retention is 86.1%.This result shows, silicon-silicon oxide-carbon composite negative pole material of lithium ion battery has higher capacity, preferably cyclical stability and higher coulombic efficiency first.
Embodiment 2
Under argon gas atmosphere protection, be the mixing of the silicon monoxide of 1:0.5:10, silicon and graphite machinery ball milling by weight ratio, obtained mixed once material.Mix with the coal tar pitch of 3 times of weight and the cyclohexane of 60 times of weight, ultrasonic disperse, dry process obtains secondary composite material again.By secondary composite material in argon gas atmosphere, 900 DEG C of process 2h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
According to the battery condition of embodiment 1, test the cycle performance of made silicon-Si oxide-carbon compound cathode materials in 2032 type button cells.Testing result is: this electrode first discharge capacity is 605.7mAh/g, and coulombic efficiency is 78.5% first, and after circulating 50 weeks, capability retention is 96.3%.
Embodiment 3
Under argon gas atmosphere protection, be the mixing of the silicon monoxide of 1:1:3, silicon and graphite machinery ball milling by weight ratio, obtained mixed once material.Mix with the petroleum asphalt of 0.5 times of weight and the ethanol wet ball grinding of 5 times of weight, dry process obtains secondary composite material again.By secondary composite material in argon gas atmosphere, 900 DEG C of process 1h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
According to the battery condition of embodiment 1, test the cycle performance of made silicon-Si oxide-carbon compound cathode materials in 2032 type button cells.Testing result is: this electrode first discharge capacity is 1297mAh/g, and coulombic efficiency is 84.3% first, and after circulating 50 weeks, capability retention is 71.6%.
Embodiment 4
Under argon gas atmosphere protection, be the mixing of the silicon monoxide of 1:5:30, silicon and graphite machinery ball milling by weight ratio, obtained mixed once material.Mix with the bitumen of 1 times of weight and the acetone wet ball grinding of 10 times of weight, dry process obtains secondary composite material again.By secondary composite material in nitrogen atmosphere, 600 DEG C of process 15h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
According to the battery condition of embodiment 1, test the cycle performance of made silicon-Si oxide-carbon compound cathode materials in 2032 type button cells.Testing result is: this electrode first discharge capacity is 833.8mAh/g, and coulombic efficiency is 83.1% first, and after circulating 50 weeks, capability retention is 73.4%.
Embodiment 5
Under argon gas atmosphere protection, be the mixing of the silicon dioxide of 1:7:10, silicon and graphite machinery ball milling by weight ratio, after obtained mixed once material.Again with the petroleum asphalt of 8 times of weight and the oxolane of 120 times of weight, be uniformly mixed, dry process obtains secondary composite material.By secondary composite material in the hydrogen of hydrogen 10% and the hybrid protection atmosphere of argon gas, after 1000 DEG C of process 10h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
According to the battery condition of embodiment 1, test the cycle performance of made silicon-Si oxide-carbon compound cathode materials in 2032 type button cells.Testing result is: this electrode first discharge capacity is 1023.4mAh/g, and coulombic efficiency is 80.3% first, and after circulating 50 weeks, capability retention is 80.5%.
Comparative example
Under argon gas atmosphere protection, be silicon monoxide and the mixing of graphite machinery ball milling of 1:1 by weight ratio, obtain mixed once material.Mix with the petroleum asphalt of 2 times of weight and the oxolane of 10 times of weight, be uniformly mixed, dry process obtains secondary composite material.By secondary composite material in the hydrogen of hydrogen 5% and the hybrid protection atmosphere of argon gas, 800 DEG C of process 4h, lower the temperature and obtain silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
According to the battery condition of embodiment 1, test the cycle performance of made Si oxide-carbon negative pole material in 2032 type button cells.Testing result is: this electrode first discharge capacity is 966.3mAh/g, and coulombic efficiency is 74.3% first, and after circulating 50 weeks, capability retention is 85.0%.
In sum, content of the present invention is not limited in the above-described embodiment, and the knowledgeable people in same area can propose other embodiment easily within technological guidance's thought of the present invention, but this embodiment all comprises within the scope of the present invention.
Claims (5)
1. a preparation method for silicon-silicon oxide-carbon composite negative pole material of lithium ion battery, is characterized in that, comprises the following steps:
1) under argon gas atmosphere protection, Si oxide, silicon and graphite mix through mechanical ball milling, obtain mixed once material, then mix with pitch and organic solvent, obtain secondary composite material after dry process; The weight ratio of described Si oxide, silicon and graphite is 1:0.01 ~ 10:0.5 ~ 50, and the weight ratio of described mixed once material and pitch is 1:0.1 ~ 10;
2) by above-mentioned secondary composite material under inert gas shielding, at 500 ~ 1100 DEG C, high-temperature heat treatment 0.5 ~ 20h, lowers the temperature and obtains silicon-silicon oxide-carbon composite negative pole material of lithium ion battery.
2. the preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery according to claim 1, is characterized in that, described Si oxide is the one in silicon monoxide and silicon dioxide.
3. the preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery according to claim 1, it is characterized in that, described pitch is the one of petroleum asphalt, coal tar pitch and bitumen.
4. the preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery according to claim 1, it is characterized in that, described organic solvent is the one in acetone, ethanol, isopropyl alcohol, oxolane, cyclohexane, benzinum, toluene and solvent naphtha, and the weight ratio of mixed once material and organic solvent is 1:1 ~ 200.
5. the preparation method of silicon-silicon oxide-carbon composite negative pole material of lithium ion battery according to claim 1, it is characterized in that, the inert protective gas of described high-temperature heat treatment is the gaseous mixture of argon gas, nitrogen, hydrogen and argon gas.
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| CN104577066B (en) * | 2014-12-29 | 2017-02-22 | 南开大学 | Silicon oxide composite negative pole material for lithium ion secondary battery and preparation method thereof |
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| CN112133898B (en) * | 2020-09-21 | 2022-04-19 | 陕西煤业化工技术研究院有限责任公司 | Silicon-based negative electrode material and preparation method thereof |
| CN112142060B (en) * | 2020-09-21 | 2022-04-19 | 陕西煤业化工技术研究院有限责任公司 | Coal-based silicon-carbon composite negative electrode material and preparation method thereof |
| CN114497469B (en) * | 2020-11-11 | 2023-12-22 | 成都爱敏特新能源技术有限公司 | Silicon monoxide-cobalt fluoride-graphene composite negative electrode material and preparation method thereof |
| CN112467112A (en) * | 2020-12-01 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium ion battery negative electrode material |
| CN113380992A (en) * | 2021-04-07 | 2021-09-10 | 万向一二三股份公司 | Silicon monoxide/graphite composite material and preparation method and application thereof |
| CN113745483B (en) * | 2021-09-07 | 2023-04-07 | 宁波特粒科技有限公司 | Hollow silicon-carbon-based composite material, preparation method thereof and negative electrode energy storage material for non-aqueous electrolyte secondary battery |
| CN113903892A (en) * | 2021-09-13 | 2022-01-07 | 惠州市贝特瑞新材料科技有限公司 | Silicon monoxide composite negative electrode material and preparation method thereof |
| CN114105133B (en) * | 2021-10-19 | 2023-09-05 | 湖南金硅科技有限公司 | Graphite-silicon/silicon oxide-carbon composite material and preparation method and application thereof |
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