CN108172779A - SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure - Google Patents
SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure Download PDFInfo
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- CN108172779A CN108172779A CN201711285543.2A CN201711285543A CN108172779A CN 108172779 A CN108172779 A CN 108172779A CN 201711285543 A CN201711285543 A CN 201711285543A CN 108172779 A CN108172779 A CN 108172779A
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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
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- 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
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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
- H01M4/58—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
-
- 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 present invention relates to field of lithium ion battery, particularly disclose a kind of SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure.The SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure, it is characterized in that：Graphite is placed in atmosphere revolving burner；Atmosphere is rotated into stove evacuation, drains stove chamber air；Vent valve is opened, is heated up in the case where protecting gas atmosphere；Silicon source is heated in gasification burner, carrier gas is passed through and brings silicon source gas in atmosphere revolving burner into and react；Cool down after reaction, take out sample, with hydrogen fluoride solution corrosion sample removal impurity, separation of solid and liquid is washed, is dried in vacuo, and sieving obtains Si-C composite material.Si-C composite material prepared by the present invention is functional for negative material, and making is simple, environmentally protective, and can prepare in batches, suitable for industrialized production.
Description
（One）Technical field
The present invention relates to field of lithium ion battery, more particularly to a kind of SiCl4In-situ deposition prepares the silicon-carbon with micro-nano structure
The method of composite material.
（Two）Background technology
Since traditional energy automobile (i.e. fuel vehicle) brings pollution, have multiple countries in recent years and announce the fuel oil that prohibits selling comprehensively in succession
Automobile timetable.New-energy automobile (i.e. electric vehicle) is considered as future automobile development Main way.Wherein, battery is new energy
The primary crucial and core component of source development of automobile, battery performance directly affect the application of new-energy automobile, and electric vehicle needs
Be equipped with high quality, high-performance, high-specific-power battery.Lithium ion battery has that operating voltage is high, small, matter bigger than energy
Amount is light, the features such as having extended cycle life becomes the focus of development of automobile industry competition.This cause develop more high-energy-density and
The lithium ion battery of more preferable cycle performance seems extremely urgent.
2016, China issued power battery energy density hardness index, according to《Energy saving and new-energy automobile technology road
Line chart》, the energy density target of the year two thousand twenty power battery of pure electric automobile is 350Wh/kg.Negative material is as lithium ion battery
One of four big component parts play important function, for negative material in terms of the capacity and cycle performance for improving battery
R＆D work be constantly in popular state, but much remains to be done in terms of the core technologies such as high-capacity battery.
At present, commercialized graphite cathode material theoretical specific capacity only has 372mAh/g, therefore, researchs and develops high power capacity
Lithium cell negative pole material is extremely urgent.Silicon can generate Li with lithium alloyage at normal temperatures15Si4Phase, theoretical specific capacity are up to
4200mAh/g, far above business graphite theoretical specific capacity (372mAh/g), and derive from a wealth of sources, be of low cost, environment it is friendly
It is good, scientific research personnel's concern is received always, becomes one of most potential next-generation lithium ion battery negative material.However,
Silicon, there are serious volume expansion (~ 300%), causes active material dusting, is in electrical contact between collector in charge and discharge process
Deteriorate, and then initiation capacity attenuation is very fast, conductivity reduces, and larger ohmic polarization and electrochemistry occurs in high current charge-discharge
Polarization limits the commercial applications of silicium cathode material.
（Three）Invention content
In order to compensate for the shortcomings of the prior art, the present invention provides it is a kind of effectively inhibit silicon in charge and discharge process volume change,
Improve the SiCl of reversible capacity and cycle performance4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure.
The present invention is achieved through the following technical solutions：
A kind of SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure, includes the following steps：
（1）Graphite is placed in atmosphere revolving burner；
（2）Vacuum valve is closed after atmosphere revolving burner is evacuated to -0.1MPa, protection gas is passed through and furnace chamber is inflated, make vacuum degree
0 is dropped to, vacuum valve is closed, in triplicate, drains stove chamber air；
（3）Vent valve is opened, adjust protection air-flow amount and keeps stable, 500-1000 DEG C is warming up in the case where protecting gas atmosphere；
（4）Silicon source is heated in gasification burner, carrier gas is passed through and brings silicon source gas in atmosphere revolving burner into, reacts 1-6h, until
The silicon of graphite surface depositing dosed quantities；
（5）Stop continuing to be passed through protection gas after leading to carrier gas and silicon source gas into atmosphere revolving burner, treat that atmosphere revolving burner is cooled to
100 DEG C hereinafter, take out sample, with hydrogen fluoride solution corrosion sample removal impurity, separation of solid and liquid, and are washed with distilled water to
Property, it is dried in vacuo, sieving obtains Si-C composite material.
The present invention is attempted by a large amount of, and using Composite technology, Si-C composite material is made by vapour deposition process, will
Nano-silicon is coated on graphite surface, to inhibit volume expansion of the silicon in charge and discharge process, meanwhile, " cushioning frame " is utilized to compensate
Material expand improves reversible capacity and cycle performance, realizes the multiple elements design of silicon and carbon.
The present invention more excellent technical solution be：
Step（1）In, graphite is Delanium, native graphite, blocky graphite or the crystalline flake graphite of 10 μm -80 μm of grain size；It is preferred that
The Delanium that 30 μm -60 μm of grain size.
Step（2）In, protection gas is argon gas, one or more in helium, neon.
Step（3）In, it is heated up in the case where protecting gas atmosphere with the rate of 5 DEG C/min.
Step（4）In, the temperature of gasification burner is 60-80 DEG C, and carrier gas is hydrogen and the gaseous mixture of protection gas, wherein hydrogen
Product content is 2%；Silicon source gas is more than 90% SiCl for purity4Gas, preferably purity are 99.9%；Bring atmosphere revolving burner into
Airflow rate is 1-10L/min.
Step（5）In, a concentration of 5wt% of hydrogen fluoride solution, the mass ratio of sample and hydrogen fluoride solution is 1：50, fluorination
The etching time of hydrogen solution is 1h.
Si-C composite material prepared by the present invention is functional for negative material, and making is simple, environmentally protective, and can
Prepared by batch, suitable for industrialized production.
（Four）Specific embodiment
Of the invention for ease of understanding, the present invention enumerates embodiment to further illustrate the present invention.Those skilled in the art it should be appreciated that
The embodiment is only to assist understanding the present invention, but be not limited to specific embodiment.
Embodiment 1：
（1）1000g average grain diameters are placed in for 50 μm of graphite in rotation atmosphere furnace；
（2）Rotation atmosphere furnace is warming up to 600 DEG C under Ar protections；
（3）Gasification burner is warming up to 60 DEG C, makes SiCl4Vaporization closes Ar, is passed through carrier gas (H2/ Ar gaseous mixtures) control gas stream
It measures as 5L/min, is continually fed into 1h；
（4）Carrier gas is closed, is passed through protection gas Ar, treats that atmosphere revolving burner is cooled to 100 DEG C hereinafter, sample is taken out, with the HF of 5wt%
Corrode 1h, separation of solid and liquid, and be washed with distilled water to neutrality, be dried in vacuo, sieving separating obtains silicon-carbon cathode material；
（5）The silicon-carbon cathode material of gained is made into CR2032 button cells, pole piece formula presses major ingredient:SP:CMC:SBR=80:
10:5:5, electrolyte is 1mol/L LiPF6, diaphragm is PP films, and button cell is made by anode of lithium piece.
Silicon-carbon cathode material performance is studied using blue electrical testing cabinet, Si-C composite material specific capacity is reachable
683mAh/g, for the first time coulombic efficiency recycle 100 specific capacity conservation rates 97.6% up to 89.3%.
Embodiment 2：
（1）1000g average grain diameters are placed in for 50 μm of graphite in rotation atmosphere furnace；
（2）Rotation atmosphere furnace is warming up to 600 DEG C under Ar protections；
（3）Gasification burner is warming up to 60 DEG C, makes SiCl4Vaporization closes Ar, is passed through carrier gas (H2/ Ar gaseous mixtures) control gas
Flow is 5L/min, is continually fed into 2h；
（4）Carrier gas is closed, is passed through protection gas Ar, treats that atmosphere revolving burner is cooled to 100 DEG C hereinafter, sample is taken out, with the HF of 5wt%
Corrode 1h, separation of solid and liquid, and be washed with distilled water to neutrality, be dried in vacuo, sieving separating obtains silicon-carbon cathode material；
（5）The silicon-carbon cathode material of gained is made into CR2032 button cells, pole piece formula presses major ingredient:SP:CMC:SBR=80:
10:5:5, electrolyte is 1mol/L LiPF6, diaphragm is PP films, and button cell is made by anode of lithium piece.
Silicon-carbon cathode material performance is studied using blue electrical testing cabinet, Si-C composite material specific capacity is reachable
735mAh/g, for the first time coulombic efficiency recycle 100 specific capacity conservation rates 94.7% up to 86.4%.
Embodiment 3：
（1）1000g average grain diameters are placed in for 50 μm of graphite in rotation atmosphere furnace；
（2）Rotation atmosphere furnace is warming up to 600 DEG C under Ar protections；
（3）Gasification burner is warming up to 60 DEG C, makes SiCl4Vaporization closes Ar, is passed through carrier gas (H2/ Ar gaseous mixtures) control gas
Flow is 5L/min, is continually fed into 3h；
（4）Carrier gas is closed, is passed through protection gas Ar, treats that atmosphere revolving burner is cooled to 100 DEG C hereinafter, sample is taken out, with the HF of 5wt%
Corrode 1h, separation of solid and liquid, and be washed with distilled water to neutrality, be dried in vacuo, sieving separating obtains silicon-carbon cathode material；
（5）The silicon-carbon cathode material of gained is made into CR2032 button cells, pole piece formula presses major ingredient:SP:CMC:SBR=80:
10:5:5, electrolyte is 1mol/L LiPF6, diaphragm is PP films, and button cell is made by anode of lithium piece.
Silicon-carbon cathode material performance is studied using blue electrical testing cabinet, Si-C composite material specific capacity is reachable
792mAh/g, for the first time coulombic efficiency recycle 100 specific capacity conservation rates 93.6% up to 84.1%.
Embodiment 4：
（1）1000g average grain diameters are placed in for 50 μm of graphite in rotation atmosphere furnace；
（2）Rotation atmosphere furnace is warming up to 600 DEG C under Ar protections；
（3）Gasification burner is warming up to 60 DEG C, makes SiCl4Vaporization closes Ar, is passed through carrier gas (H2/ Ar gaseous mixtures) control gas
Flow is 5L/min, is continually fed into 3h；
（4）Carrier gas is closed, is passed through protection gas Ar, treats that atmosphere revolving burner is cooled to 100 DEG C hereinafter, sample is taken out, with the HF of 5wt%
Corrode 1h, separation of solid and liquid, and be washed with distilled water to neutrality, be dried in vacuo, sieving separating obtains silicon-carbon cathode material；
（5）The silicon-carbon cathode material of gained is made into CR2032 button cells, pole piece formula presses major ingredient:SP:CMC:SBR=80:
10:5:5, electrolyte is 1mol/L LiPF6, diaphragm is PP films, and button cell is made by anode of lithium piece.
Silicon-carbon cathode material performance is studied using blue electrical testing cabinet, Si-C composite material specific capacity is reachable
853mAh/g, for the first time coulombic efficiency recycle 100 specific capacity conservation rates 91.5% up to 81.9%.
Claims (8)
1. a kind of SiCl4The method that in-situ deposition prepares the Si-C composite material with micro-nano structure, it is characterized in that, including as follows
Step：（1）Graphite is placed in atmosphere revolving burner；（2）Vacuum valve is closed after atmosphere revolving burner is evacuated to -0.1MPa, is led to
Enter to protect gas to be inflated to furnace chamber, vacuum degree is made to drop to 0, close vacuum valve, in triplicate, drain stove chamber air；（3）It opens
Vent valve adjusts protection air-flow amount and keeps stable, 500-1000 DEG C is warming up in the case where protecting gas atmosphere；（4）In gasification burner
Silicon source is heated, carrier gas is passed through and brings silicon source gas in atmosphere revolving burner into, reacts 1-6h, until graphite surface deposition has silicon；
（5）Stop continuing to be passed through protection gas after leading to carrier gas and silicon source gas into atmosphere revolving burner, treat that atmosphere revolving burner is cooled to 100 DEG C
Hereinafter, taking out sample, impurity, separation of solid and liquid are removed, and be washed with distilled water to neutrality with hydrogen fluoride solution corrosion sample, vacuum
Dry, sieving obtains Si-C composite material.
2. SiCl according to claim 14The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：Step（1）In, graphite is Delanium, native graphite, blocky graphite or the crystalline flake graphite of 10 μm -80 μm of grain size.
3. SiCl according to claim 14The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：Step（2）In, protection gas is argon gas, one or more in helium, neon.
4. SiCl according to claim 14The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：Step（3）In, it is heated up in the case where protecting gas atmosphere with the rate of 5 DEG C/min.
5. SiCl according to claim 14The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：Step（4）In, the temperature of gasification burner is 60-80 DEG C, and carrier gas is hydrogen and the gaseous mixture of protection gas, wherein hydrogen
Volume content is 2%；Silicon source gas is more than 90% SiCl for purity4Gas, the airflow rate for bringing atmosphere revolving burner into are 1-
10L/min。
6. SiCl according to claim 14The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：Step（5）In, a concentration of 5wt% of hydrogen fluoride solution, the mass ratio of sample and hydrogen fluoride solution is 1：50, fluorination
The etching time of hydrogen solution is 1h.
7. SiCl according to claim 24The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：The graphite is the Delanium of 30 μm -60 μm of grain size.
8. SiCl according to claim 54The method that in-situ deposition prepares the Si-C composite material with micro-nano structure,
It is characterized in that：The SiCl4The purity of gas is 99.9%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028067A (en) * | 2020-09-02 | 2020-12-04 | 南京同宁新材料研究院有限公司 | Silicon-carbon negative electrode material and preparation method thereof |
| CN114050251A (en) * | 2021-11-18 | 2022-02-15 | 兰州城市学院 | Preparation and application of silicon-carbon composite micro-nano structure material |
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| CN105185970A (en) * | 2015-08-13 | 2015-12-23 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon-coated carbon particle composite material and preparation method and equipment and application |
| TW201739088A (en) * | 2015-04-12 | 2017-11-01 | 加利福尼亞鋰電池股份有限公司 | Apparatus and process for semi-continuous and multi-step composite production |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080261116A1 (en) * | 2007-04-23 | 2008-10-23 | Burton David J | Method of depositing silicon on carbon materials and forming an anode for use in lithium ion batteries |
| CN104577084A (en) * | 2015-01-20 | 2015-04-29 | 深圳市贝特瑞新能源材料股份有限公司 | Nano silicon composite negative electrode material for lithium ion battery, preparation method and lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028067A (en) * | 2020-09-02 | 2020-12-04 | 南京同宁新材料研究院有限公司 | Silicon-carbon negative electrode material and preparation method thereof |
| CN114050251A (en) * | 2021-11-18 | 2022-02-15 | 兰州城市学院 | Preparation and application of silicon-carbon composite micro-nano structure material |
| CN114050251B (en) * | 2021-11-18 | 2024-01-19 | 兰州城市学院 | Preparation and application of silicon-carbon composite micro-nano structure material |
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