CN108807868A - A method of preparing graphene coated silicon-carbon composite cathode material - Google Patents
A method of preparing graphene coated silicon-carbon composite cathode material Download PDFInfo
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- CN108807868A CN108807868A CN201810378738.XA CN201810378738A CN108807868A CN 108807868 A CN108807868 A CN 108807868A CN 201810378738 A CN201810378738 A CN 201810378738A CN 108807868 A CN108807868 A CN 108807868A
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 present invention discloses a kind of method preparing graphene coated silicon-carbon composite cathode material, includes following steps：（1）The preparation of nano Si particle：Pre- logical Ar/H2 gas 15-25 min, gas flow rate 0.1-2 L/min；Si particles are commercialized in 8-12g to be sent into grinding pot by feed inlet, 150-190 mL acetone is injected into grinding pot by feed inlet, feed inlet is sealed with rubber plug, screws buckle closure；It sets rotating speed to 2200-2700rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2h respectively；The sample of recycling is placed in vacuum drying chamber, temperature setting is 70-80 DEG C of vacuum drying；（2）Mechanical mixing.Present invention application high speed grinding method, is prepared for binary composite nano Si-graphene complex, and the specific capacity for effectively improving Si sills and the cycle performance under low current density meet the needs used.
Description
Technical field
The present invention relates to negative material field technology, refer in particular to a kind of preparing graphene coated silicon-carbon composite cathode material
Method.
Background technology
Graphene is a kind of two dimension (2D) cellular network with monoatomic thickness combined by Sp2 carbon hydridization,
Monoatomic thickness belongs to nano-scale range.Since 1987 introduce " graphene " term, this material is due to having
Unique physicochemical characteristics and in chemistry, physics, the generality applied in biology and engineering science and attract
Too many concern.In the surprising special nature of graphene, the charge of high conductivity, high mechanical stability, high-speed moves
Dynamic and high-specific surface area graphene extremely suitable to be applied as the negative material of lithium ion battery.
However, there are conductivity is relatively low and put larger intrinsic scarce of volume change in charging process for current silica-base material
It falls into, the needs used cannot be met.
Invention content
In view of this, preparing graphene in view of the deficiencies of the prior art, the present invention aims to provide a kind of
The method for coating silicon-carbon composite cathode material, capable of effectively solving existing silica-base material, there are conductivity is relatively low and put and charged
The larger problem of volume change in journey.
To achieve the above object, the present invention is using following technical solution：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical Ar/H2 gas 15-25 min, gas flow rate 0.1-2 L/min；By 8-12g quotient
Product Si particles are sent by feed inlet in grinding pot, are injected 150-190 mL acetone into grinding pot by feed inlet, are used rubber plug
Feed inlet is sealed, buckle closure is screwed；It sets rotating speed to 2200-2700rpm, starts to grind, respectively in 0.5 h, 1 h, 1.5 h
Sample is collected with 2 h；The sample of recycling is placed in vacuum drying chamber, temperature setting is 70-80 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 1.5-2.5h, it is ultrasonically treated 1.5-2.5h, vacuum filtration is then empty dry under 70-90 DEG C of condition vacuum condition
Dry 10-20 h, obtained black powder are graphene coated silicon-carbon composite cathode material.
As a preferred embodiment, include following steps：
（1）The preparation of nano Si particle：Pre- logical 20 min of Ar/H2 gas, 0.1 L/min of gas flow rate；10g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 170 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2500rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2 h respectively；
The sample of recycling is placed in vacuum drying chamber, temperature setting is 75 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2h, it is ultrasonically treated 2h, vacuum filtration, then empty dry 15 h under 80 DEG C of condition vacuum conditions, obtained
Black powder is graphene coated silicon-carbon composite cathode material.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal
Known to：
Present invention application high speed grinding method, is prepared for binary composite nano Si-graphene complex, effectively improves Si base materials
The specific capacity of material and the cycle performance under low current density, meet the needs used.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of graphene coated silicon-carbon composite cathode material in the present invention.
Specific implementation mode
Present invention is disclosed a kind of methods preparing graphene coated silicon-carbon composite cathode material, include following steps：
（1）The preparation of nano Si particle：Pre- logical Ar/H2 gas 15-25 min, gas flow rate 0.1-2 L/min；By 8-12g quotient
Product Si particles are sent by feed inlet in grinding pot, are injected 150-190 mL acetone into grinding pot by feed inlet, are used rubber plug
Feed inlet is sealed, buckle closure is screwed；It sets rotating speed to 2200-2700rpm, starts to grind, respectively in 0.5 h, 1 h, 1.5 h
Sample is collected with 2 h；The sample of recycling is placed in vacuum drying chamber, temperature setting is 70-80 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 1.5-2.5h, it is ultrasonically treated 1.5-2.5h, vacuum filtration is then empty dry under 70-90 DEG C of condition vacuum condition
Dry 10-20h, obtained black powder are graphene coated silicon-carbon composite cathode material.
With multiple embodiments, invention is further described in detail below：
Embodiment 1：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 20 min of Ar/H2 gas, 0.1 L/min of gas flow rate；10g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 170 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2500rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2 h respectively；
The sample of recycling is placed in vacuum drying chamber, temperature setting is 75 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2h, it is ultrasonically treated 2h, vacuum filtration, then empty dry 15 h under 80 DEG C of condition vacuum conditions, obtained
Black powder is graphene coated silicon-carbon composite cathode material.
As shown in Figure 1, for the scanning electron microscope (SEM) photograph of graphene coated silicon-carbon composite cathode material in the present embodiment.It can by Fig. 1
Know, material surface has a small amount of graphene coated in material surface.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
672mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 613mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
Embodiment 2：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 15 min of Ar/H2 gas, 0.5 L/min of gas flow rate；8g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 160 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2200-2700rpm, starts to grind, collected respectively in 0.5 h, 1 h, 1.5 h and 2 h
Sample；The sample of recycling is placed in vacuum drying chamber, temperature setting is 75 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 1.5h, it is ultrasonically treated 2h, vacuum filtration, then the empty dry 12h under 80 DEG C of condition vacuum conditions, acquired
Black powder be graphene coated silicon-carbon composite cathode material.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
651mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 601mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
Embodiment 3：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 18 min of Ar/H2 gas, gas flow rate 1L/min；By 9g be commercialized Si particles by
Feed inlet is sent into grinding pot, is injected 150 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug, screw
Buckle closure；It sets rotating speed to 2200-2700rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2 h respectively；
The sample of recycling is placed in vacuum drying chamber, temperature setting is 70 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2h, it is ultrasonically treated 1.8h, vacuum filtration, then the empty dry 10h under 70 DEG C of condition vacuum conditions, acquired
Black powder be graphene coated silicon-carbon composite cathode material.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
645mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 605mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
Embodiment 4：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 22 min of Ar/H2 gas, 1.2 L/min of gas flow rate；10g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 190 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2200-2700rpm, starts to grind, collected respectively in 0.5 h, 1 h, 1.5 h and 2 h
Sample；The sample of recycling is placed in vacuum drying chamber, temperature setting is 80 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2.2h, it is ultrasonically treated 2.5h, is filtered by vacuum, then empty dry 15h, gained under 75 DEG C of condition vacuum conditions
To black powder be graphene coated silicon-carbon composite cathode material.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
661mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 599mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
Embodiment 5：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 25 min of Ar/H2 gas, 2 L/min of gas flow rate；Si particles are commercialized in 11g
It is sent into grinding pot by feed inlet, injects 180 mL acetone into grinding pot by feed inlet, sealed feed inlet with rubber plug, revolved
Link closely lid；It sets rotating speed to 2200-2700rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2 h respectively
Product；The sample of recycling is placed in vacuum drying chamber, temperature setting is 72 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 1.8h, it is ultrasonically treated 1.5h, is filtered by vacuum, then empty dry 20h, gained under 88 DEG C of condition vacuum conditions
To black powder be graphene coated silicon-carbon composite cathode material.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
648mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 590mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
Embodiment 6：
A method of graphene coated silicon-carbon composite cathode material is prepared, includes following steps：
（1）The preparation of nano Si particle：Pre- logical 24 min of Ar/H2 gas, 1.8 L/min of gas flow rate；12g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 170 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2200-2700rpm, starts to grind, collected respectively in 0.5 h, 1 h, 1.5 h and 2 h
Sample；The sample of recycling is placed in vacuum drying chamber, temperature setting is 78 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2.4h, it is ultrasonically treated 2.3h, is filtered by vacuum, then empty dry 18h, gained under 90 DEG C of condition vacuum conditions
To black powder be graphene coated silicon-carbon composite cathode material.
After tested, the initial charge specific capacity of the graphene coated silicon-carbon composite cathode material obtained in the present embodiment is
652mAh/g, hence it is evident that after cycle 40 times, charge specific capacity 605mAh/g, from data, it is apparent that graphene
Cladding silicon-carbon composite cathode material significantly improves its cycle performance.
The design focal point of the present invention is：Present invention application high speed grinding method, is prepared for binary composite nano Si-stone
Black alkene compound, the specific capacity for effectively improving Si sills and the cycle performance under low current density, meet the needs used.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore it is every according to the technical essence of the invention to any subtle modifications, equivalent variations and modifications made by above example, still
Belong in the range of technical solution of the present invention.
Claims (2)
1. a kind of method preparing graphene coated silicon-carbon composite cathode material, it is characterised in that：Include following steps：
（1）The preparation of nano Si particle：Pre- logical Ar/H2 gas 15-25 min, gas flow rate 0.1-2 L/min；By 8-12g quotient
Product Si particles are sent by feed inlet in grinding pot, are injected 150-190 mL acetone into grinding pot by feed inlet, are used rubber plug
Feed inlet is sealed, buckle closure is screwed；It sets rotating speed to 2200-2700rpm, starts to grind, respectively in 0.5 h, 1 h, 1.5 h
Sample is collected with 2 h；The sample of recycling is placed in vacuum drying chamber, temperature setting is 70-80 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 1.5-2.5h, it is ultrasonically treated 1.5-2.5h, vacuum filtration is then empty dry under 70-90 DEG C of condition vacuum condition
Dry 10-20 h, obtained black powder are graphene coated silicon-carbon composite cathode material.
2. a kind of method preparing graphene coated silicon-carbon composite cathode material according to claim 1, it is characterised in that：
Include following steps：
（1）The preparation of nano Si particle：Pre- logical 20 min of Ar/H2 gas, 0.1 L/min of gas flow rate；10g is commercialized Si
Grain is sent by feed inlet in grinding pot, is injected 170 mL acetone into grinding pot by feed inlet, is sealed feed inlet with rubber plug,
Screw buckle closure；It sets rotating speed to 2500rpm, starts to grind, collect sample in 0.5 h, 1 h, 1.5 h and 2 h respectively；
The sample of recycling is placed in vacuum drying chamber, temperature setting is 75 DEG C of vacuum drying；
（2）Mechanical mixing：By graphene and nano Si particle with mass ratio for 1:1 is added among absolute ethyl alcohol, passes through
After magnetic agitation 2h, it is ultrasonically treated 2h, vacuum filtration, then empty dry 15 h under 80 DEG C of condition vacuum conditions, obtained
Black powder is graphene coated silicon-carbon composite cathode material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122749A (en) * | 2019-12-31 | 2021-07-16 | 山西沃特海默新材料科技股份有限公司 | Carbon source reinforcing agent, carbon source reinforcing alloy and preparation method thereof |
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| US20150295227A1 (en) * | 2014-04-11 | 2015-10-15 | Xin Zhao | Silicon and graphene-incorporated rechargeable li-ion batteries with enhanced energy delivery and cycling life by using silecon and graphene based anode for energy storage |
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| CN103022436A (en) * | 2011-09-21 | 2013-04-03 | 海洋王照明科技股份有限公司 | Electrode composite material preparation method |
| US20150295227A1 (en) * | 2014-04-11 | 2015-10-15 | Xin Zhao | Silicon and graphene-incorporated rechargeable li-ion batteries with enhanced energy delivery and cycling life by using silecon and graphene based anode for energy storage |
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| CN113122749A (en) * | 2019-12-31 | 2021-07-16 | 山西沃特海默新材料科技股份有限公司 | Carbon source reinforcing agent, carbon source reinforcing alloy and preparation method thereof |
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