CN107946542A - Lithium ion battery negative material and preparation method, anode and lithium ion battery - Google Patents
Lithium ion battery negative material and preparation method, anode and lithium ion battery Download PDFInfo
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- CN107946542A CN107946542A CN201711214806.0A CN201711214806A CN107946542A CN 107946542 A CN107946542 A CN 107946542A CN 201711214806 A CN201711214806 A CN 201711214806A CN 107946542 A CN107946542 A CN 107946542A
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- lithium ion
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
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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 relates to lithium ion battery negative material and preparation method, anode and lithium ion battery.The negative active core-shell material is three-layer nuclear shell structure, and innermost layer is graphene, and intermediate layer is nano-silicon, and outermost layer is amorphous carbon, and the mass fraction of graphene, nano-silicon and amorphous carbon is respectively：50 80 parts of graphene, 20 30 parts of nano-silicon, 30 40 parts of amorphous carbon.The lithium ion battery negative material of the present invention is used in lithium ion battery, and high rate performance is high, and cyclical stability is strong.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material and preparation method thereof, contain the lithium ion battery negative material
Negative electrode of lithium ion battery and lithium ion battery containing the negative electrode of lithium ion battery.
Background technology
With the high speed development of today's society Portable movable electronic equipment, to light-weight, small, capacity and energy
The market demand of the lithium ion battery of density higher is increasing.Lithium ion battery success application, key is can be reversible
Ground is embedded in and the negative material of deintercalate lithium ions, and therefore, negative material is the chief component of lithium ion battery, negative material
Performance directly affects the performance of lithium ion battery.
Commercial Li-ion battery is all using carbon-based material as anode, but due to the reversible capacity of graphite cathode at present
Only 372mAh/g (LiC6), seriously limits the development of following lithium ion battery, and therefore, there is an urgent need to one kind, and there is higher to hold
The lithium ion battery negative material of amount.
The content of the invention
In order to solve the problems, such as that the reversible capacity of graphite cathode is low, the present invention proposes a kind of negative electrode of lithium ion battery material
Material, preparation method and the negative electrode of lithium ion battery containing the lithium ion battery negative material, and contain the lithium ion battery
The lithium ion battery of anode.
First purpose of the present invention is to provide a kind of lithium ion battery negative material, which is three-layer nuclear shell knot
Structure, innermost layer are graphene, and intermediate layer is nano-silicon, and outermost layer is amorphous carbon, the matter of graphene, nano-silicon and amorphous carbon
Measuring number is respectively：50-80 parts of graphene, 20-30 parts of nano-silicon, 30-40 parts of amorphous carbon.
As preference, the amorphous carbon presoma is selected from sucrose, soluble starch, selected from coal tar pitch and petroleum asphalt, phenolic aldehyde
At least one of resin, epoxy resin and glucose.
Second object of the present invention is to provide the method for preparing above-mentioned negative material, includes the following steps：With silicic acid second
Ester is raw material, after adding graphene, water and ammonium hydroxide is added dropwise in ultrasound and ultrahigh speed whipping process, makes silester in stone
Black alkene surface hydrolysis, 20-30 DEG C of insulation 1-2h, 50-60 DEG C of insulation reaction 1-3h, dry 2-6h at 120-150 DEG C；Utilize magnesium heat
In-situ reducing silica is reacted into nano-silicon, and is attached to the graphene particles that graphene surface forms nano-silicon cladding；
The graphene particles mixing of amorphous carbon presoma and nano-silicon cladding, is warming up to 100-120 DEG C, then keeps the temperature 1-3h, then with
The heating rate of 2-6 DEG C/min is warming up to 140-150 DEG C, keeps the temperature 0.5-1.5h；Then carbonization treatment is carried out, in inert gas ring
Under border, 350-450 DEG C is warming up to the heating rate of 4-6 DEG C/min, keeps the temperature 1.5-2.5h, then the speed liter with 5-15 DEG C/min
Temperature arrives 600-800 DEG C, keeps the temperature 2-4h, obtains lithium ion battery negative material.
Third object of the present invention is to provide a kind of negative electrode of lithium ion battery, the anode include collector and coating and/
Or it is filled in the negative material on collector, it is characterised in that the negative material is above-mentioned lithium ion battery negative material.
Fourth object of the present invention is to provide a kind of lithium ion battery, and the anode is above-mentioned anode, efficient first,
Volume and capacity ratio is high, and high rate performance is high, and cyclical stability is strong.
Embodiment
Embodiment 1
80 parts of graphene, 20 parts of nano-silicon, 40 parts of amorphous carbon, amorphous carbon presoma are sucrose.
Using silester as raw material, after adding graphene, water and ammonia is added dropwise in ultrasound and ultrahigh speed whipping process
Water, makes silester be hydrolyzed in graphene surface, 20 DEG C of insulation 2h, 50 DEG C of insulation reaction 3h, dry 2h at 150 DEG C；Utilize magnesium
Thermal response in-situ reducing silica is attached to the graphene that graphene surface forms nano-silicon cladding into nano-silicon
Grain；The graphene particles mixing of amorphous carbon presoma and nano-silicon cladding, is warming up to 100 DEG C, then keeps the temperature 3h, then with 2 DEG C/
The heating rate of min is warming up to 150 DEG C, keeps the temperature 1.5h；Then carbonization treatment is carried out, in an inert atmosphere, with 6 DEG C/min
Heating rate be warming up to 450 DEG C, keep the temperature 2.5h, then 600 DEG C are warming up to the speed of 5 DEG C/min, keep the temperature 4h, obtain lithium ion
Cell negative electrode material.
Embodiment 2
50 parts of graphene, 30 parts of nano-silicon, 40 parts of amorphous carbon, amorphous carbon presoma are epoxy resin.
Using silester as raw material, after adding graphene, water and ammonia is added dropwise in ultrasound and ultrahigh speed whipping process
Water, makes silester be hydrolyzed in graphene surface, 30 DEG C of insulation 1h, 60 DEG C of insulation reaction 1h, dry 6h at 120 DEG C；Utilize magnesium
Thermal response in-situ reducing silica is attached to the graphene that graphene surface forms nano-silicon cladding into nano-silicon
Grain；The graphene particles mixing of amorphous carbon presoma and nano-silicon cladding, is warming up to 120 DEG C, then keeps the temperature 1h, then with 6 DEG C/
The heating rate of min is warming up to 150 DEG C, keeps the temperature 1.5h；Then carbonization treatment is carried out, in an inert atmosphere, with 4 DEG C/min
Heating rate be warming up to 350 DEG C, keep the temperature 1.5h, then 800 DEG C are warming up to the speed of 15 DEG C/min, keep the temperature 2h, obtain lithium from
Sub- cell negative electrode material.
Embodiment 3
80 parts of graphene, 30 parts of nano-silicon, 0 part of amorphous carbon, amorphous carbon presoma are glucose.
Using silester as raw material, after adding graphene, water and ammonia is added dropwise in ultrasound and ultrahigh speed whipping process
Water, makes silester be hydrolyzed in graphene surface, 20 DEG C of insulation 2h, 60 DEG C of insulation reaction 1h, dry 6h at 150 DEG C；Utilize magnesium
Thermal response in-situ reducing silica is attached to the graphene that graphene surface forms nano-silicon cladding into nano-silicon
Grain；The graphene particles mixing of amorphous carbon presoma and nano-silicon cladding, is warming up to 120 DEG C, then keeps the temperature 3h, then with 2 DEG C/
The heating rate of min is warming up to 150 DEG C, keeps the temperature 1.5h；Then carbonization treatment is carried out, in an inert atmosphere, with 4 DEG C/min
Heating rate be warming up to 350 DEG C, keep the temperature 1.5h, then 600 DEG C are warming up to the speed of 5 DEG C/min, keep the temperature 4h, obtain lithium ion
Cell negative electrode material.
It is by weight by the negative material of embodiment 1-3, acetylene black and PVDF：Negative material：Acetylene black：PVDF=
80：10：The tabletting after mixing of 10 ratio, then be dried in vacuo 24h at 120 DEG C and obtain work pole piece；Using metal lithium sheet as pair
Electrode, celgard2400 polypropylene porous films are membrane, and LiPF6 is dissolved in ethylene carbonate (EC) and dimethyl carbonate
(DMC) be electrolyte mixed solution (volume ratio of EC and DMC be=1：1) the LiPF6 solution that concentration is 1mol/L is formed in,
And assembled in the glove box full of argon gas, battery sample S1-S3 is obtained, by lithium ion battery S1-S3 respectively in 0.1C charge and discharges
Charge-discharge test is carried out under the conditions of electric multiplying power.
The performance parameter of S1-S3 is shown in Table 1.With high specific capacity, first discharge specific capacity reaches more than 590mAh/g, first
Secondary efficiency is more than 92%, and after 50 circulations, gram specific capacity is still in 530mAh/g or so, still greater than the theoretical specific capacity of graphite
372mAh/g.It can be seen from the above that the lithium ion battery negative material of the present invention is used in lithium ion battery, high rate performance is high, circulation
Stability is strong.
Claims (5)
1. a kind of lithium ion battery negative material, it is characterised in that the negative material is three-layer nuclear shell structure, and innermost layer is graphite
Alkene, intermediate layer are nano-silicon, and outermost layer is amorphous carbon, and the mass fraction of graphene, nano-silicon and amorphous carbon is respectively：Stone
Black alkene 50-80 parts, 20-30 parts of nano-silicon, 30-40 parts of amorphous carbon.
A kind of 2. lithium ion battery negative material as claimed in claim 1, it is characterised in that the amorphous carbon presoma choosing
From at least one of sucrose, soluble starch, selected from coal tar pitch and petroleum asphalt, phenolic resin, epoxy resin and glucose.
3. the method for the negative material as described in claim 1-2 is any is prepared it is characterised in that it includes following steps：With silicic acid second
Ester is raw material, after adding graphene, water and ammonium hydroxide is added dropwise in ultrasound and ultrahigh speed whipping process, makes silester in stone
Black alkene surface hydrolysis, 20-30 DEG C of insulation 1-2h, 50-60 DEG C of insulation reaction 1-3h, dry 2-6h at 120-150 DEG C；Utilize magnesium heat
In-situ reducing silica is reacted into nano-silicon, and is attached to the graphene particles that graphene surface forms nano-silicon cladding；
The graphene particles mixing of amorphous carbon presoma and nano-silicon cladding, is warming up to 100-120 DEG C, then keeps the temperature 1-3h, then with
The heating rate of 2-6 DEG C/min is warming up to 140-150 DEG C, keeps the temperature 0.5-1.5h；Then carbonization treatment is carried out, in inert gas ring
Under border, 350-450 DEG C is warming up to the heating rate of 4-6 DEG C/min, keeps the temperature 1.5-2.5h, then the speed liter with 5-15 DEG C/min
Temperature arrives 600-800 DEG C, keeps the temperature 2-4h, obtains lithium ion battery negative material.
4. a kind of negative electrode of lithium ion battery, which includes collector and coating and/or the negative material being filled on collector,
It is characterized in that, the negative material is the lithium ion battery negative material described in claim 1 or 2.
5. a kind of lithium ion battery, it is characterised in that the anode is the anode described in claim 4.
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| CN201711214806.0A CN107946542A (en) | 2017-11-28 | 2017-11-28 | Lithium ion battery negative material and preparation method, anode and lithium ion battery |
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| CN201711214806.0A CN107946542A (en) | 2017-11-28 | 2017-11-28 | Lithium ion battery negative material and preparation method, anode and lithium ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807940A (en) * | 2018-07-18 | 2018-11-13 | 绍兴文理学院 | A kind of preparation method of graphene enhancing carbon-silicon composite material |
| CN108923048A (en) * | 2018-07-06 | 2018-11-30 | 武汉霖泉环保科技有限公司 | A kind of lithium ion battery negative material, preparation facilities and method |
| CN109244401A (en) * | 2018-09-04 | 2019-01-18 | 南京工业大学 | A kind of porous nano Si-C composite material and preparation method thereof using magnesium reduction process preparation |
| CN111816856A (en) * | 2020-07-21 | 2020-10-23 | 深圳先进技术研究院 | Composite material, preparation method thereof and negative electrode |
| WO2022016374A1 (en) * | 2020-07-21 | 2022-01-27 | 深圳先进技术研究院 | Composite material, preparation method therefor, and negative electrode |
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Application publication date: 20180420 |