CN106505189A - A kind of three-dimensional silica-polypyrrole-graphite cathode material and preparation method thereof - Google Patents
A kind of three-dimensional silica-polypyrrole-graphite cathode material and preparation method thereof Download PDFInfo
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- CN106505189A CN106505189A CN201510897574.8A CN201510897574A CN106505189A CN 106505189 A CN106505189 A CN 106505189A CN 201510897574 A CN201510897574 A CN 201510897574A CN 106505189 A CN106505189 A CN 106505189A
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- graphite
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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
- 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
- H01M4/362—Composites
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- 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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- 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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
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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
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- 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 lithium battery three-dimensional silica-polypyrrole-graphite cathode material and preparation method thereof.Elemental silicon as base material, is combined together with graphite using the method for Chemical bonding, makes a kind of lithium battery three-dimensional silica-polypyrrole-graphite cathode material using graphite material by the present invention.The present invention has capacity height, efficiency high, the characteristic for expanding little, good cycle, and cost of material is low, step is simple, favorable repeatability, can really realize the large-scale production containing silicium cathode in field of lithium ion battery.
Description
Technical field：The present invention relates to a kind of lithium battery three-dimensional silica-polypyrrole-graphite cathode material, belongs to
Technical field of lithium-ion battery.
Technical background：
The research of negative material is always the emphasis in Study on Li-ion batteries field, with the progress of science and technology, lithium
The demand of ion battery is more and more diversified.Diversified demand is faced, negative material should possess following
Feature：1. good cycle life, 2. relatively low irreversible capacity, 3. good with compatibility of electrolyte, 4. higher
Specific capacity.Existing negative material mainly based on carbon materials (graphite, soft carbon, hard carbon), due to stone
The relatively low theoretical lithium storage content (372mAh/g) of black negative pole itself makes which be difficult to have breakthrough progress again.Therefore,
The new lithium cell cathode material of research has become the heat subject of lithium battery research field, wherein especially with silicon material
Material is more popular.
At present, silicon materials are always the focus of negative pole area research.With graphite-phase ratio, the specific capacity of silicon materials
It is more than ten times of graphite, up to 4200mAh/g.But silicon materials directly act on cathode of lithium battery and there is also
Larger problem：In battery charge and discharge process, the bulking effect of negative pole affects the cycle performance of battery than more serious.
Solve the problems, such as that expansion mainly has at present：1. simple with graphite material be used in mixed way, but this use silicon material
The addition of material is generally below 5%, is not very high to the lifting of capacity；2. nano level silicon is prepared, so may be used
To alleviate the volumetric expansion in charging process；3. special structure is prepared, and the advantage using structure is alleviating volume
Expansion.
Content of the invention：
For the problem that present silicium cathode uses process, the negative pole material for lithium ion battery proposed by the present invention
Material has three dimensional structure, and it can be that the expansion of silicon improves certain cushion space, alleviate material in discharge and recharge
Bulk effect in journey, improves capacity and the circulation of lithium ion battery, reduces expansion.
For achieving the above object, involved technical scheme is：A kind of three-dimensional silica-polypyrrole-graphite cathode
Material and preparation method thereof, comprises the following steps：
Step (1)：Elemental silicon, pyrroles are dissolved in deionized water, are placed in ultrasonic stirrer and are stirred,
Graphite is added in the mixed liquor, mixed slurry is formed through ultrasonic disperse and magnetic agitation.
Step (2)：The appropriate FeCl of Deca toward the mixed liquor of step 13·6H2O, during Deca not
Disconnected stirring, makes pyrroles fully react into polypyrrole, by product first with dehydrated alcohol and deionized water wash mistake
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.?
Heat treatment is carried out in vacuum or inert atmosphere, three-dimensional silicon substrate composite negative pole material is obtained.
The material of the present invention is had the advantage that due to its construction features：1. due to structure itself the characteristics of,
Big perforate is conducive to the migration of liquid electrolyte；2. structure can be such that electrolyte is fully contacted with material, reduce
3. structure can improve the electrical conductivity of lithium ion in the path of the diffusion mobility of lithium ion, so as to conductive agent need not be added,
4. three dimensional structure can effectively absorb and buffer the bulk effect of silicon, improve the cycle performance of material.
Description of the drawings
Loop test figures of the Fig. 1 for preferred embodiment 4.
SEMs of the Fig. 2 for preferred embodiment 4.
Specific embodiment
Below in conjunction with the embodiment of the present invention, to the embodiment of the present invention in technical scheme carry out clear, complete
Ground description, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole enforcement
Example.Embodiment in based on the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The every other embodiment for being obtained, belongs to the scope of protection of the invention.
Embodiment 1
Step (1)：10g elemental silicons, 10g pyrroles are dissolved in 200ml deionized waters, ultrasound are placed in and are stirred
Mix in device and stir, 80g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 2
Step (1)：10g elemental silicons, 15g pyrroles are dissolved in 200ml deionized waters, ultrasound are placed in and are stirred
Mix in device and stir, 75g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 3
Step (1)：10g elemental silicons, 20g pyrroles are dissolved in 200ml deionized waters, ultrasound are placed in and are stirred
Mix in device and stir, 70g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 4
Step (1)：15g is dissolved in elemental silicon, 10g pyrroles in 200ml deionized waters, is placed in ultrasound and stirs
Mix in device and stir, 75g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 5
Step (1)：20g is dissolved in elemental silicon, 10g pyrroles in 200ml deionized waters, is placed in ultrasound and stirs
Mix in device and stir, 70g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 6
Step (1)：20g is dissolved in elemental silicon, 15g pyrroles in 200ml deionized waters, is placed in ultrasound and stirs
Mix in device and stir, 65g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica/graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Embodiment 7
Step (1)：20g is dissolved in elemental silicon, 20g pyrroles in 200ml deionized waters, is placed in ultrasound and stirs
Mix in device and stir, 60g graphite is added in the mixed liquor, formed through ultrasonic disperse and magnetic agitation mixed
Close slurry.
Step (2)：Toward the appropriate FeCl of the mixed solution and dripping of step 13·6H2O, during Deca
It is stirred continuously, makes pyrroles fully react into polypyrrole, reflection product is first used dehydrated alcohol and deionized water wash
Filter, then at -40 DEG C to -50 DEG C, lyophilization obtains the presoma of three-dimensional silica-graphite cathode material.
In nitrogen atmosphere, 1150 carry out heat treatment, obtain three-dimensional silicon substrate composite negative pole material.
Three-dimensional silicon substrate composite negative pole material in embodiment 1～7 carries out particle diameter, true density, compacting respectively
Density, specific surface area, ash and gram volume and the test of efficiency, the results are shown in Table 1.Test is used
Instrument title and model：Particle diameter：Laser fineness gage MS2000；True density：Super constant temperature water tank
SC-15；Ash：High-temperature electric resistance furnace SX2-2.5-12；Specific surface area：Specific surface area measuring instrument NOVA2000；
Discharge capacity, first discharging efficiency first：Multi-channel battery test Bt2000 type.The data of above-described embodiment
It is listed in Table 1
Half-cell method of testing used by of the invention is：Composite negative pole material, contain 6～7% Kynoar
N-Methyl pyrrolidone and 2% conductive black mix homogeneously, be applied on Copper Foil, the pole piece for coating be put into
Temperature is standby for being vacuum dried 4 hours in 110 DEG C of vacuum drying ovens.Simulated battery is assemblied in the Germany of applying argon gas
Carry out in Braun glove box, electrolyte is 1M LiPF6+EC: DEC: DMC=1: 1: 1 (volume ratio),
Metal lithium sheet is that electrochemical property test is carried out on U.S. ArbinBT2000 type cell testers to electrode,
Charging/discharging voltage scope is 0.005 to 1.0V, and charge-discharge velocity is 0.1C.Preferred embodiment 4 is followed
Ring test, test data such as table 1.
Table 1:
Full battery testing method used is：With material as cathode, cobalt acid lithium obtained in the embodiment of the present invention 1
Make positive pole, 1M-LiPF6EC: EMC: DMC=1: 1: 1 (volume ratio) solution is made electrolyte assembling and helps battery,
Tested.Cycle performance is shown in Fig. 1.As can be seen, the Delanium-silicon composite cathode prepared by the present invention
Material circulation excellent performance
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and
And without departing from the spirit or essential characteristics of the present invention, this can be realized in other specific forms
Bright.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and is non-limiting
, the scope of the present invention is by claims rather than described above is limited, it is intended that will fall will in right
All changes in the implication and scope of the equivalency that asks are included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only
Comprising an independent technical scheme, this narrating mode of description is only this area skill for clarity
Art personnel should using description as an entirety, the technical scheme in each embodiment can also through appropriately combined,
Formed it will be appreciated by those skilled in the art that other embodiment.
Claims (8)
1. a kind of preparation method of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that including following step
Suddenly：
Step (1) is dissolved in elemental silicon, pyrroles in deionized water, is placed in ultrasonic stirrer and stirs,
Graphite fine powder is added in the mixed liquor, mixed slurry is formed through ultrasonic disperse and magnetic agitation；
Step (2) is toward the appropriate FeCl of Deca in the mixed liquor of step 13·6H2O, during Deca constantly
Stirring, makes pyrroles fully react into polypyrrole, and product is first washed with dehydrated alcohol and deionization
Filtration is washed, then lyophilization obtains three-dimensional silica-graphite cathode material at -40 DEG C to -50 DEG C
Presoma.Heat treatment is carried out in vacuum or inert atmosphere, a kind of three-dimensional silica-polypyrrole-graphite is obtained
Negative material.
2. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that institute
Stating graphite fine powder includes one or more in Delanium, native graphite, carbonaceous mesophase spherules.
3. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that institute
The particle diameter of graphite fine powder graphite is stated at 1-50 μm, whole composite negative pole material gross mass is accounted for
60%-80%.
4. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that poly-
Pyrroles is evenly coated at graphite surface by synthesis, and polypyrrole accounts for whole composite negative pole material
10%-20%.
5. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that
By polypyrrole together with graphite gluing, silicon accounts for the 10%-20% of whole material to silicon materials.
6. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that silicon
Material includes polycrystalline silica flour, amorphous silicon powders, the sub- Si powder of oxidation.
7. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that heat
Temperature ranges are 1000 DEG C -1300 DEG C.
8. according to claim 1, a kind of three-dimensional silica-polypyrrole-graphite cathode material, it is characterised in that lazy
Property gas includes nitrogen, argon.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195874A (en) * | 2017-04-19 | 2017-09-22 | 深圳市沃特玛电池有限公司 | A kind of preparation method of the Si-C composite material of polypyrrole cladding |
| CN109524630A (en) * | 2017-09-20 | 2019-03-26 | 上海杉杉科技有限公司 | A kind of preparation method of cladded type composite negative pole material |
| CN110474038A (en) * | 2019-09-19 | 2019-11-19 | 山东大学 | A kind of silicium cathode material and preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347857A (en) * | 2013-07-29 | 2015-02-11 | 华为技术有限公司 | Lithium ion secondary cell cathode active material and preparation method thereof, lithium ion secondary cell cathode pole piece and lithium ion secondary cell |
| CN104752698A (en) * | 2013-12-25 | 2015-07-01 | 北京有色金属研究总院 | Silicon carbon composite material for lithium ion battery cathode, and preparation method of composite material |
-
2015
- 2015-12-08 CN CN201510897574.8A patent/CN106505189A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347857A (en) * | 2013-07-29 | 2015-02-11 | 华为技术有限公司 | Lithium ion secondary cell cathode active material and preparation method thereof, lithium ion secondary cell cathode pole piece and lithium ion secondary cell |
| CN104752698A (en) * | 2013-12-25 | 2015-07-01 | 北京有色金属研究总院 | Silicon carbon composite material for lithium ion battery cathode, and preparation method of composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195874A (en) * | 2017-04-19 | 2017-09-22 | 深圳市沃特玛电池有限公司 | A kind of preparation method of the Si-C composite material of polypyrrole cladding |
| CN107195874B (en) * | 2017-04-19 | 2019-05-28 | 深圳市沃特玛电池有限公司 | A kind of preparation method of the Si-C composite material of polypyrrole cladding |
| CN109524630A (en) * | 2017-09-20 | 2019-03-26 | 上海杉杉科技有限公司 | A kind of preparation method of cladded type composite negative pole material |
| CN110474038A (en) * | 2019-09-19 | 2019-11-19 | 山东大学 | A kind of silicium cathode material and preparation method and application |
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