CN107925073A - The method and silicon-carbon compound of carbon coating are prepared on silica-base material - Google Patents
The method and silicon-carbon compound of carbon coating are prepared on silica-base material Download PDFInfo
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- CN107925073A CN107925073A CN201580082393.8A CN201580082393A CN107925073A CN 107925073 A CN107925073 A CN 107925073A CN 201580082393 A CN201580082393 A CN 201580082393A CN 107925073 A CN107925073 A CN 107925073A
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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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- 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
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Abstract
The present invention provides the method that carbon coating is prepared on silica-base material.In addition, the silicon-carbon compound comprising silica-base material and carbon coating is made by the method.
Description
Technical field
The present invention relates to the method that carbon coating is prepared on silica-base material and by including silicon substrate made from the method
The silicon-carbon compound of material and carbon coating.
Background technology
Present graphite is mainly used as lithium ion battery negative material.Many times charging cycle is still shown surely graphite experience
Fixed performance, but low capacity is only provided.Such as in order to extend the operating range of electric car, must using, there is higher to store
The negative material of capacity replaces graphite.Someone considers silicon for this, it provides the capacity than graphite higher.However, the conduction of silicon
Property several orders of magnitude lower than graphite.Which has limited high rate performance, i.e., the short charging interval.Therefore, conductive black is added to carry
The electric conductivity of high silicon-based anode and thus improve high rate performance.However, the very high specific surface area of conductive black causes in head
Irreversible capacity loss increase in secondary charge and discharge cycles.In addition, conductive black must be distributed so as to effectively as homogeneously as possible
Silicon is contacted, this make it that the processing of electrode material slurry is even more difficult.
The content of the invention
Therefore, it is an object of the invention to be led by applying carbon coating on silica-base material and thus reducing in electrode material
The content of electric carbon black, so that obvious more uniformly contact silicon and improve the electric conductivity of silica-base material and thus improve forthright again
Can, so that the shortcomings that overcoming the prior art.In addition, carbon coating well known in the art can also make the SEI to be formed (solid electricity
Solve matter interface) stabilize.
The purpose can realize that the described method includes following step by preparing the method for carbon coating on silica-base material
Suddenly：
1) carbon precursor is applied on the surface of the silica-base material；
2) product that heating is obtained by step 1) in protective atmosphere at a temperature of 300 to 1000 DEG C；Wherein described carbon
Precursor is one or more silicon compounds with carbon-containing group.
According to another aspect of the present invention, there is provided the silicon-carbon compound comprising silica-base material and carbon coating, wherein the carbon
Coating is by prepared in accordance with the method for the present invention.
According to another aspect of the present invention, there is provided electrode, wherein the electrode includes silicon-carbon compound according to the present invention
And one or more powder and/or the conductive carbonaceous additive of form of chips.
According to another aspect of the present invention, there is provided battery, wherein the battery pack contains electrode according to the present invention.
Brief description of the drawings
Various aspects of the invention are explained in more detail according to attached drawing, wherein：
Fig. 1 show the SEM photograph of pure silicon granules (CE2)；
Fig. 2 show the SEM photograph of the silicon-carbon compound of embodiment 1 (E1)；
Fig. 3 show the silicon-carbon compound of embodiment 1 (E1), the silicon-carbon compound of comparative example 1 (CE1) and comparative example 2
(CE2) high rate performance of pure silicon granules.
Embodiment
If without in addition illustrating, by publications all referred in this, patent application, patent and other bibliography
Full content is clearly incorporated herein by reference for all purposes, as fully illustrated.
Unless otherwise defined, all technical and scientific terms as used herein have and the technical field of the invention
Those of ordinary skill is common to understand identical implication.It is subject to the present specification if there is conflict, including definition.
If quantity, concentration or other numerical value or parameter as scope, preferable scope or a series of preferable upper limits and
Preferable lower limit provides, then should be understood to particularly discloses by any pair of any range upper limit or preferable numerical value with
All scopes that any range lower limit or preferable numerical value are formed, no matter whether these scopes are respectively disclosed.Carry herein
And numerical value scope when, unless otherwise indicated, it is meant that the scope includes its endpoint and all integers within the range
And fraction.
According on one side, the present invention relates to the method that carbon coating is prepared on silica-base material, the described method includes following
Step：
1) carbon precursor is applied on the surface of the silica-base material；
2) product that heating is obtained by step 1) in protective atmosphere at a temperature of 300 to 1000 DEG C；Wherein described carbon
Precursor is one or more silicon compounds with carbon-containing group.
According to an embodiment of the method according to the invention, the silica-base material can be in the following group：Silicon is received
Rice grain, silicon micron particles, porous silicon powder, silicon oxide particle, silicon substrate compound and silicon-base alloy.Within the scope of the present invention,
The particle diameter of nano particle is less than 100nm, and the particle diameter of micron particles is more than or equal to 100nm and less than 100 μm.
According to another embodiment of the method according to the invention, the carbon precursor can be it is one or more be selected from
Silicon compound in the following group：Silane, siloxanes, silazane, polysilane, polysiloxanes, polysilazane and based on aforementioned polymer
Copolymer, its condition is：These silicon compounds have carbon-containing group.
According to another embodiment of the method according to the invention, in step 1), the silicon with carbon-containing group
Compound can be attached on the surface of the silica-base material via chemical bond.
According to another embodiment of the method according to the invention, the carbon-containing group can be in the following group：Through
C1-20 alkyl, C2-20 alkenyls, C2-20 alkynyls, C6-12 aryl, C7-20 aralkyl and the C7-20 alkane for substituting or being unsubstituted
Aryl.
According to another embodiment of the method according to the invention, the carbon-containing group can be phenyl.
According to another embodiment of the method according to the invention, the silicon compound with carbon-containing group can be
Polyphenyl base silane comprising following formula unit
Wherein n is 1 to 500 000 integer.
According to another aspect, the present invention relates to the silicon-carbon compound for including silica-base material and carbon coating, wherein the carbon applies
Layer is by prepared in accordance with the method for the present invention.
According on the other hand, the present invention relates to electrode, wherein the electrode include silicon-carbon compound according to the present invention and
The conductive carbonaceous additive of one or more powder and/or form of chips.
According to an embodiment of electrode according to the present invention, the conductive carbonaceous additive of the form of chips can be stone
Ink.
According to another embodiment of electrode according to the present invention, the BET of the conductive carbonaceous additive of the powder type
Specific surface area is 40 to 1500m2/ g, is preferably 50 to 100m2/g。
According to another embodiment of electrode according to the present invention, the conductive carbonaceous additive of the powder type can be
Carbon black, such as acetylene black, Super P carbon blacks and Ketjen are black.
According to another embodiment of electrode according to the present invention, based on the weight of the electrode, the powder type
The content of conductive carbonaceous additive be less than 20 weight %, be preferably less than 10 weight %, more preferably less than 5 weight %.
According to another aspect, the present invention relates to battery, wherein the battery pack contains electrode according to the present invention.
Embodiment 1 (E1)：
Prepare carbon precursor：
By polymerizeing dichloro base silane, so as to synthesize polyphenyl base silane.1.5 grams of polyphenyl base silanes are made to exist
Dissolved in 100mL THF.Then 1.5 grams of silica flours (Sunsil, D are added50=700-800nm) and be stirred.During churning
Evaporation of the solvent.
Apply carbon coating：
When heating silicon-polyphenylene silane precursor 2 is small in protective atmosphere at a temperature of 700 DEG C.The powder of gained includes
The carbon of about 20 weight % (according to thermogravimetric analysis).
Structural appraisal：
Use the size and structure of scanning electron microscope (SEM) characterization product.
Fig. 2 show the SEM photograph of the silicon-carbon compound of embodiment 1 (E1).Compared with showing Fig. 1 of pure silicon granules, by
Fig. 2 can be seen that silicon grain has been evenly coated with carbon coating.
Battery assembles and electrochemistry assessment：
Use the chemical property of the so obtained composition of bipolar electrode button cell test.By make active material,
Super P conductive blacks (40nm, Timcal)/graphite scrap (12 as conductive carbonaceous additive:13 weight ratios) and as viscous
Mixture styrene butadiene ribber/sodium carboxymethylcellulose (SBR/SCMC, 1:1 weight ratio) weight ratio be 60:25:15
(active material:Conductive carbonaceous additive:Adhesive) mixture gelatinization, preparation work electrode.It is pure the mixture is coated in
After on Cu paper tinsels, make pole drying, cut into Φ 14mm thin slices, be then further dried in a vacuum at 70 DEG C 6 it is small when.
In the glove box (MB-10compact, MBraun) of applying argon gas, 1M LiPF are used6/EC+EMC(1:1 weight ratio, ethylene two
Ester (EC), methyl ethyl carbonate (EMC)) electrolyte is used as, it includes 5 weight % fluoro ethylene carbonates (FEC), use glass fibers
Dimension is used as membrane, using pure lithium paper tinsel as to electrode, so as to assemble CR2016 button cells.In Basytec battery test systems
On at 23 DEG C assessments performance.Blanking voltage is when discharging (embedding Li) relative to Li/Li+For 0.01V, (de- Li) is being charged
When relative to Li/Li+For 1.5V.
Fig. 3 show the high rate performance of the silicon-carbon compound of embodiment 1 (E1).
Embodiment 2：
Embodiment 2 is implemented similar to Example 1ly, and difference lies in use 0.7 gram of polyphenyl base silane.The powder of gained contains
The carbon of about 10 weight % (according to TGA).
Comparative example 1 (CE1)：
Comparative example 1 is implemented similar to Example 1ly, and polyphenyl base silane is replaced as the carbon difference lies in citric acid is used
Precursor.
Fig. 3 show the high rate performance of the silicon-carbon compound of comparative example 1 (CE1).
As can be seen that the specific capacity with the silicon-carbon compound (CE1) of carbon coating made of citric acid is minimum, under 1C
Even close to zero.
Comparative example 2 (CE2)：
Comparative example 2 is implemented similar to Example 1ly, and difference lies in carbon coating is not applied on silicon grain, active material, lead
The weight ratio of electrical carbon additive and adhesive is 54:31:15.
Fig. 1 show the SEM photograph of pure silicon granules (CE2).Fig. 3 show the multiplying power of the pure silicon granules of comparative example 2 (CE2)
Performance.
As can be seen that it is being, for example, less than pure silicon granules (CE2) and with made of polyphenyl base silane under C/2 compared with low range
The difference of the specific capacity of the silicon-carbon compound (E1) of carbon coating is negligible, and is being greater than being equal to C/2 compared with high magnification
The lower specific capacity with the silicon-carbon compound (E1) of carbon coating made of polyphenyl base silane is then significantly greater than pure silicon granules
(CE2).It means that with made of polyphenyl base silane the silicon-carbon compound (E1) of carbon coating show the aobvious of high rate performance
Writing improves.
Although describing specific embodiment, these embodiments only provide in an exemplary fashion, are not meant to
Limit the scope of the invention.Appended appended claims and their equivalents mean that covering is fallen within the spirit and scope of the invention
All modifications, replacement and change scheme.
Claims (12)
1. preparing the method for carbon coating on silica-base material, the described method comprises the following steps：
1) carbon precursor is applied on the surface of the silica-base material；
2) product that heating is obtained by step 1) in protective atmosphere at a temperature of 300 to 1000 DEG C；
It is characterized in that, the carbon precursor is one or more silicon compounds with carbon-containing group.
2. the method according to claim 1, it is characterised in that the silica-base material is in the following group：Nano silicon particles, silicon are micro-
Rice grain, porous silicon powder, silicon oxide particle, silicon substrate compound and silicon-base alloy.
3. according to the method for claim 1 or 2, it is characterised in that the carbon precursor is one or more in the following group
Silicon compound：Silane, siloxanes, silazane, polysilane, polysiloxanes, polysilazane and the copolymer based on aforementioned polymer,
Its condition is：These silicon compounds have carbon-containing group.
4. according to the method for one of claims 1 to 3, it is characterised in that the carbon-containing group is in the following group：Be substituted or
C1-20 alkyl, C2-20 alkenyls, C2-20 alkynyls, C6-12 aryl, C7-20 aralkyl and the C7-20 alkaryls being unsubstituted.
5. method according to claim 4, it is characterised in that the carbon-containing group is phenyl.
6. according to the method for one of claim 1 to 5, it is characterised in that the silicon compound with carbon-containing group is polyphenyl
Base silane.
7. the silicon-carbon compound comprising silica-base material and carbon coating, it is characterised in that the carbon coating is by being wanted according to right
Ask made from one of 1 to 6 method.
8. electrode, it is characterised in that the electrode includes silicon-carbon compound according to claim 7 and one or more powder
And/or the conductive carbonaceous additive of form of chips.
9. electrode according to claim 8, it is characterised in that the BET specific surface area of the conductive carbonaceous additive of the powder type
For more than 40 to 1500m2/g。
10. according to the electrode of claim 8 or 9, it is characterised in that the conductive carbonaceous additive of the powder type is carbon black, example
As acetylene black, Super P carbon blacks and Ketjen are black.
11. according to the electrode of one of claim 8 to 10, it is characterised in that the weight based on the electrode, the powder type
The content of conductive carbonaceous additive be less than 20 weight %, be preferably less than 10 weight %, more preferably less than 5 weight %.
12. battery, it is characterised in that the battery includes the electrode according to one of claim 8 to 11.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2015/087240 WO2017028160A1 (en) | 2015-08-17 | 2015-08-17 | A method for preparing a carbon coating on a silicon-based material and a silicon-carbon composite |
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| Publication Number | Publication Date |
|---|---|
| CN107925073A true CN107925073A (en) | 2018-04-17 |
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| CN201580082393.8A Pending CN107925073A (en) | 2015-08-17 | 2015-08-17 | The method and silicon-carbon compound of carbon coating are prepared on silica-base material |
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| WO (1) | WO2017028160A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899527A (en) * | 2018-07-12 | 2018-11-27 | 浙江工业职业技术学院 | A kind of preparation method of high magnification silicon based composite material |
| CN110649254A (en) * | 2019-09-06 | 2020-01-03 | 成都新柯力化工科技有限公司 | Lithium battery silicon-carbon negative electrode composite material and preparation method thereof |
| WO2020073889A1 (en) * | 2018-10-08 | 2020-04-16 | 广东美的厨房电器制造有限公司 | Coating composition and preparation method therefor, coating member and preparation method therefor, and household appliance |
| CN112467098A (en) * | 2020-10-30 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | High-capacity and good-stability silicon-carbon negative electrode material and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950478B (en) * | 2017-12-20 | 2020-12-15 | 中国科学院化学研究所 | Coating method of electrode material, coating object and application thereof |
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2015
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| CN1674325A (en) * | 2004-03-26 | 2005-09-28 | 信越化学工业株式会社 | Silicon composite particles, preparation thereof, and negative electrode material for non-aqueous electrolyte secondary cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108899527A (en) * | 2018-07-12 | 2018-11-27 | 浙江工业职业技术学院 | A kind of preparation method of high magnification silicon based composite material |
| CN108899527B (en) * | 2018-07-12 | 2021-06-15 | 浙江工业职业技术学院 | Preparation method of high-rate silicon-based composite material |
| WO2020073889A1 (en) * | 2018-10-08 | 2020-04-16 | 广东美的厨房电器制造有限公司 | Coating composition and preparation method therefor, coating member and preparation method therefor, and household appliance |
| CN110649254A (en) * | 2019-09-06 | 2020-01-03 | 成都新柯力化工科技有限公司 | Lithium battery silicon-carbon negative electrode composite material and preparation method thereof |
| CN112467098A (en) * | 2020-10-30 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | High-capacity and good-stability silicon-carbon negative electrode material and preparation method thereof |
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| WO2017028160A1 (en) | 2017-02-23 |
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