CN105680026A - Carbon composite material, preparation method for carbon composite material and battery - Google Patents
Carbon composite material, preparation method for carbon composite material and battery Download PDFInfo
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- CN105680026A CN105680026A CN201610254924.3A CN201610254924A CN105680026A CN 105680026 A CN105680026 A CN 105680026A CN 201610254924 A CN201610254924 A CN 201610254924A CN 105680026 A CN105680026 A CN 105680026A
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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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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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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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 invention relates to the field of batteries, in particular to a carbon composite material. The carbon composite material comprises a core, a middle layer covering the core, and an outer layer covering the middle layer, wherein the core is graphite; the middle layer is a silicon-based material or a tin-based material; and the outer layer is porous carbon. According to the carbon composite material, the silicon-based material or the tin-based material is positioned between the graphite and the porous carbon, so that the material pulverization can be inhibited; the porous carbon reserves sufficient space, so that the cyclic stress generated by expansion of the silicon-based material or the tin-based material can be buffered and the pulverization is avoided; and therefore, the carbon composite material has good cyclic performance. In addition, the porous carbon of the outer layer can effectively prevent the silicon-based material or the tin-based material from being in direct contact with an electrolyte solution, reduce the irreversible capacity and improve the conductive performance of the carbon composite material; and the porous carbon is favorable for insertion and extraction of lithium ions due to porosity. The invention furthermore discloses a preparation method for the carbon composite material and a battery.
Description
Technical field
The present invention relates to field of batteries, particularly relate to a kind of carbon composite and its preparation method and battery.
Background technology
Compared with tradition ground graphite cathode material, silicon has the theoretical specific capacity (4200mAh/g) of superelevation and lower de-lithium current potential (< 0.5V), and the voltage platform of silicon is a little more than graphite, surface analysis lithium behavior it is less likely to occur when charging, safety performance is better, therefore becomes the research direction that the negative material of battery is new.
But, owing to silicon is semiconductor material, during as cell negative electrode material, self specific conductivity is lower, the embedding of lithium ion in charge and discharge process and deviate to make silicon volume that expansion and the contraction of more than 300% occur, powder body material structure can be made to cave in gradually, finally cause electrode active material and collector to depart from, cause cycle performance of battery greatly to reduce.
For improving the cycle performance of silicon materials, it is to increase cyclical stability, improve the electroconductibility of silicon materials simultaneously. Usually by silicon materials and carbon material Composite, because carbon material has higher electronic conductivity and ionic conductivity, can significantly improve the high rate performance of silica-base material, suppress the volume effect of silicon in working cycle and improve the conductivity of silica-base material.
But, the cycle performance of traditional matrix material need to improve.
Summary of the invention
Based on this, it is necessary to for the problem of existing matrix material cycle performance difference, it is provided that the carbon composite that a kind of cycle performance is high.
A kind of carbon composite, the middle layer comprise kernel, being coated on outside described kernel and the skin being coated on outside described middle layer; Described kernel is graphite, and described middle layer is silica-base material or tin-based material, and described skin is porous carbon.
Above-mentioned carbon composite, silica-base material or tin-based material are between graphite and porous carbon, such that it is able to effectively suppression silica-base material or tin-based material efflorescence; And the porousness due to porous carbon, it has reserved enough spaces, buffering silica-base material or the tin-based material cyclic stress self expanding and producing in working cycle, thus it also avoid silica-base material or tin-based material efflorescence, subside, it is to increase structural stability; So the carbon composite of the present invention has good cycle performance. In addition, porous carbon is positioned at the skin of carbon composite, it is possible to effective prevention silica-base material or tin-based material directly contact with electrolytic solution and redox reaction occurs, and effectively reduce irreversible capacity. Secondly, porous carbon has good conductivity, such that it is able to effectively promote the conductivity of carbon composite; And porous carbon is due to its porousness, also help the deintercalation of lithium ion.
Wherein in an embodiment, described silica-base material is nano cilicon fibre;Described tin-based material is nanometer tin fiber.
Wherein in an embodiment, the median size of described graphite is 5～40 μm.
Wherein in an embodiment, the thickness in described middle layer is 20～100nm.
Wherein in an embodiment, described outer field thickness is 100～500nm.
Wherein in an embodiment, the median size of described carbon composite is 5～50 μm.
Wherein in an embodiment, taking the quality of described carbon composite as benchmark, described graphite accounts for 85～98wt%, and described middle layer accounts for 1～10wt%, and described porous carbon accounts for 1～5wt%.
Present invention also offers the preparation method of a kind of above-mentioned carbon composite.
A preparation method for carbon composite, comprises the steps:
Silica-base material or tin-based material are coated on graphite particle, obtain the first core-shell material;
Being dispersed in dispersion agent by described first core-shell material and carbon matrix precursor, at 160～180 DEG C of temperature, under the pressure of 0.15MPa～0.3MPa, reaction 3～6h, obtains carbon composite.
Above-mentioned preparation method, technique easily controls, and production capacity is big, is conducive to the industrialization scale operation of carbon composite.
Wherein in an embodiment, silica-base material or tin-based material are coated on graphite particle and adopt vapour deposition process coated.
Wherein in an embodiment, described carbon matrix precursor be selected from Mierocrystalline cellulose, sucrose, glucose, fructose, maltose and starch one or more.
Present invention also offers a kind of battery.
A kind of battery, it comprises carbon composite provided by the present invention.
Above-mentioned battery, owing to adopting carbon composite provided by the present invention, so battery has good cycle performance, and irreversible capacity is low.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the carbon composite of the embodiment of the present invention one.
Fig. 2 is the SEM figure of the carbon composite of comparative example one of the present invention.
Fig. 3 is the cycle performance of battery figure of the carbon composite of the embodiment of the present invention one and comparative example one.
Embodiment
In order to make the object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated. It is to be understood that embodiment described herein is only in order to explain the present invention, it is not intended to limit the present invention.
A kind of carbon composite, the middle layer comprise kernel, being coated on outside kernel and the skin being coated on outside middle layer; Kernel is graphite, and middle layer is silica-base material or tin-based material, and skin is porous carbon.
Wherein, graphite as the kernel of carbon composite, for carrying middle layer and skin. The graphite of the present invention can be natural graphite or synthetic graphite, and more specifically, natural graphite preferably adopts crystalline flake graphite. Preferably, the median size of graphite is 5～40 μm. Be conducive to carbon composite to have suitable size like this, be conducive to the performance of carbon composite performance. Preferably, taking the quality of carbon composite as benchmark, graphite accounts for 85～98wt%. That is, the per-cent of graphite in carbon composite is 85～98wt%. The over-all properties of carbon composite can be made so more excellent, meet battery to the demand of negative material.
Wherein, silica-base material can be elemental silicon, also or the oxide compound of silicon, it is also possible to be silicon metallizing compound. The silica-base material of the present invention is preferably nano cilicon fibre. Tin-based material can be simple substance tin or stannic oxide, and the tin-based material of the present invention is preferably nanometer tin fiber.
Preferably, the thickness in middle layer is 20～100nm.
Preferably, taking the quality of carbon composite as benchmark, silica-base material or tin-based material account for 1～10wt%. That is, per-cent in carbon composite of silica-base material or tin-based material is 1～10wt%. The over-all properties of carbon composite can be made so more excellent, meet battery to the demand of negative material.
Wherein, porous carbon is positioned at the skin of carbon composite. Porous carbon can avoid the detrimentally affect that silicon materials directly contact and bring with electrolytic solution, owing to the contact performance of porous carbon and electrolytic solution is better, thus improves the contact performance of whole carbon composite and electrolytic solution.
Preferably, the aperture of porous carbon is 2～100nm. Like this can advantageously in the deintercalation of lithium ion, and the formation of SEI film.
Preferably, outer field thickness is 100～500nm. Be conducive to the deintercalation of lithium ion like this, be conducive to improving the specific storage of carbon composite simultaneously.
Preferably, taking the quality of carbon composite as benchmark, porous carbon accounts for 1～10wt%. That is, the per-cent of porous carbon in carbon composite is 1～10wt%. Be conducive to improving the specific storage of carbon composite like this.
Wherein, the median size of carbon composite is 5～50 μm. The later stage is so more conducive to apply on a current collector.
Preferably, in carbon composite, graphite accounts for 85～98wt%, and middle layer accounts for 1～10wt%, and porous carbon accounts for 1～5wt%.
Above-mentioned carbon composite, silica-base material or tin-based material are between graphite and porous carbon, such that it is able to effectively suppression silica-base material or tin-based material efflorescence; And the porousness due to porous carbon, it has reserved enough spaces, buffering silica-base material or the tin-based material cyclic stress self expanding and producing in working cycle, thus it also avoid silica-base material or tin-based material efflorescence, subside, it is to increase structural stability; So the carbon composite of the present invention has good cycle performance. In addition, porous carbon is positioned at the skin of carbon composite, it is possible to effective prevention silica-base material or tin-based material directly contact with electrolytic solution and redox reaction occurs, and effectively reduce irreversible capacity. Secondly, porous carbon has good conductivity, such that it is able to effectively promote the conductivity of carbon composite; And porous carbon is due to its porousness, also help the deintercalation of lithium ion.
Present invention also offers the preparation method of a kind of above-mentioned carbon composite.
A preparation method for carbon composite, comprises the steps:
S1, silica-base material or tin-based material are coated on graphite particle, obtain the first core-shell material;
S2, being dispersed in dispersion agent by the first core-shell material and carbon matrix precursor, at 160～180 DEG C of temperature, under the pressure of 0.15～0.3MPa, reaction 3～6h, obtains carbon composite.
In S1, coated practical situation chemistry can be selected coated or physics is coated. Wherein, chemistry is coated can adopt vapour deposition process, such as, with SiO2For raw material, adopt rough vacuum tubular type furnace system, lead to into Ar gas or N2Reaction pressure, as carrier gas, is adjusted to 50000Pa by gas, temperature 900-1200 DEG C, reaction 1-3h. Wherein, physics is coated can be that ball milling is coated or stir coated, the such as ball milling in ball mill by nano cilicon fibre and graphite particle.
In S2, carbon matrix precursor refer at high temperature under high pressure can carbonization formed porous carbon organic compound. Preferably, the carbon matrix precursor of the present invention be selected from Mierocrystalline cellulose, sucrose, glucose, fructose, maltose and starch one or more. Of course, it is understood that be not limited to above-claimed cpd, carbon matrix precursor can also be polyvinyl alcohol or resol etc.
In S2, dispersion agent dissolves carbon matrix precursor or disperse carbon matrix precursor and the first core-shell material are evenly disperseed.Preferably, dispersion agent can be water, ethanol, propyl alcohol, Virahol or acetone. More preferably, dispersion agent is water. Can reduce costs further like this.
Above-mentioned preparation method, technique easily controls, and production capacity is big, is conducive to the industrialization scale operation of carbon composite.
Present invention also offers a kind of battery.
A kind of battery, it comprises carbon composite provided by the present invention.
Other parts in battery and the relation of connection thereof, all could adopt various parts known in those skilled in the art and various connection relation thereof, not repeat them here!
Above-mentioned battery, owing to adopting carbon composite provided by the present invention, thus its energy density height, and have extended cycle life.
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
30g natural graphite (median size is 25 μm) is positioned in ball mill, then adds 3g nano cilicon fibre (diameter is less than 100nm, length 1 μm～50 μm), obtain the first core-shell material.
The first core-shell material obtained is positioned in the tempering reactor of 1L, then adds the cellulose aqueous solution (1wt%) of 200g; At 170 DEG C, under 0.25MPa, react 6h.
The carbon composite obtained, is denoted as A1.
Embodiment two
In rough vacuum tubular type furnace system, on 30g natural graphite (median size is 45 μm), with the SiO of 6g2For raw material, using Ar gas as carrier gas, being 50000Pa at pressure, temperature is react 2h at 1000 DEG C, by the time the first core-shell material.
The first core-shell material obtained is positioned in the tempering reactor of 1L, then adds the aqueous sucrose solution (1wt%) of 300g; At 180 DEG C, under 0.15MPa, react 5h.
The carbon composite obtained, is denoted as A2.
Embodiment three
30g natural graphite (median size is 25 μm) is positioned in ball mill, then adds 2g nanometer tin fiber (diameter is less than 100nm, length 1 μm～50 μm), obtain the first core-shell material.
The first core-shell material obtained is positioned in the tempering reactor of 1L, then adds the D/W (1wt%) of 250g; At 160 DEG C, under 0.3MPa, react 4h.
The carbon composite obtained, is denoted as A3.
Comparative example 1
Being positioned in ball mill by 30g natural graphite (median size is 25 μm), then add 3g nano cilicon fibre (diameter is less than 100nm, length 1 μm-10 μm), the material obtained, is denoted as D1.
Performance test
SEM tests:
Carbon composite A1 and D1 is done electron-microscope scanning respectively, and SEM figure is shown in Fig. 1 and Fig. 2 respectively.
From Fig. 1 and Fig. 2 it can be seen that carbon composite A1 has not seen fibrous nano-silicon; And carbon composite D1 can find out fibrous nano-silicon.
Cycle performance is tested:
Using carbon composite A1 and D1 as negative material, using cobalt acid lithium as to electrode, polyethylene unitary film is barrier film, electrolytic solution is 1mol/LLiPF6The mixing solutions of NSC 11801 (EC)/methylcarbonate (DMC)/Methyl ethyl carbonate (EMC); It is assembled into test battery. Test battery is carried out 0.5C rate charge-discharge circulation, and probe temperature is 25 DEG C. Test result is shown in Fig. 3. Curve above in Fig. 3 is carbon composite A1, and the curve below in Fig. 3 is carbon composite D1.
As can be seen from Figure 3, carbon composite A1 is after circulation 300 circle, and capability retention still maintains more than 90%, and after carbon composite D1 encloses from 100, cycle life obviously decays. This illustrates carbon composite provided by the present invention, has good cycle performance.
Claims (10)
1. a carbon composite, it is characterised in that, the middle layer comprise kernel, being coated on outside described kernel and the skin being coated on outside described middle layer;Described kernel is graphite, and described middle layer is silica-base material or tin-based material, and described skin is porous carbon.
2. carbon composite according to claim 1, it is characterised in that, described silica-base material is nano cilicon fibre; Described tin-based material is nanometer tin fiber.
3. carbon composite according to claim 1, it is characterised in that, the median size of described graphite is 5～40 μm.
4. carbon composite according to claim 1, it is characterised in that, the thickness in described middle layer is 20～100nm.
5. carbon composite according to claim 1, it is characterised in that, described outer field thickness is 100～500nm.
6. carbon composite according to claim 1, it is characterised in that, the median size of described carbon composite is 5～50 μm.
7. carbon composite according to claim 1, it is characterised in that, taking the quality of described carbon composite as benchmark, described graphite accounts for 85～98wt%, and described middle layer accounts for 1～10wt%, and described porous carbon accounts for 1～5wt%.
8. the preparation method of a carbon composite according to claim 1, it is characterised in that, comprise the steps:
Silica-base material or tin-based material are coated on graphite particle, obtain the first core-shell material;
Being dispersed in dispersion agent by described first core-shell material and carbon matrix precursor, at 160～180 DEG C of temperature, under the pressure of 0.15MPa～0.3MPa, reaction 3～6h, obtains carbon composite.
9. preparation method according to claim 8, it is characterised in that, described carbon matrix precursor be selected from Mierocrystalline cellulose, sucrose, glucose, fructose, maltose and starch one or more.
10. a battery, it is characterised in that, the carbon composite described in the described arbitrary item of battery claim 1～7.
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| CN106941170A (en) * | 2017-04-24 | 2017-07-11 | 广东烛光新能源科技有限公司 | A kind of silicon-carbon cathode material and preparation method thereof |
| US10468674B2 (en) | 2018-01-09 | 2019-11-05 | South Dakota Board Of Regents | Layered high capacity electrodes |
| CN112133898A (en) * | 2020-09-21 | 2020-12-25 | 陕西煤业化工技术研究院有限责任公司 | Silicon-based negative electrode material and preparation method thereof |
| CN112125294A (en) * | 2020-09-21 | 2020-12-25 | 陕西煤业化工技术研究院有限责任公司 | Coal-based silicon-carbon composite negative electrode material and preparation method thereof |
| CN112142060A (en) * | 2020-09-21 | 2020-12-29 | 陕西煤业化工技术研究院有限责任公司 | Coal-based silicon-carbon composite negative electrode material and preparation method thereof |
| CN112310347A (en) * | 2020-11-03 | 2021-02-02 | 珠海冠宇电池股份有限公司 | Lithium ion battery with high energy density and charging capacity |
| CN113690424A (en) * | 2021-10-26 | 2021-11-23 | 天津师范大学 | Carbon-tin-silicon negative electrode material of lithium ion battery and preparation method thereof |
| 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 |
| US11626584B2 (en) | 2014-04-25 | 2023-04-11 | South Dakota Board Of Regents | High capacity electrodes |
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| CN112310347A (en) * | 2020-11-03 | 2021-02-02 | 珠海冠宇电池股份有限公司 | Lithium ion battery with high energy density and charging capacity |
| CN112310347B (en) * | 2020-11-03 | 2022-03-18 | 珠海冠宇电池股份有限公司 | Lithium ion battery with high energy density and charging capacity |
| CN113690424A (en) * | 2021-10-26 | 2021-11-23 | 天津师范大学 | Carbon-tin-silicon negative electrode material of lithium ion battery and preparation method thereof |
| CN113690424B (en) * | 2021-10-26 | 2022-01-07 | 天津师范大学 | Carbon-tin-silicon negative electrode material of lithium ion battery and preparation method thereof |
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