CN105680026B - Carbon composite and preparation method thereof and battery - Google Patents

Carbon composite and preparation method thereof and battery Download PDF

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Publication number
CN105680026B
CN105680026B CN201610254924.3A CN201610254924A CN105680026B CN 105680026 B CN105680026 B CN 105680026B CN 201610254924 A CN201610254924 A CN 201610254924A CN 105680026 B CN105680026 B CN 105680026B
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carbon composite
carbon
graphite
tin
middle layer
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CN105680026A (en
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相江峰
郝三存
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Gcl Energy Storage Technology Suzhou Co ltd
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Suzhou Xiexin Integrated Energy Storage Technology Co Ltd
Suzhou Gcl System Integration Technology Industrial Application Research Institute Co Ltd
GCL System Integration Technology Co Ltd
GCL System Integration Technology Suzhou Co Ltd
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 field of batteries, specifically disclose a kind of carbon composite comprising kernel, the middle layer being coated on outside kernel and the outer layer being coated on outside middle layer；Kernel is graphite, and middle layer is silica-base material or tin-based material, and outer layer is porous carbon.Above-mentioned carbon composite, silica-base material or tin-based material are between graphite and porous carbon, to can inhibit material powder；Porous carbon has reserved enough spaces, can buffer the cyclic stress of silica-base material or tin-based material itself expansion generation, also avoid dusting；So the present invention has good cycle performance.In addition, the porous carbon of outer layer can effectively prevent silica-base material or tin-based material directly and electrolyte contacts, irreversible capacity is reduced, while porous carbon promotes the electric conductivity of carbon composite；And porous carbon also helps the deintercalation of lithium ion due to its porosity.The invention also discloses a kind of preparation method of carbon composite and batteries.

Description

Carbon composite and preparation method thereof and battery
Technical field
The present invention relates to field of batteries, more particularly to a kind of carbon composite and preparation method thereof and battery.
Background technique
Compared with traditionally graphite cathode material, silicon have superelevation theoretical specific capacity (4200mAh/g) and it is lower take off Lithium current potential (< 0.5V), and the voltage platform of silicon is slightly above graphite, is less likely to occur surface analysis lithium behavior, safety in charging More preferably, therefore the new research direction of negative electrode material of battery can be become.
But since silicon is semiconductor material, when as cell negative electrode material, self-conductance rate is lower, and lithium ion is filling Insertion and abjection in discharge process can make silicon volume occur 300% or more expansion and contraction, can make powder body material structure by It gradually collapses, eventually leads to electrode active material and collector is detached from, cycle performance of battery is caused to substantially reduce.
For the cycle performance for improving silicon materials, cyclical stability is improved, while improving the electric conductivity of silicon materials.Usually by silicon Material and carbon material Composite, because carbon material electronic conductivity with higher and ionic conductivity, can significantly improve silicon substrate The high rate performance of material inhibits the electric conductivity of bulk effect and improvement silica-base material of the silicon in cyclic process.
But the cycle performance of traditional composite material need to be improved.
Summary of the invention
Based on this, it is necessary to aiming at the problem that existing composite material poor circulation, it is high to provide a kind of cycle performance Carbon composite.
A kind of carbon composite including kernel, the middle layer being coated on outside the kernel and is coated on the middle layer Outer outer layer；The kernel is graphite, and the middle layer is silica-base material or tin-based material, and the outer layer is porous carbon.
Above-mentioned carbon composite, silica-base material or tin-based material are between graphite and porous carbon, so as to effectively press down Silica-base material or tin-based material dusting processed；And due to the porosity of porous carbon, enough spaces are reserved, have buffered silicon substrate The cyclic stress that itself expansion of material or tin-based material in cyclic process generates, to also avoid silica-base material or tinbase Material dusting collapses, and improves structural stability；So carbon composite of the invention has good cycle performance.In addition, more Hole carbon potential can effectively prevent silica-base material or tin-based material from directly sending out with electrolyte contacts in the outer layer of carbon composite Raw redox reaction, effectively reduces irreversible capacity.Secondly, porous carbon has good conductive property, so as to have Effect promotes the electric conductivity of carbon composite；And porous carbon also helps the deintercalation of lithium ion due to its porosity.
The silica-base material is nano cilicon fibre in one of the embodiments,；The tin-based material is nanometer tin fiber.
The average grain diameter of the graphite is 5~40 μm in one of the embodiments,.
In one of the embodiments, the middle layer with a thickness of 20~100nm.
In one of the embodiments, the outer layer with a thickness of 100~500nm.
The average grain diameter of the carbon composite is 5~50 μm in one of the embodiments,.
In one of the embodiments, on the basis of the quality of the carbon composite, the graphite accounts for 85~ 98wt%, the middle layer account for 1~10wt%, and the porous carbon accounts for 1~5wt%.
The present invention also provides a kind of preparation methods of above-mentioned carbon composite.
A kind of preparation method of carbon composite, includes the following steps:
Silica-base material or tin-based material are coated on graphite particle, the first core-shell material is obtained；
First core-shell material and carbon matrix precursor are dispersed in dispersing agent, at a temperature of 160~180 DEG C, Under the pressure of 0.15MPa~0.3MPa, 3~6h is reacted, carbon composite is obtained.
Above-mentioned preparation method, technique are easy to control, and production capacity is big, are conducive to the industrialization large-scale production of carbon composite.
Silica-base material or tin-based material are coated on graphite particle using vapour deposition process in one of the embodiments, Cladding.
In one of the embodiments, the carbon matrix precursor be selected from cellulose, sucrose, glucose, fructose, maltose and One or more of starch.
The present invention also provides a kind of batteries.
A kind of battery comprising carbon composite provided by the present invention.
Above-mentioned battery, due to using carbon composite provided by the present invention, so battery has good cycle performance, And irreversible capacity is low.
Detailed description of the invention
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.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with specific embodiment The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are only used to explain the present invention, It is not intended to limit the present invention.
A kind of carbon composite including kernel, the middle layer being coated on outside kernel and is coated on outer outside middle layer Layer；Kernel is graphite, and middle layer is silica-base material or tin-based material, and outer layer is porous carbon.
Wherein, kernel of the graphite as carbon composite, for carrying middle layer and outer layer.Graphite of the invention can be with It is natural or artificial graphite, more specifically, natural graphite preferably uses crystalline flake graphite.Preferably, the average grain diameter of graphite It is 5~40 μm.Be conducive in this way carbon composite have it is suitably sized, be conducive to the performance of carbon composite performance.It is preferred that Ground, on the basis of the quality of carbon composite, graphite accounts for 85~98wt%.That is, graphite in carbon composite hundred Divide than being 85~98wt%.The comprehensive performance of carbon composite can be made more excellent in this way, meet the needs of battery is to negative electrode material.
Wherein, silica-base material can be the oxide of elemental silicon or silicon, can also be silicon metal compounds.The present invention Silica-base material be preferably nano cilicon fibre.Tin-based material can be simple substance tin or tin oxide, and tin-based material of the invention is excellent It is selected as nanometer tin fiber.
Preferably, middle layer with a thickness of 20~100nm.
Preferably, on the basis of the quality of carbon composite, silica-base material or tin-based material account for 1~10wt%.Namely It says, the percentage of silica-base material or tin-based material in carbon composite is 1~10wt%.It can make the comprehensive of carbon composite in this way It is more excellent to close performance, meets the needs of battery is to negative electrode material.
Wherein, porous carbon is located at the outer layer of carbon composite.Porous carbon can directly contact to avoid silicon materials with electrolyte And bring adverse effect, since the contact performance of porous carbon and electrolyte is preferable, so as to improve entire carbon composite and electricity Solve the contact performance of liquid.
Preferably, the aperture of porous carbon is 2~100nm.It can be more conducive to deintercalation and the SEI of lithium ion in this way The formation of film.
Preferably, outer layer with a thickness of 100~500nm.Be conducive to the deintercalation of lithium ion in this way, while being conducive to improve carbon The specific capacity of composite material.
Preferably, on the basis of the quality of carbon composite, porous carbon accounts for 1~10wt%.That is, porous carbon is in carbon Percentage in composite material is 1~10wt%.Be conducive to improve the specific capacity of carbon composite in this way.
Wherein, the average grain diameter of carbon composite is 5~50 μm.It is more advantageous to later period coating so 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, so as to effectively press down Silica-base material or tin-based material dusting processed；And due to the porosity of porous carbon, enough spaces are reserved, have buffered silicon substrate The cyclic stress that itself expansion of material or tin-based material in cyclic process generates, to also avoid silica-base material or tinbase Material dusting collapses, and improves structural stability；So carbon composite of the invention has good cycle performance.In addition, more Hole carbon potential can effectively prevent silica-base material or tin-based material from directly sending out with electrolyte contacts in the outer layer of carbon composite Raw redox reaction, effectively reduces irreversible capacity.Secondly, porous carbon has good conductive property, so as to have Effect promotes the electric conductivity of carbon composite；And porous carbon also helps the deintercalation of lithium ion due to its porosity.
The present invention also provides a kind of preparation methods of above-mentioned carbon composite.
A kind of preparation method of carbon composite, includes the following steps:
S1, silica-base material or tin-based material are coated on graphite particle, obtain the first core-shell material；
S2, the first core-shell material and carbon matrix precursor are dispersed in dispersing agent, at a temperature of 160~180 DEG C, Under the pressure of 0.15~0.3MPa, 3~6h is reacted, carbon composite is obtained.
In S1, cladding can select chemistry cladding or physics cladding with actual conditions.Wherein, chemistry cladding can use gas Phase sedimentation, such as with SiO2Ar gas or N are passed through using low vacuum tubular type furnace system for raw material2Gas will be reacted as carrier gas Pressure is adjusted to 50000Pa, 900-1200 DEG C of temperature, reacts 1-3h.Wherein, physics cladding can be ball milling cladding or stirring packet It covers, such as by nano cilicon fibre and graphite particle ball milling in the ball mill.
In S2, carbon matrix precursor refers to can be carbonized to form the organic compound of porous carbon at high temperature under high pressure.Preferably, originally The carbon matrix precursor of invention is selected from one or more of cellulose, sucrose, glucose, fructose, maltose and starch.Certainly, may be used What it is with understanding is, it is not limited to which above compound, carbon matrix precursor can also be polyvinyl alcohol or phenolic resin etc..
In S2, dispersing agent is to dissolve carbon matrix precursor or disperse to keep carbon matrix precursor and the first core-shell material evenly dispersed. Preferably, dispersing agent can be water, ethyl alcohol, propyl alcohol, isopropanol or acetone.It is highly preferred that dispersing agent is water.It in this way can be into one Step reduces cost.
Above-mentioned preparation method, technique are easy to control, and production capacity is big, are conducive to the industrialization large-scale production of carbon composite.
The present invention also provides a kind of batteries.
A kind of battery comprising carbon composite provided by the present invention.
Other components and its connection relationship in battery can use various parts known in those skilled in the art And its various connection relationships, details are not described herein.
Above-mentioned battery, due to using carbon composite provided by the present invention, so that its energy density is high, and cycle life It is long.
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
30g natural graphite (average grain diameter is 25 μm) is placed in ball mill, 3g nano cilicon fibre (diameter is then added Less than 100nm, 1 μm~50 μm of length), obtain the first core-shell material.
The first obtained core-shell material is placed in the tempering reaction kettle of 1L, the cellulose aqueous solution of 200g is then added (1wt%)；At 170 DEG C, 6h is reacted at 0.25MPa.
Obtained carbon composite, is denoted as A1.
Embodiment two
In low vacuum tubular type furnace system, on 30g natural graphite (average grain diameter is 45 μm), with the SiO of 6g2For original Material is 50000Pa in pressure using Ar gas as carrier gas, and temperature is to react 2h at 1000 DEG C, waits until the first core-shell material.
The first obtained core-shell material is placed in the tempering reaction kettle of 1L, the aqueous sucrose solution of 300g is then added (1wt%)；At 180 DEG C, 5h is reacted at 0.15MPa.
Obtained carbon composite, is denoted as A2.
Embodiment three
30g natural graphite (average grain diameter is 25 μm) is placed in ball mill, 2g nanometer tin fiber (diameter is then added Less than 100nm, 1 μm~50 μm of length), obtain the first core-shell material.
The first obtained core-shell material is placed in the tempering reaction kettle of 1L, the glucose solution of 250g is then added (1wt%)；At 160 DEG C, 4h is reacted at 0.3MPa.
Obtained carbon composite, is denoted as A3.
Comparative example 1
30g natural graphite (average grain diameter is 25 μm) is placed in ball mill, 3g nano cilicon fibre (diameter is then added Less than 100nm, 1 μm -10 μm of length), obtained material is denoted as D1.
Performance test
SEM test:
Electron-microscope scanning is done respectively to carbon composite A1 and D1, SEM figure is shown in Fig. 1 and Fig. 2 respectively.
It can be seen that from Fig. 1 and Fig. 2, carbon composite A1 has not seen the nano-silicon of threadiness；And carbon composite D1 It can find out the nano-silicon of threadiness.
Cycle performance test:
Using carbon composite A1 and D1 as negative electrode material, using cobalt acid lithium as to electrode, polyethylene monolayer film be every Film, electrolyte are 1mol/L LiPF6The mixing of ethylene carbonate (EC)/dimethyl carbonate (DMC)/methyl ethyl carbonate (EMC) Solution；It is assembled into test battery.0.5C rate charge-discharge circulation is carried out to test battery, test temperature is 25 DEG C.Test result See Fig. 3.Curve above in Fig. 3 is carbon composite A1, in Fig. 3 below curve be carbon composite D1.
From figure 3, it can be seen that carbon composite A1 is after the circle of circulation 300, capacity retention ratio still maintains 90% More than, and carbon composite D1 obviously decays from cycle life after 100 circles.This illustrates carbon composite wood provided by the present invention Material has good cycle performance.

Claims (4)

1. a kind of preparation method of carbon composite, which comprises the steps of:
Tin-based material is coated on graphite particle, the first core-shell material is obtained, wherein tin-based material is nanometer tin fiber, is received The length of rice tin fiber is 1 micron~50 microns；
First core-shell material and carbon matrix precursor are dispersed in dispersing agent, at a temperature of 160~180 DEG C, Under the pressure of 0.15MPa~0.3MPa, 3~6h is reacted, carbon composite is obtained, wherein the carbon composite is by kernel, packet The middle layer overlayed on outside the kernel and the outer layer being coated on outside middle layer composition；The kernel be graphite, it is described in Interbed is nanometer tin fiber, and the outer layer is porous carbon, and the average grain diameter of the graphite is 5~40 μm, the thickness of the middle layer Degree is 20~100nm, the outer layer with a thickness of 100~500nm, the average grain diameter of the carbon composite is 5~50 μm, with On the basis of the quality of the carbon composite, the graphite accounts for 85~98wt%, and the middle layer accounts for 1~10wt%, described more Hole carbon accounts for 1~5wt%.
2. preparation method according to claim 1, which is characterized in that the carbon matrix precursor is selected from cellulose, sucrose, grape One or more of sugar, fructose, maltose and starch.
3. a kind of carbon composite obtained using any one of claim 1~2 preparation method, which is characterized in that described Carbon composite is made of kernel, the middle layer being coated on outside the kernel and the outer layer being coated on outside the middle layer；Institute Stating kernel is graphite, and the middle layer is nanometer tin fiber, and the outer layer is porous carbon, the average grain diameter of the graphite is 5~ 40 μm, the middle layer with a thickness of 20~100nm, the outer layer with a thickness of 100~500nm, the carbon composite Average grain diameter is 5~50 μm, and on the basis of the quality of the carbon composite, the graphite accounts for 85~98wt%, the centre Layer accounts for 1~10wt%, and the porous carbon accounts for 1~5wt%.
4. a kind of battery, which is characterized in that the battery includes carbon composite as claimed in claim 3.
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CN106058228A (en) * 2016-07-15 2016-10-26 中天储能科技有限公司 Core-shell structure silicon-carbon composite material as well as preparation method and application thereof
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
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
CN112142060B (en) * 2020-09-21 2022-04-19 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
CN112133898B (en) * 2020-09-21 2022-04-19 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
CN112125294B (en) * 2020-09-21 2022-04-19 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
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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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