CN106058228A - Core-shell structure silicon-carbon composite material as well as preparation method and application thereof - Google Patents
Core-shell structure silicon-carbon composite material as well as preparation method and application thereof Download PDFInfo
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- CN106058228A CN106058228A CN201610559413.2A CN201610559413A CN106058228A CN 106058228 A CN106058228 A CN 106058228A CN 201610559413 A CN201610559413 A CN 201610559413A CN 106058228 A CN106058228 A CN 106058228A
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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
- 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 invention discloses a core-shell structure silicon-carbon composite material as well as a preparation method and application thereof. The core-shell structure silicon-carbon composite material is of a three-layer structure, wherein the inner layer is a graphite base body; the middle layer is a silicon-base coated layer; the outer layer is a carbon layer. The core-shell structure silicon-carbon composite material can be adopted to manufacture lithium batteries of the core-shell structure silicon-carbon composite material. As graphite is taken as the base body, silicon-base powder is adhered to surfaces of graphite granules to form the coated layer by using an adhesive in a spraying manner, subsequently the coated layer is further coated by a layer of carbon by using a chemical vapor deposition method, and meanwhile carbon can be also generated from the adhesive in a pyrolysis manner. The prepared material structurally comprises a graphite core, a silicon-base coated layer and an outer carbon coated layer, due to the three layers of the core-shell structure, volume change of the silicon-base material in the charge and discharge process can be effectively inhibited, the conductivity of the material can be improved, and the material is prepared by using specially designed devices and is simple in process, convenient to operate and applicable to industrialization.
Description
Technical field
The invention belongs to electrode material and prepare field of lithium, be specifically related to a kind of nucleocapsid structure Si-C composite material and
Preparation method and purposes.
Background technology
Current business-like lithium cell cathode material is mainly graphite type material, and its theoretical specific capacity only has 372mAh/g,
The requirement of lithium ion battery high-energy-density and high security cannot be met.Silica-base material has and closely decuples at present commercial graphite
The theoretical capacity of capacity of negative plates, gets more and more people's extensive concerning recently.On the basis of existing battery processing technique, if it is possible to
Replace Carbon anode with silicium cathode, negative material consumption in the battery will can be greatly decreased, reduce negative pole shared in the battery
Volume, and in identical battery space, just can increase the consumption of positive electrode, thus promote the energy density of battery.This
Outward, select silica-base material as negative pole, it is also possible to the safety of battery is greatly improved, even if because silica-base material under oxygen
Also will not burn.
But the actual application of silicon-based anode also faces many difficult problems, most important of which is that it and meeting during lithium alloyage
The enormousness produced expands and causes self efflorescence so that loses electricity between granule and granule or between granule and collector on electrode and connects
Touch, the cyclical stability of serious infringement electrode and reversible capacity.For this problem, researcher finds through substantial amounts of research,
Build as granule, line pipe or the silicon nanostructure such as nucleocapsid can effectively alleviate the bulk strain of silicon, it is thus achieved that preferably circulation is surely
Qualitative, but build Si-based nanometer material and also face the predicament that cost is high, be difficult to large-scale production.Additionally, silicium cathode self is electric
The poor problem of electronic conductivity is also one of actually used required important problem solved of future trend.
Silica-base material and material with carbon element are combined is to solve silica-base material cycle performance difference and the effective ways of poorly conductive, mesh
Before have been carried out numerous studies, and define a series of patent.CN103904307A disclose a kind of Si-C composite material and
Preparation method and application, slurry amorphous silica powder, graphite, organic carbon source obtained with alcohol solvent, after being dried pelletize
Heat treatment under the conditions of non-oxidizing atmosphere, i.e. can get Si-C composite material.This material silica flour, graphite and cracking carbon are blended in
Together, the most obvious nucleocapsid structure, the silicon in material may be caused to be easy to expose in the electrolytic solution, it is difficult to formed stable
SEI film, and then cause that efficiency for charge-discharge is low, cycle performance of battery is poor.
CN103474667A discloses a kind of Si-C composite material and preparation method thereof, uses nano-silicon to add graphite and mixes
Closing, then CVD is coated with one layer of carbon, then one layer of carbon of liquid phase coating, finally pulverizes and obtains final material.Silicon-carbon prepared by the method
Composite includes nano-silicon/graphite granule, the first carbon coating layer and organic cracking carbon-coating outside interior successively, has excellence
Cycle performance and rate charge-discharge performance.But the method operation complexity, step is more, and equipment needed thereby is the most more, is not suitable for industry
Change.
Summary of the invention
Present invention aims to the deficiencies in the prior art, now provide a kind of and there is higher specific capacity and good
Cycle performance, technique is simple, and equipment needed thereby is less, and cost is relatively low, be suitable for industrialization nucleocapsid structure Si-C composite material and
Preparation method and purposes.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of nucleocapsid structure Si-C composite material, its
Innovative point is: described Si-C composite material is three-decker, and described internal layer is graphite matrix, and described intermediate layer is silica-based cladding
Layer, described outer layer is carbon-coating；
Described graphite matrix is the one kind or two or more combination in micro crystal graphite, carbonaceous mesophase spherules and soft carbon, described graphite
The particle diameter of matrix is 10-30 μm；
Described silica-based clad is a kind in pure silicon powder, silicon monoxide powder or the combination of 2 kinds, described silica-based clad grain
Footpath is 50-1000nm；
Described middle carbon clad is graphitized carbon, amorphous carbon or CNT, and the thickness of described middle carbon clad is
100-1000nm。
Another object of the present invention is the preparation method disclosing a kind of nucleocapsid structure Si-C composite material, and its innovative point exists
In: specifically comprise the following steps that
(1) a certain proportion of silica-based powder and binding agent being dissolved in organic solvent, high speed dispersion is mixed to get slurry；
(2) a certain amount of graphite matrix is put into silicon carbon material and prepare in special purpose device, use noble gas to drain air, open
Stir and be warming up to uniform temperature；
(3) being kept stirring for rotating speed constant, the nozzle that slurry step (1) obtained prepares special purpose device by silicon carbon material is carried out
Spraying, by silica-based powder coated on graphite matrix；
(4) then use one layer of carbon-coating of chemical vapor deposition, be kept stirring for rotating speed constant, temperature is continuously heating to one
Fixed temperature, is passed through gas phase organic carbon source gas heat insulating a period of time；
(5) it is finally cooled to room temperature, shuts down discharging, obtain final nucleocapsid structure Si-C composite material.
Further, in described step (1), silica-based powder is a kind in pure silicon powder, silicon monoxide powder or the group of 2 kinds
Close；Described binding agent is a kind in sodium carboxymethyl cellulose, polyvinyl alcohol or polyvinylpyrrolidone；Described binding agent adds
Mass percent be 2-5%；Described organic solvent is a kind in ethanol, ethylene glycol, isopropanol, acetone, n-butyl alcohol；Described height
Speed dispersion mixing uses high speed dispersor, and described rotating speed is 500-1500rpm, and described rotation time is 0.5-3h, described slurry
Solid content is 10-30%.
Further, the silicon carbon material in described step (2) prepares special purpose device, including Hybrid Heating cavity, stirring paddle,
Rewinding bucket and electric rotating machine；Being provided with heater in described Hybrid Heating cavity, the upper end of described Hybrid Heating cavity sets
Being equipped with a upper cover, described rewinding bucket is arranged on the bottom of Hybrid Heating cavity, and described stirring paddle passes through shaft and electric rotating
Machine is connected, and described electric rotating machine is arranged on the upper end of the upper cover of Hybrid Heating cavity, described on cover be symmetrically arranged with logical
Pore and steam vent, described on cover and be additionally provided with a slurry nozzle and charging aperture, the bottom of described shipping and cavity also sets
It is equipped with a discharging opening.
Further, the graphite matrix in described step (2) is a kind in micro crystal graphite, carbonaceous mesophase spherules or soft carbon
Or combination of more than two kinds, described graphite matrix particle diameter is 10-30 μm, and described graphite matrix and silica-based powder quality are than for 2-5:
1, described noble gas is a kind in nitrogen, argon, helium, neon, and described speed of agitator is 50-300rpm, described intensification speed
Rate 5-20 DEG C/min, 100-200 DEG C of intensification terminal.
Further, described step (4) heating rate is 1-10 DEG C/min, 700-1000 DEG C of described intensification terminal；Described
Gas phase organic carbon source is a kind in methane, ethylene, acetylene, benzene, toluene, styrene, phenol or the combination of at least 2 kinds, described
Flow is 1-5L/min, and described temperature retention time is 1-5h.
The purposes also disclosing a kind of nucleocapsid structure Si-C composite material of the present invention, its innovative point is: described nucleocapsid
Structure Si-C composite material is for manufacturing the lithium battery of nucleocapsid structure Si-C composite material.
Beneficial effects of the present invention is as follows: the present invention uses graphite as matrix, is glued by spraying and binding agent by silica-based powder
Being attached to graphite granule surface, form clad, then use chemical vapour deposition technique to be coated with one layer of carbon again, binding agent also may be used simultaneously
Carbon is generated with pyrolysis.The material structure prepared includes graphite kernel, silica-based clad and outer layer carbon coating layer, this three layers
Nucleocapsid structure can effectively suppress the change in volume of silica-base material in charge and discharge process, increases material conductivity, the preparation of this material
Using custom-designed device, technique is simple, easy to operate, is suitable for industrialization.
Accompanying drawing explanation
Fig. 1 is the structural representation of the nucleocapsid structure Si-C composite material of the present invention；
Fig. 2 is the structural representation that the nucleocapsid structure Si-C composite material of the present invention prepares special purpose device；
Fig. 3 is the surface scan Electronic Speculum figure of the Si-C composite material of embodiment 1
Fig. 4 is the cross-sectional scans Electronic Speculum figure of the Si-C composite material of embodiment 1
Fig. 5 is that the Si-C composite material of embodiment 1 is as button cell loop test figure during negative pole.
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
A kind of nucleocapsid structure Si-C composite material, Si-C composite material is three-decker, and internal layer is graphite matrix 13, middle
Layer is silica-based clad 12, and outer layer is carbon-coating 11.
Silicon carbon material prepares special purpose device, including Hybrid Heating cavity 1, stirring paddle 2, rewinding bucket 8 and electric rotating machine 9；Mixed
Being provided with heater in closing heating cavity 1, the upper end of Hybrid Heating cavity 1 is provided with a upper cover, and rewinding bucket 8 is arranged on mixed
Closing the bottom of heating cavity 1, stirring paddle 2 is connected with electric rotating machine 9 by shaft, and electric rotating machine 9 is arranged on mixing and adds
The upper end of the upper cover of hot cavity 1, above covers and is symmetrically arranged with passage 4 and steam vent 5, above cover and be additionally provided with a pulp spraying
Mouth 3 and charging aperture 6, the bottom of cavity 1 is additionally provided with a discharging opening 7.
Embodiment 1
Prepared by Si-C composite material: silicon monoxide powder and 3g polyvinylpyrrolidone that 100g particle diameter is 200nm are added
In 1000g ethanol, using high speed dispersor to carry out mixing dispersion 1h, rotating speed is 1000rpm, obtains slurry；By 500g average particle
Footpath is that the Delanium of 20 microns is added silicon carbon material prepared in special purpose device by charging aperture 6, opens stirring, and rotating speed is
150rpm, is then passed through argon by blow vent 4 and air vent 5, drains air；Then open heating, heat up with 10 DEG C/min
To 100 DEG C, then the slurry of preparation is sprayed at graphite surface by spraying 3 and is coated with.Then it is warming up to 5 DEG C/min
900 DEG C, being passed through ethylene, flow is 2.5L/min, deposits 3 hours.Finally close heating and gas phase carbon source, treat that temperature is down to room temperature
After from discharging opening 7 discharging collect obtain final Si-C composite material.
Prepared by negative plate: electrode slice is prepared slurry by stirring and then used automatic spray dehydrator to be coated on Copper Foil
Becoming, slurry solvent is deionized water, and conductive agent is Super-p, and binding agent is that carboxymethyl cellulose adds SBR emulsion, activity
Material, conductive agent and binding agent ratio are 8:1:1.
Prepared by battery: button half-cell use lithium sheet as to electrode, in glove box according to anode cover, electrode slice, every
The order of film, lithium sheet, stainless steel gasket, nickel foam and negative electrode casing assembles CR2025 button cell, and electrolyte uses 1mol/L's
LiPF6As electrolyte, solvent is the EC/EMC/DMC of 1:1:1, adds 10%FEC.
Battery testing: use the charging and discharging curve of blue electrical testing button cell, 0.1C rate charge-discharge, blanking voltage
0.005-1.5V。
Preparation Si-C composite material scanning electron microscope (SEM) photograph as shown in Figure 3, owing to silicon monoxide powder diameter is less, it is difficult to
Observe, but it can be seen that graphite granule surface becomes coarse, show that Surface coating has one silica layer and carbon-coating.The cross section of granule
Scanning electron microscope (SEM) photograph as shown in Figure 4, can more be clearly seen that three-decker.
The charging and discharging curve test knot of the button cell that the Si-C composite material of the employing present invention is prepared as negative material
Fruit is as shown in Figure 5, it can be seen that the specific capacity of material is about 550mAh/g, first efficiency about 85.6%, circulates 20 capacity
Conservation rate is close to 98.7%.
Embodiment 2
The silicon monoxide powder of 200nm " the 100g particle diameter be " in embodiment 1 is changed into " 50g particle diameter is 200nm's by embodiment 2
Silicon monoxide powder and 50g particle diameter are the Si powder of 200nm ", other are constant.
Embodiment 3
Embodiment 3 changes the temperature " 900 DEG C " of chemical gaseous phase deposition bag carbon in embodiment 1 into " 700 DEG C ", and other are constant.
Comparative example
Prepared by Si-C composite material: the silicon monoxide powder that 100g particle diameter is 200nm is passed through common chemical vapour deposition technique
Cladding carbon-coating, is warming up to 900 DEG C with 5 DEG C/min, is passed through ethylene, and flow is 2.5L/min, deposits 3 hours.By the sample after bag carbon
Product are mixed by VC mixer with the Delanium that 500g mean diameter is 20 microns, obtain final Si-C composite material.Negative
Prepared by pole piece, battery is prepared consistent with embodiment 1 with battery testing.
Si-C composite material button electricity relevant parameter prepared by embodiment 1-3 and comparative example is as shown in table 1:
Table 1
The present invention uses graphite as matrix, by spraying and binding agent, silica-based powder is sticked to graphite granule surface, is formed
Clad, then uses chemical vapour deposition technique to be coated with one layer of carbon again, and binding agent can also be pyrolyzed generation carbon simultaneously.Prepare
Material structure include graphite kernel, silica-based clad and outer layer carbon coating layer, this three-layer nuclear shell structure can effectively suppress to fill
The change in volume of silica-base material in discharge process, increases material conductivity, and the preparation of this material uses custom-designed device, work
Skill is simple, easy to operate, is suitable for industrialization.
Above-described embodiment is presently preferred embodiments of the present invention, is not the restriction to technical solution of the present invention, as long as
The technical scheme that can realize on the basis of above-described embodiment without creative work, is regarded as falling into patent of the present invention
Rights protection in the range of.Above-described embodiment is presently preferred embodiments of the present invention, is not the limit to technical solution of the present invention
System, as long as the technical scheme that can realize on the basis of above-described embodiment without creative work, is regarded as falling into
In the range of the rights protection of patent of the present invention.
Claims (7)
1. a nucleocapsid structure Si-C composite material, it is characterised in that: described Si-C composite material is three-decker, described internal layer
For graphite matrix, described intermediate layer is silica-based clad, and described outer layer is carbon-coating；
Described graphite matrix is the one kind or two or more combination in micro crystal graphite, carbonaceous mesophase spherules and soft carbon, described graphite
The particle diameter of matrix is 10-30 μm；
Described silica-based clad is a kind in pure silicon powder, silicon monoxide powder or the combination of 2 kinds, described silica-based clad grain
Footpath is 50-1000nm；
Described middle carbon clad is graphitized carbon, amorphous carbon or CNT, and the thickness of described middle carbon clad is
100-1000nm。
2. the preparation method of a nucleocapsid structure Si-C composite material as claimed in claim 1, it is characterised in that: concrete steps
As follows:
A certain proportion of silica-based powder and binding agent being dissolved in organic solvent, high speed dispersion is mixed to get slurry；
A certain amount of graphite matrix being put into silicon carbon material and prepares in special purpose device, use noble gas to drain air, unlatching is stirred
Mix and be warming up to uniform temperature；
It is kept stirring for rotating speed constant, the nozzle that the slurry that step (1) obtains prepares special purpose device by silicon carbon material is sprayed
Mist, by silica-based powder coated on graphite matrix；
Then use one layer of carbon-coating of chemical vapor deposition, be kept stirring for rotating speed constant, temperature is continuously heating to necessarily
Temperature, is passed through gas phase organic carbon source gas heat insulating a period of time；
It is finally cooled to room temperature, shuts down discharging, obtain final nucleocapsid structure Si-C composite material.
The preparation method of a kind of nucleocapsid structure Si-C composite material the most according to claim 2, it is characterised in that: described step
Suddenly a kind during silica-based powder is pure silicon powder, silicon monoxide powder in (1) or the combination of 2 kinds；Described binding agent is that carboxymethyl is fine
In dimension element sodium, polyvinyl alcohol or polyvinylpyrrolidone a kind；The mass percent that described binding agent adds is 2-5%；Described
Organic solvent is a kind in ethanol, ethylene glycol, isopropanol, acetone, n-butyl alcohol；The mixing of described high speed dispersion uses high speed dispersion
Machine, described rotating speed is 500-1500rpm, and described rotation time is 0.5-3h, and described slurry solid content is 10-30%.
The preparation method of a kind of nucleocapsid structure Si-C composite material the most according to claim 2, it is characterised in that: described step
Suddenly the silicon carbon material in (2) prepares special purpose device, including Hybrid Heating cavity, stirring paddle, rewinding bucket and electric rotating machine；Described mixed
Being provided with heater in closing heating cavity, the upper end of described Hybrid Heating cavity is provided with a upper cover, and described rewinding bucket sets
Putting the bottom at Hybrid Heating cavity, described stirring paddle is connected with electric rotating machine by shaft, and described electric rotating machine sets
Put the upper end of upper cover at Hybrid Heating cavity, described on cover and be symmetrically arranged with passage and steam vent, described on cover
Being additionally provided with a slurry nozzle and charging aperture, the bottom of described shipping and cavity is additionally provided with a discharging opening.
The preparation method of a kind of nucleocapsid structure Si-C composite material the most according to claim 2, it is characterised in that: described step
Suddenly the one kind or two or more combination during the graphite matrix in (2) is micro crystal graphite, carbonaceous mesophase spherules or soft carbon, described graphite
Matrix particle diameter is 10-30 μm, and described graphite matrix and silica-based powder quality are than for 2-5:1, and described noble gas is nitrogen, argon
In gas, helium, neon a kind, described speed of agitator is 50-300rpm, described heating rate 5-20 DEG C/min, intensification terminal
100-200℃。
The preparation method of a kind of nucleocapsid structure Si-C composite material the most according to claim 2, it is characterised in that: described step
Suddenly (4) heating rate is 1-10 DEG C/min, 700-1000 DEG C of described intensification terminal；Described gas phase organic carbon source be methane, ethylene,
In acetylene, benzene, toluene, styrene, phenol a kind or the combination of at least 2 kinds, described flow is 1-5L/min, described insulation
Time is 1-5h.
7. the purposes of a nucleocapsid structure Si-C composite material as claimed in claim 1, it is characterised in that: described nucleocapsid structure
Si-C composite material is for manufacturing the lithium battery of nucleocapsid structure Si-C composite material.
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