CN106450192A - Silicon/carbon composite material for lithium ion battery and preparation method and application thereof - Google Patents
Silicon/carbon composite material for lithium ion battery and preparation method and application thereof Download PDFInfo
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- CN106450192A CN106450192A CN201610893497.3A CN201610893497A CN106450192A CN 106450192 A CN106450192 A CN 106450192A CN 201610893497 A CN201610893497 A CN 201610893497A CN 106450192 A CN106450192 A CN 106450192A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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 discloses a silicon/carbon composite material for a lithium ion battery and a preparation method and application of the silicon/carbon composite material for the lithium ion battery, and belongs to the field of material science. The preparation method comprises the following steps: firstly, filling silicon powder and template agents in a carbon precursor, when carbon is pyrolyzed, dissolving the template agents, leaving a large number of holes in a carbon matrix, thus making silicon uniformly dispersed in the porous carbon matrix. The composite material is used as a lithium ion battery cathode material, in the process of charging and discharging, the porous structure of the carbon matrix can buffer a stress generated by silicon expansion to prevent active materials shedding from a current collector so as to effectively prolong the cycle life of an electrode; the porous structure in the carbon matrix enlarges the contact surface of an electrolyte and the active materials and shortens the transmission distance of lithium ions to facilitate utilization of active substances. The lithium ion battery prepared by using the silicon/carbon material is high in specific capacity and excellent in cycle and rate performances.
Description
Technical field
The present invention relates to materialogy field, and in particular to a kind of Silicon-carbon composite material for lithium ion battery and preparation method thereof
And application.
Background technology
Lithium ion battery is as with voltage height, energy density is big, good cycle, self discharge amount are little, memory-less effect
Deng outstanding advantages, from the nineties in last century start practical since, be widely used to mobile terminal, digital product and portable
The field such as mobile device, electric automobile and energy-accumulating power station.
Business-like lithium ion battery negative material mainly adopts graphite at present, but its theoretical capacity only has 372mAh/
G, in order to improve the energy density of lithium ion battery further, in addition to properly increasing positive electrode specific capacity, from height ratio capacity
Negative material to replace traditional graphite cathode be also a key measure.
Silicon is so that its specific capacity height (4200mAh/g), intercalation potential be low, raw material sources extensively have become as most application prospect
Negative material.However, silicon has serious bulk effect during embedding de- lithium, alloy is formed when which combines lithium atom
Li4.4During Si, volumetric expansion reaches 300%, and volume contraction occurs after lithium ion is deviate from, and lasting change in volume is easily caused material
Material structural breakdown and electrode material are peeled off from collector, cause the cyclical stability of electrode poor, and seriously limiting its commercialization should
With.In order to alleviate volumetric expansion of the alloy material in charging process, its cyclical stability is improved, prepare the silicon of nanoscale
Grain, or carbon/silicon nano composite material is relatively effective method.
In prior art, after being often simply mixed silica flour with organic carbon source, high-temperature heat treatment prepares silicon-carbon composite wood again
Material, although improve cyclical stability to a certain extent, but the work for being still unavoidable from causing because of the volumetric expansion of silicon
Property the problem that comes off from collector of material, several times circulation Posterior circle performance start rapid decay.
If the patent documentation of CN 103840140A is for a kind of porous carbon-silicon composite material that can be applicable to cathode of lithium battery.
The porous carbon-silicon composite material includes porous carbon and is attached to the silicon grain of the hole wall of the porous carbon, multiple with the porous carbon silicon
The total restatement of condensation material, the porous carbon-silicon composite material includes the silicon of 20-70 weight % and the porous carbon of 80-30 weight %, and
The BET specific surface area of porous carbon-silicon composite material is 50-250m2/ g, pore volume is 0.2-0.6cc/g.The porous carbon silicon is combined
Material has relatively large specific discharge capacity and has good cyclicity.
Content of the invention
The invention provides a kind of preparation method of Silicon-carbon composite material for lithium ion battery, using multiple obtained in the method
Condensation material has the pattern that silicon is dispersed in porous carbon base body, can effectively reduce what silicon was produced when there is bulk effect
Stress, significantly improves active substance efflorescence, obscission that stress change causes, improves the cycle life of lithium ion battery.
A kind of preparation method of Silicon-carbon composite material for lithium ion battery, comprises the following steps：
(1) organic carbon source is dissolved in solvent, obtains organic carbon source solution；
(2) silica flour and template are added in organic carbon source solution and are mixed, after solvent evaporated, obtain silicon-template
Agent-carbon matrix precursor composite；
(3) silicon-template-carbon matrix precursor composite is calcined under non-oxygen atmosphere, obtains silicon-template-pyrolytic carbon
Composite；
(4) silicon-template-pyrolysis carbon composite is placed in acid solution and template agent removing is removed, obtain after cleaning, drying described
Silicon-carbon composite material for lithium ion battery.
The present invention makes organic carbon source uniformly wrap up silica flour and mould by mixing silica flour, template with organic carbon source solution
Plate agent.After calcining, organic carbon source is pyrolyzed into the material with carbon element with electric action, and last pickling removes template, forms carbon base body
Loose structure, now silica flour be dispersed in porous carbon base body.During charging and discharging lithium battery, the porous knot of carbon base body
Structure provides cushion space for silicon volumetric expansion, and improving causes material structure avalanche and electrode material from collection because of lasting change in volume
Peeling phenomenon on fluid.
The organic carbon source be polyvinyl alcohol, sucrose, glucose, polyacrylonitrile, phenolic resin, polrvinyl chloride, Colophonium, three
One or more in poly cyanamid, polypyrrole, polyaniline and polyacrylic acid.
The solvent is the one kind in water, ethanol, acetone, benzene, toluene, hexamethylene, trichloro ethylene, pyridine and tetrahydrofuran
Or it is several.
Preferably, the organic carbon source is glucose or phenolic resin.
By adjusting silica flour and mixing ratio and the granular size of template in preparation process, final porous can be controlled carbon-based
Pore size distribution in body and hole size.Preferably, the particle diameter that the particle diameter of the silica flour is 50-500nm, template is 50-
1000nm.
Silica flour particle diameter is less, and the bulk effect of generation is less, and cycle performance is more excellent；And small particle is conducive to lithium ion
Migration, reduces impedance.But particle diameter is less, cost is higher, and powder body is easily reunited, in order between balance quality and cost
Relation, more preferably, the particle diameter that the particle diameter of silica flour is 100-150nm, template is 100-300nm.
Preferably, the silica flour is 1 with the mass ratio of template:0.1-1.More preferably, the silica flour and template
Mass ratio be 1:1.
Preferably, organic carbon source is 100-2 with the mass ratio of silica flour:1.More preferably, the matter of organic carbon source and silica flour
Amount is than being 10:1.
The template is metal or metal-oxide or nonmetal oxide or metal carbon that is water insoluble but being dissolved in acid
Hydrochlorate.Wherein, metal be ferrum, zinc, aluminum, one or more in magnesium；Metal-oxide is ferrum oxide, magnesium oxide, zinc oxide, oxygen
Change one or more in copper, aluminium oxide, manganese oxide and lead oxide；Nonmetal oxide is silicon dioxide；Metal carbonate is
One or more in magnesium carbonate, Calcium Carbonate, strontium carbonate, brium carbonate, zinc carbonate and ceruse.
Preferably, in step (2), silica flour is added to using ultrasonic disperse 30- in organic carbon source solution with template
45min, stirs solvent evaporated under the conditions of being subsequently placed in 50-70 DEG C.
Ultrasonic disperse ensures the uniform mixing of raw material.Solvent evaporated while stirring under relatively mild temperature conditionss, carbon
Covered effect can be more preferable, more preferably, stirring solvent evaporated under the conditions of 60 DEG C.
In step (3), the non-oxygen atmosphere is nitrogen, argon, one or more in helium.
The temperature of the calcining is 400-1000 DEG C, and temperature retention time is 1-10h.The temperature and time of calcining is organic to ensure
The abundant carbonization of carbon source, more preferably, the temperature of calcining is 600-1000 DEG C.
Next step removes template agent removing for convenience, and the composite after being pyrolyzed carbon is ground forming powder, then soaks
Steeping template is dissolved in acid solution.The acid solution is one or more in hydrochloric acid, sulphuric acid, nitric acid and Fluohydric acid..Enter during immersion
Row stirring can help to the carrying out that reacts.
Present invention also offers obtained in above-mentioned preparation method Silicon-carbon composite material for lithium ion battery, by silicon and porous
Carbon is constituted, and silicon is dispersed in porous carbon base body, and wherein the mass percent of silicon is 5-40%.Its structural representation such as Fig. 1
Shown.Preferably, the mass percent of silicon is 5-30% in the composite of the present invention.
Present invention also offers a kind of lithium ion battery, including negative electrode active material, the negative electrode active material is above-mentioned
Silicon-carbon composite material for lithium ion battery.
The first discharge specific capacity of the button cell for being assembled as negative active core-shell material using the Si-C composite material of the present invention
More than 1200mAh/g is reached, specific discharge capacity is still in more than 800mAh/g after 50 circulations.
The beneficial effect that the present invention possesses：
(1) the inventive method is first dispersed in template and silica flour in carbon matrix precursor, again by template after carbon pyrolysis
Agent is dissolved, and leaves a large amount of holes in carbon base body, and preparation method is simple, it is adaptable to large-scale production.
(2) composite of the present invention is used as lithium ion battery negative material, in charge and discharge process, the porous of carbon base body
Structure can buffer the stress that silicon expansion is produced, and prevent active material from coming off from collector, effectively increase the circulation longevity of electrode
Life；Loose structure in carbon base body expands the contact surface of electrolyte and active material, shortens the transmission range of lithium ion, has
Help the utilization of active substance.
(3) the lithium ion battery specific capacity for being prepared using silicon carbon material of the present invention is high, circulate and high rate performance is excellent.
Description of the drawings
Fig. 1 is Si-C composite material structural representation, and in figure is numbered：1- silica flour, 2- carbon base body, 3- hole.
Fig. 2 is the cycle performance curve of battery obtained in Si-C composite material in embodiment 1.
Specific embodiment
For making those skilled in the art more fully understand technical scheme, with reference to specific embodiment to this
Invention is described in further detail.
Embodiment 1
(1) use deionized water as solvent, prepare the glucose solution that mass fraction is 10%.
(2) weigh 0.5g silica flour respectively and 0.5g calcium carbonate powder is added in 50g glucose solution, wherein silica flour and carbon
The particle diameter of sour calcium powder is 100nm, and then ultrasound makes which be uniformly dispersed in 30 minutes.
(3) dispersion that step (2) is obtained is stirred under the conditions of 60 DEG C, until moisture content is evaporated, obtains a kind of sticky
Thing.This dope is placed in vacuum drying oven and is dried, obtain silico-carbo acid calcium-carbon matrix precursor composite.
(4) silico-carbo acid calcium-carbon matrix precursor composite that step (3) is obtained is placed in quartz boat, is put into tube-type atmosphere furnace
In, be passed through high pure nitrogen, rise to 900 DEG C with the speed of 5 DEG C/min, be incubated 2h, after natural cooling take out, grinding, obtain silicon-
Calcium oxide-carbon composite.
(5) silicon-calcium oxide-carbon composite that step (4) is obtained is added in the hydrochloric acid of 1M, stirring reaction 3h, makes
Calcium oxide fully dissolves, and filters, is washed with deionized water 3 times, has both obtained silicon/porous carbon composite, its structural representation after drying
As shown in Figure 1.
By gained Si-C composite material and conductive agent, binding agent according to 8:1:1 mass ratio mixing, adds solvent to mix this
Compound modulates uniformly slurry.Wherein conductive agent selects Super-P conductive black, and sodium carboxymethyl cellulose selected by binding agent
(CMC) and butadiene-styrene rubber (SBR) mixed system (CMC and SBR mass ratio be 1:1), solvent is deionized water.Slurry is uniform
It is coated on Copper Foil, first 60 DEG C of forced air drying 3h, then 120 DEG C of vacuum drying 12h, obtain battery pole piece.Using metal lithium sheet
As to electrode, using the LiPF of 1M6Solution as electrolyte, solvent be ethylene carbonate (EC)+diethyl carbonate (DEC)+
Dimethyl carbonate (DMC) system (volume ratio 1:1:1).Using 2325 barrier film of Celgard, in the glove box full of high-purity argon gas
In be assembled into CR2032 type button cell.Electrochemical property test is carried out using blue electric tester.
Battery manufactured in the present embodiment, as shown in Figure 2, first discharge specific capacity reaches 1206mAh/g to cyclic curve, first
Coulombic efficiency is 74.5%, and after 50 circulations, specific discharge capacity is 826.7mAh/g.
Embodiment 2
(1) use ethanol as solvent, prepare the phenol resin solution that mass fraction is 5%.
(2) weigh 0.5g silica flour respectively and 0.5g SiO 2 powder is added in 100mL phenol resin solution, wherein silicon
Powder footpath is 100nm, and the particle diameter of silicon dioxide is 200nm, and then ultrasound 30min makes which be uniformly dispersed.
(3) dispersion that step (2) is obtained is stirred under the conditions of 60 DEG C, until solvent is evaporated, obtains a kind of sticky
Thing.This dope is placed in vacuum drying oven and is dried, obtain silicon-silica-carbon forerunner's composite material.
(4) silicon-silica-carbon forerunner's composite material that step (3) is obtained is placed in quartz boat, is put into tubular type atmosphere
In stove, high-purity argon gas being passed through, 800 DEG C are risen to the speed of 5 DEG C/min, be incubated 3h, takes out after natural cooling, grinding, obtain
Silicon-silica-carbon composite.
(5) silicon-silica-carbon composite for obtaining step (4) is added in 5% Fluohydric acid., stirring reaction
2h, makes silicon dioxide fully dissolve, and filters, is washed with deionized water 3 times, has both obtained silicon/porous carbon composite after drying.
Using silicon carbon material manufactured in the present embodiment as negative active core-shell material, the method for button cell is assembled with embodiment 1.
Battery manufactured in the present embodiment, first discharge specific capacity reaches 1220mAh/g, and coulombic efficiency is 80.3%, 50 first
After secondary circulation, specific discharge capacity is 921mAh/g.
Claims (10)
1. a kind of preparation method of Silicon-carbon composite material for lithium ion battery, it is characterised in that comprise the following steps：
(1) organic carbon source is dissolved in solvent, obtains organic carbon source solution；
(2) silica flour and template are added in organic carbon source solution and are mixed, after solvent evaporated, obtain silicon-template-carbon
Forerunner's composite material；
(3) silicon-template-carbon matrix precursor composite is calcined under non-oxygen atmosphere, obtains silicon-template-pyrolytic carbon and be combined
Material；
(4) silicon-template-pyrolysis carbon composite is placed in acid solution and removes template agent removing, cleaning, dry after obtain the lithium from
Sub- battery Si-C composite material.
2. preparation method as claimed in claim 1, it is characterised in that the organic carbon source is glucose or phenolic resin.
3. preparation method as claimed in claim 1, it is characterised in that the particle diameter of the silica flour is 50-500nm, template
Particle diameter is 50-1000nm.
4. preparation method as claimed in claim 1, it is characterised in that the silica flour is 1 with the mass ratio of template:0.1-1.
5. preparation method as claimed in claim 1, it is characterised in that organic carbon source is 100-2 with the mass ratio of silica flour:1.
6. preparation method as claimed in claim 1, it is characterised in that the template is metal that is water insoluble but being dissolved in acid
Or metal-oxide or nonmetal oxide or metal carbonate.
7. preparation method as claimed in claim 1, it is characterised in that in step (2), silica flour is added to organic carbon with template
Using ultrasonic disperse 30-45min in the solution of source, solvent evaporated under the conditions of being subsequently placed in 50-70 DEG C, is stirred.
8. preparation method as claimed in claim 1, it is characterised in that the temperature of the calcining is 400-1000 DEG C, during insulation
Between be 1-10h.
9. Silicon-carbon composite material for lithium ion battery obtained in one kind preparation method described in any one of claim 1-8, which is special
Levy and be, be made up of silicon and porous carbon, silicon is dispersed in porous carbon base body, wherein the mass percent of silicon is 5-40%.
10. a kind of lithium ion battery, including negative electrode active material, it is characterised in that the negative electrode active material be
Described Silicon-carbon composite material for lithium ion battery.
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| CN107528063A (en) * | 2017-08-01 | 2017-12-29 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of core shell structure silicon/carbon material of cornstarch porous carbon encapsulation |
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