CN106920938A - Silicon-carbon composite material and preparation method thereof - Google Patents
Silicon-carbon composite material and preparation method thereof Download PDFInfo
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- CN106920938A CN106920938A CN201710201993.2A CN201710201993A CN106920938A CN 106920938 A CN106920938 A CN 106920938A CN 201710201993 A CN201710201993 A CN 201710201993A CN 106920938 A CN106920938 A CN 106920938A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/023—Preparation by reduction of silica or free silica-containing material
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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
- 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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- 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 belongs to the technical field of silicon-carbon composite materials, and particularly relates to a silicon-carbon composite material and a preparation method thereof, wherein the silicon-carbon composite material comprises porous silicon and porous carbon, the mass part ratio of the porous silicon to the porous carbon is 4:1-1:4, and the particle size of the silicon-carbon composite material is 3-5 nm. The silicon carbide composite material is formed by mixing the porous silicon and porous carbon according to the mass ratio, ball-milling the mixture by a ball mill under the protection of inert gas to form a mixture, sintering the mixture in a carbonization furnace and grinding the mixture. The carbon-silicon composite negative electrode material for the lithium ion battery is prepared by sintering porous carbon and porous silicon prepared by a specific process as raw materials, so that the carbon and the silicon are uniformly distributed and combined more tightly, and the composite material has high conductivity and good cycling stability when being used for the lithium ion battery, so that the lithium ion battery has high specific capacity and long service life.
Description
Technical field
The invention belongs to Si-C composite material technical field, and in particular to a kind of Si-C composite material and preparation method thereof.
Background technology
Lithium ion battery as a kind of new electrochmical power source, because its output voltage is high, specific energy is high, have extended cycle life,
Self discharge is small, safety, memory-less effect and environment-friendly turned into the weight that our times various countries develop in new energy materialses field
Point.Electrode material is the principal element for influenceing battery performance and cost, and development of the research and development electrode material to lithium battery has
Significance.
At present, commercial li-ion battery typically uses carbonaceous mesophase spherules and modified graphite as negative material, but exists
Theoretical capacity is relatively low (graphite is 372mAh/g), it is easy to the shortcomings of organic solvent is embedded in altogether, it is impossible to meet growing high energy
The demand of Portable power source is measured, therefore the research of cathode material for high capacity lithium ion battery has turned into raising battery with application
The key of performance.
In known lithium ion battery negative material, silicon has highest theoretical capacity 4200mAh/g, and appropriate
Removal lithium embedded current potential (0.1-0.5Vvs.Li/Li+), but its in charge and discharge process due to volumetric expansion easily cause structure destruction, hold
Amount sharp-decay.In order to alleviate the bulk effect of silicon, the method such as researcher is modified to silicium cathode material, adulterates, being combined,
Such as Si-Ni alloys, Cu5Si alloys, CrSi2Alloy, Si-TiN composites, SiCN composites etc., obtain on cycle performance
Certain improvement but still not ideal enough.
Recent study personnel have carried out a series of study on the modification to silicon based anode material, including nanosizing to silicon,
With carbon-coating coated Si and silicon alloy composite etc. is prepared, but the cycle performance of silicium cathode material is not fundamentally improved.
The content of the invention
A kind of Si-C composite material and preparation method thereof is provided it is an object of the invention to solve above-mentioned technical problem,
The negative material prepared using the material, with good electric conductivity and cyclical stability.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of Si-C composite material, including porous silicon and porous carbon, the porous silicon, the quality parts ratio of porous carbon are 4:1-
1:4, the particle diameter of the Si-C composite material is 3-5nm.
A kind of preparation method of Si-C composite material, after being mixed in mass ratio with porous carbon by the porous silicon, in inertia
Under gas shield after ball mill ball milling forms compound, ground after being sintered in carbide furnace and formed.
The rotating speed of the ball mill is 800-850r/min rotating speed ball milling 8-10h, obtains the compound；
The compound is put into carbide furnace, 1200- is risen to 12-15 DEG C/min heating rates in the carbide furnace
1400 DEG C, carbonization treatment 3-4h is cooled to the polished prepared cellular carbon silicon composite cathode material of room temperature.
The rotating speed of the ball mill is 830r/min rotating speed ball milling 9h, obtains the compound；
The compound is put into carbide furnace, 1300 DEG C, carbon are risen to 13 DEG C/min heating rates in the carbide furnace
Change treatment 3h, be cooled to the polished prepared cellular carbon silicon composite cathode material of room temperature.
The preparation method of the porous silicon is as follows：
It is 1 by mol ratio：3∶3∶2-1：5: 5: 3 nano silica fume, absolute ethyl alcohol, deionized water and ammoniacal liquor are by mixing
Obtain solution A；By tetraethyl orthosilicate in molar ratio 1:5-1:6 are dispersed in absolute ethyl alcohol and stir, and obtain solution B, will be molten
Liquid A and solution B by volume 1:4-1:6 are sufficiently mixed, and are stirred 16-18 hours under constant temperature, and generation includes the titanium dioxide of nano-silicon
Silicon microballoon colloidal sol, by silicon dioxide microsphere colloidal sol the organic formwork containing cetyl trimethylammonium bromide ethylene glycol solution
Middle pyrolysis, prepares porous silica, will obtain porous silica filter, centrifugation, cleaning, dries, then in atmosphere
Carry out being heat-treated for 2 hours at a temperature of 800-900 DEG C, obtain porous silica；
By porous silica and nanometer aluminium powder in mass ratio 1:4-4:1 mixing 700-750r/min rotating speed ball milling mixings 8-
9h, is immersed into concentration in 1-3.5mol/L hydrochloric acid, the relatively complete use for falling reactive aluminum of hydrochloric acid by the mixing material after ball milling
Amount adds 10-15%, and 5-6h is stirred in a kettle., is cleaned to pH more than or equal to 6 with deionized water after filtering, in 140-
Dried at 150 DEG C, cellular silicon is obtained.
The preparation method of the porous carbon is as follows：
By 1: phenolic resin and ethylene glycol mixing and stirring are subsequently added phenolic resin and second by 3-1: 5 weight ratio
The benzene sulfonyl chloride of glycol gross weight 10-12% is well mixed to be made mixture, mixture is poured into mould, at 70-80 DEG C
Lower insulation 1-1.5h, by the sample demoulding after just solidification, carries out deeply-curing treatment, in 60-80 DEG C of initial temperature to sample
Insulation 10-12h, then temperature often increases by 20 DEG C of insulation 3-4h, until temperature rises to 200-250 DEG C is incubated 4~9h again, in N2Protect
It is carbonized under shield, is risen to 700 DEG C, be incubated 2h, 3-5 DEG C of heating rate/min is cooled to the furnace room temperature, stopped after completing carbonization
For N2, obtain porous carbon.
The present invention prepare lithium ion battery carbon silicon composite cathode material, employ special process preparation porous carbon and
Porous silicon is sintered as raw material and forms so that carbon silicon is uniformly distributed and combination is more tight, therefore the composite exists
During for lithium ion battery, with electric conductivity and good cyclical stability higher so that lithium ion battery has high
Specific capacity and service life more long.
Specific embodiment
Below, substantive distinguishing features of the invention and advantage are further described with reference to example, but the present invention not office
It is limited to listed embodiment.
Embodiment one
Prepare porous silicon
It is 1 by mol ratio：5: 5: 3 nano silica fumes, absolute ethyl alcohol, deionized water and ammoniacal liquor obtain solution A by mixing；
By tetraethyl orthosilicate in molar ratio 1:6 are dispersed in absolute ethyl alcohol, stir, and obtain solution B, and solution A and solution B are pressed into body
Product compares 1:6 are sufficiently mixed, and are stirred 18 hours under constant temperature, and generation includes the silicon dioxide microsphere colloidal sol of nano-silicon, by silica
Microballoon colloidal sol is pyrolyzed in the ethylene glycol solution of the organic formwork containing cetyl trimethylammonium bromide, prepares porous dioxy
SiClx, the porous silica filter containing template that will be obtained, centrifugation, cleaning, dries, then 900 DEG C of temperature in atmosphere
Template is removed in the heat treatment for carrying out 7 hours under degree, obtains porous silica；Porous silica and nanometer aluminium powder are pressed into quality
Than 1:4 mixing 750r/min rotating speed ball milling mixing 8h, concentration is immersed into in 2.5mol/L hydrochloric acid by the mixing material after ball milling,
15% is added the relatively complete consumption for falling reactive aluminum of hydrochloric acid more, 6h is stirred in a kettle., cleaned with deionized water after filtering
It is more than or equal to 6 to pH, in being dried at 150 DEG C, cellular silicon materials is obtained.
Prepare porous carbon
Phenolic resin and ethylene glycol mixing and stirring are subsequently added phenolic resin and second by 1: 3 weight ratio first
The benzene sulfonyl chloride of glycol gross weight 12% is well mixed to be made mixture, and mixture is poured into mould, is incubated at 70 DEG C
1h, by the sample demoulding after just solidification, deeply-curing treatment is carried out to sample, and 10h, Ran Houwen are incubated in 60 DEG C of initial temperature
Degree often increases by 20 DEG C of insulation 3h, until temperature rises to 250 DEG C is incubated 4h again, in N2It is carbonized under protection, 700 is risen to by room temperature
DEG C, 1h is incubated, heating rate is 3 DEG C/min, and room temperature is cooled to the furnace after completing carbonization, is finally stopped and supplies N2, obtain porous carbon
Material.
Sintering prepares porous carbon/silicon composite
By above-mentioned porous silicon and porous carbon according to mass ratio 4:1 ratio mixing, in ball milling under the protection of inert gas
With 800r/min rotating speed ball milling 10h in tank, compound is obtained, compound is placed with the carbide furnace of inert gas shielding, with
15 DEG C/min heating rates rise to 1400 DEG C, and carbonization treatment 3h is cooled to the polished prepared cellular carbon silicon Compound Negative of room temperature
Pole material.
Embodiment two
Prepare porous silicon
It is 1 by mol ratio：3: 3: 2 nano silica fumes, absolute ethyl alcohol, deionized water and ammoniacal liquor obtain solution A by mixing；
By tetraethyl orthosilicate in molar ratio 1:5 are dispersed in absolute ethyl alcohol, stir, and obtain solution B, and solution A and solution B are pressed into body
Product compares 1:5 are sufficiently mixed, and are stirred 17 hours under constant temperature, and generation includes the silicon dioxide microsphere colloidal sol of nano-silicon, by silica
Microballoon colloidal sol is pyrolyzed in the ethylene glycol solution of the organic formwork containing cetyl trimethylammonium bromide, prepares porous dioxy
SiClx, the porous silica filter containing template that will be obtained, centrifugation, cleaning, dries, then 850 DEG C of temperature in atmosphere
Template is removed in the heat treatment for carrying out 2 hours under degree, obtains porous silica；Porous silica and nanometer aluminium powder are pressed into quality
Than 4:1 mixing 400r/min rotating speed ball milling mixing 5h, concentration is immersed into in 3.5mol/L hydrochloric acid by the mixing material after ball milling,
10% is added the relatively complete consumption for falling reactive aluminum of hydrochloric acid more, 5h is stirred in a kettle., cleaned with deionized water after filtering
It is more than or equal to 6 to pH, in being dried at 150 DEG C, cellular silicon materials is obtained.
Prepare porous carbon
Phenolic resin and ethylene glycol mixing and stirring are subsequently added phenolic resin and second by 1: 5 weight ratio first
The benzene sulfonyl chloride of glycol gross weight 10% is well mixed to be made mixture, and mixture is poured into mould, is incubated at 70 DEG C
1h, by the sample demoulding after just solidification, deeply-curing treatment is carried out to sample, and 10h, Ran Houwen are incubated in 70 DEG C of initial temperature
Degree often increases by 20 DEG C of insulation 3h, until temperature rises to 230 DEG C is incubated 5h again, in N2It is carbonized under protection, 700 is risen to by room temperature
DEG C, 1h is incubated, heating rate is 4 DEG C/min, and room temperature is cooled to the furnace after completing carbonization, is finally stopped and supplies N2, obtain porous carbon
Material.
Sintering prepares porous carbon/silicon composite
By above-mentioned porous silicon and porous carbon according to mass ratio 1:4 ratio mixing, in ball milling under the protection of inert gas
With 800r/min rotating speed ball milling 8h in tank, compound is obtained, compound is placed with the carbide furnace of inert gas shielding, with 15
DEG C/min heating rates rise to 1200 DEG C, carbonization treatment 4h is cooled to the polished prepared cellular carbon silicon composite cathode of room temperature
Material.
Comparative example
1g magnesium powders and 1g SiO 2 powders are fully ground in mortar is well mixed it；0.94g porous carbons are added
Enter in upper step mixed-powder, being fully ground is well mixed three kinds of powder；Three of the above mixed-powder is moved into tube furnace
In, argon gas is passed through, heat, heating-up temperature is 650 DEG C, and the rate of heat addition is 5 DEG C/min, and the reaction time is 6h；After the completion of reaction, treat
Tubular type furnace temperature is cooled to room temperature, takes out product and is added in the hydrochloric acid that concentration is 0.5mol/L, soaks 6h, then use deionized water
Washing, suction filtration repeatedly after 5 times filtrate pH in neutrality；The product that will be obtained is added to the hydrofluoric acid solution that mass fraction is 20%
In, soak time is 2h, be washed with deionized, suction filtration repeatedly after 6 times filtrate pH in neutrality, by 120 DEG C of suction filtration product vacuum
Dry 12h.
By above-described embodiment one, two and comparative example products therefrom and silicon-porous carbon negative pole material and conductive agent, binding agent
Electrode slice is mixed and made into as working electrode, lithium metal is to electrode, the LiF of 1mol/L6/ EC-DMC (volume ratio 1: 1) is electricity
Solution liquid, simulated battery is assembled into argon gas atmosphere glove box.Charge-discharge test is carried out to simulated battery, voltage is 0.01~2V
(vs.Li+/ Li), current density is 100mA/g.
Electric performance test is carried out at being 25 DEG C in test temperature, after tested the material and comparative example of the embodiment one and two
Product compare, specific capacity improve 40-50%, service life improve more than 1.6 times.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of Si-C composite material, it is characterised in that including porous silicon and porous carbon, the porous silicon, the mass parts of porous carbon
Number is than being 4:1-1:4, the particle diameter of the Si-C composite material is 3-5nm.
2. the preparation method of Si-C composite material described in a kind of claim 1, it is characterised in that by the porous silicon and porous carbon
After mixing in mass ratio, after forming compound by ball mill ball milling under inert gas shielding, ground after being sintered in carbide furnace
Mill is formed.
3. the preparation method of Si-C composite material according to claim 2, it is characterised in that the rotating speed of the ball mill is
800-850r/min rotating speed ball milling 8-10h, obtain the compound；
The compound is put into carbide furnace, 1200-1400 is risen to 12-15 DEG C/min heating rates in the carbide furnace
DEG C, carbonization treatment 3-4h is cooled to the polished prepared cellular carbon silicon composite cathode material of room temperature.
4. the preparation method of Si-C composite material according to claim 3, it is characterised in that the rotating speed of the ball mill is
830r/min rotating speed ball milling 9h, obtain the compound；
The compound is put into carbide furnace, 1300 DEG C, at carbonization are risen to 13 DEG C/min heating rates in the carbide furnace
Reason 3h, is cooled to the polished prepared cellular carbon silicon composite cathode material of room temperature.
5. the preparation method of Si-C composite material according to claim 2, it is characterised in that the preparation method of the porous silicon
It is as follows：
It is 1 by mol ratio：3∶3∶2-1：5: 5: 3 nano silica fume, absolute ethyl alcohol, deionized water and ammoniacal liquor are obtained by mixing
Solution A；By tetraethyl orthosilicate in molar ratio 1:5-1:6 are dispersed in absolute ethyl alcohol and stir, and obtain solution B, by solution A with
Solution B by volume 1:4-1:6 are sufficiently mixed, and are stirred 16-18 hours under constant temperature, and generation includes the silicon dioxide microsphere of nano-silicon
Colloidal sol is warm in the ethylene glycol solution of the organic formwork containing cetyl trimethylammonium bromide by silicon dioxide microsphere colloidal sol
Solution, prepares porous silica, will obtain porous silica filter, centrifugation, cleans, drying, then 800- in atmosphere
Carry out being heat-treated for 2 hours at a temperature of 900 DEG C, obtain porous silica；
By porous silica and nanometer aluminium powder in mass ratio 1:4-4:1 mixing 700-7500r/min rotating speed ball milling mixing 8-9h,
Mixing material after ball milling is immersed into concentration in 1-3.5mol/L hydrochloric acid, the relatively complete consumption for falling reactive aluminum of hydrochloric acid is more
10-15% is added, 5-6h is stirred in a kettle., cleaned to pH more than or equal to 6 with deionized water after filtering, in 140-150 DEG C
Lower drying, is obtained cellular silicon.
6. the preparation method of Si-C composite material according to claim 2, it is characterised in that the preparation method of the porous carbon
It is as follows：
By 1: phenolic resin and ethylene glycol mixing and stirring are subsequently added phenolic resin and ethylene glycol by 3-1: 5 weight ratio
The benzene sulfonyl chloride of gross weight 10-12% is well mixed to be made mixture, and mixture is poured into mould, is protected at 70-80 DEG C
Warm 1-1.5h, by the sample demoulding after just solidification, deeply-curing treatment is carried out to sample, is incubated in 60-80 DEG C of initial temperature
10-12h, then temperature often increases by 20 DEG C of insulation 3-4h, until temperature rises to 200-2500 DEG C is incubated 4~9h again, in N2Protection
Under be carbonized, rise to 700 DEG C, be incubated 2h, 3-5 DEG C of heating rate/min cools to room temperature with the furnace, stops supplying after completing carbonization
N2, obtain porous carbon.
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| CN108611509A (en) * | 2018-05-07 | 2018-10-02 | 青海大学 | Porous aluminum carbon composite and preparation method thereof |
| CN108987710A (en) * | 2018-07-19 | 2018-12-11 | 东北大学 | A method of preparing silicon-carbon composite lithium ion battery cathode material |
| CN109065861A (en) * | 2018-08-01 | 2018-12-21 | 桑德集团有限公司 | Asphaltic base porous carbon materials and preparation method thereof, silicon-carbon cathode material and secondary cell |
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| CN109065861A (en) * | 2018-08-01 | 2018-12-21 | 桑德集团有限公司 | Asphaltic base porous carbon materials and preparation method thereof, silicon-carbon cathode material and secondary cell |
| CN114079045A (en) * | 2020-08-14 | 2022-02-22 | 昱瓴新能源科技(浙江)有限公司 | Porous silicon/carbon composite material synthesized in situ by taking porous polymer microspheres as template, preparation method and lithium ion battery |
| CN114079045B (en) * | 2020-08-14 | 2024-03-15 | 上海昱瓴新能源科技有限公司 | Porous silicon/carbon composite material synthesized in situ by taking porous polymer microspheres as templates, preparation method and lithium ion battery |
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Application publication date: 20170704 |