CN108428879A - A kind of preparation method and application of New Type of Carbon silicon based composite material - Google Patents
A kind of preparation method and application of New Type of Carbon silicon based composite material Download PDFInfo
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- CN108428879A CN108428879A CN201810293139.8A CN201810293139A CN108428879A CN 108428879 A CN108428879 A CN 108428879A CN 201810293139 A CN201810293139 A CN 201810293139A CN 108428879 A CN108428879 A CN 108428879A
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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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- 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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 kind of preparation method and applications of New Type of Carbon silicon based composite material, sucrose is combined with silica flour, 8~12h of preliminarily dried at room temperature, then under the conditions of nitrogen atmosphere 2~3h is calcined in 773~1473K, obtain primary carbon-silicon composite material, primary carbon-silicon composite material is combined with graphite fibre, obtains carbon silicon based composite material.The preparation method of the present invention is at low cost, easy to operate, raw material sources are extensive, is generated without toxic gas in preparation process, and the carbon silicon based composite material prepared is stablized in lithium cell cathode material using upper performance, excellent cycle performance is shown, there is good prospects for commercial application.
Description
Technical field
The invention belongs to lithium ion battery material technical field, more particularly to a kind of preparation of New Type of Carbon silicon based composite material
Method and application.
Background technology
Commercial li-ion cell negative electrode material is usually the main force that current graphite material is still negative material field.Stone
The material category of ink material is more, includes the Carbon Materials (having graphite-structure) of natural flake graphite, electrographite and threadiness
Deng.Non- reproducible natural flake graphite has natural graphite-structure degree can be directly as lithium ion by high-temperature process
Cell negative electrode material.Electrographite is prepared generally using natural flake graphite as aggregate, in conjunction with other materials through heat pressing process.
By recycling for a long time, natural flake graphite, electrographite lithium storage content be typically maintained in~320mAh/g；By improving
The lithium storage content of processed graphite material can in a short time, to a certain extent close to theoretical capacity level (372mAh/g；
LiC6).Compared with graphite material, fibrous Carbon Materials have potential advantage.Carbon fibe is fibrous carbon material, chemistry
Carbon element content is 90% or more in constituent.Carbon fibe have higher specific modulus, high heat conduction/electricity rate, it is corrosion-resistant, resist it is compacted
The advantages that change, low coefficient of thermal expansion, can not only be used as structural material, but also can be used as functional material, be widely used in automobile
The fields such as manufacture, bridge construction, style entertainment product.
With the development of science and technology, the specific capacity that ordinary graphite negative material can be provided cannot meet electrical source of power,
The demand of electronic product etc., and commercial graphite material be using non-reproducible natural flake graphite as main raw material(s) prepares and
At, necessarily face the problem of graphite resource exhaustion, so be badly in need of with height ratio capacity negative material appearance.Negative material
In, the materials such as silicon, germanium, tin also have higher theoretical lithium storage content.Wherein silicon materials have high lithium specific capacity embedding for the first time,
Theoretical calculation numerical value is up to 4200mAh/g, and at room temperature still up to 3500mAh/g, this can meet electronic product etc. pair well
The requirement of ion battery.But during alloying-removal alloying, violent volume change occurs for silicon materials, causes silicon negative
The destruction of pole material structure, and electrical contact failure, to reduce its cycle life and specific capacity.
Quickly update in face of consumer-elcetronics devices and electric vehicle to extend course continuation mileage requirement, compel to be essential
The energy density of battery is significantly promoted, therefore there is an urgent need for develop new heavy-duty battery.It is close to develop high-energy density, high power
It spends and the lithium ion battery of long life is to developing portable electronic device and electric vehicle with important application meaning, and incite somebody to action
Carbon Materials organically combine with silicon materials material, learn from other's strong points to offset one's weaknesses.Not only the expansion-contraction effect of silicon had been alleviated, but also has improved material
Expect whole electric conductivity, to improve the cycle life and height ratio capacity of electrode material, meets and be used as negative electrode of lithium ion battery material
That expects is inherently required, is expected to surmount the performance of graphite cathode material, becomes lithium ion battery negative material of new generation, but existing
Other novel cathode material for lithium ion batteries such as silicon substrate, majority prepared using harsh, highly difficult nanotechnology, yield compared with
It is low, it not yet realizes and commercially produces.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of preparation sides of New Type of Carbon silicon based composite material
Method, and the New Type of Carbon silicon based composite material of preparation is applied in lithium ion battery.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of New Type of Carbon silicon based composite material, includes the following steps：
S1, sucrose is added in distilled water, obtains aqueous sucrose solution；
S2, silica flour is added in the aqueous sucrose solution that S1 is obtained, ultrasonic disperse is uniform, stirs 12~20h, at room temperature
8~12h of preliminarily dried, obtains reactant, wherein the mass ratio of sucrose is 1 in the silica flour and S1 used in S2:8~20；
S3, the reactant for obtaining S2 under the conditions of protective atmosphere under 773~1473K calcine 2~3h, it is washed, from
After the heart, dry 8~12h, obtains primary carbon-silicon composite at 353K~373K；
S4, graphite fibre being added in primary carbon-silicon composite that S3 is obtained, ultrasonic disperse is uniform, stirring 4~
8h, it is dry, obtain carbon silicon based composite material, wherein the mass ratio of the primary carbon-silicon composite and graphite fibre is 1:
0.5~3.
Preferably, in S4, graphite fibre is prepared by the following procedure method and is prepared：Using pitch as raw material, melt spinning is used
Method prepares pitch-based fiber, then under hot-air atmosphere in 523K handle 30min, then under atmosphere of inert gases in
1273K is sintered 15min, is finally heat-treated 15min in graphitization temperature 3073K to get fine to graphite under atmosphere of inert gases
Dimension.
Preferably, in S1, a concentration of 0.005~0.04g/mL of sucrose in aqueous sucrose solution.
Preferably, in S3, protective gas is high pure nitrogen.
Preferably, in S4, the mass ratio of primary carbon-silicon composite and graphite fibre is 2:1.
Another technical solution of the present invention be to provide New Type of Carbon silicon based composite material prepared by a kind of above method lithium from
Application in sub- cell negative electrode material.
Compared with prior art, the invention has the advantages that：
(1) present invention combines silica flour with sucrose is prepared preliminary composite using high temperature sintering methods, former
Material cost is relatively low, and nano silicon particles derive from a wealth of sources, the rich content in the earth's crust.Sucrose Sources are extensive, and market purchasing is non-
It is often convenient, and preparation method is easy, is advantageously implemented the cost effective of product.
(2) material asphalt of graphite fibre can be artificial synthesized in the present invention, avoids the limitation of nonrenewable resources, raw material
Can continually, the added value of raisingization byproduct improves the economic well-being of workers and staff of chemical enterprise.
(3) graphite fibre in the present invention in the carbon silicon based composite material for preparing has excellent degree of graphitization, excellent
Microstructure, can effectively store/discharge lithium ion, can be used as effective reinforcing material of negative material, can be effective
Cooperate with storage/release lithium ion.
(4) carbon silicon based composite material prepared by the present invention is as lithium ion battery negative material, in 50mA/g current densities
Under, reversible capacity reaches 900mAh/g for the first time, and after recycling 20 times, reversible capacity remains within 1000mAh/g, in cyclic process
Performance is stablized, and excellent cycle performance is shown.
(5) there are not the hazardous substances such as toxic gas in preparation process of the invention, meet green, environmentally friendly, sustainable
Demand for development.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of carbon silicon based composite material.
Fig. 2 is carbon silicon based composite material first charge-discharge curve graph under 50mA/g current densities.
Fig. 3 is the chemical property curve graph that carbon silicon based composite material recycles 20 times under 50mA/g current densities.
Specific implementation mode
The specific implementation mode of invention is described in detail below, it is to be understood that protection scope of the present invention not by
The limitation of specific implementation mode.The test method of actual conditions is not specified in the following example, usually according to normal condition, or
According to the condition proposed by each manufacturer.
Graphite fibre in following embodiment is prepared by following specific steps：
Using pitch as raw material, pitch-based fiber is prepared with melt spinning method, by the pitch-based fiber being prepared in heat
30min is handled in 523K under air atmosphere, then 15min is sintered in 1273K under an argon atmosphere, finally in inert argon body atmosphere
In graphitization temperature 3073K heat treatment 15min to get to graphite fibre under enclosing.
Embodiment 1
A kind of preparation method of New Type of Carbon silicon based composite material, is as follows：
S1,8g sucrose is added in 200mL distilled water, obtains the aqueous sucrose solution of a concentration of 0.04g/mL；
In the aqueous sucrose solution that S2, the S1 that 0.1g silica flours are added to 20mL are obtained, ultrasonic disperse is uniform, will be scattered
Solution is placed in porcelain boat, stirs 12h, preliminarily dried 8h, obtains reactant at room temperature；
S3, the reactant that S2 is obtained calcined to 2h under high pure nitrogen atmosphere in tube furnace under 1173K, it is washed, from
After the heart, 8h is dried under 373K in vacuum drying chamber, obtains primary carbon-silicon composite；
S4,0.1g graphite fibres are added in 0.1g primary carbon-silicon composite that S3 is obtained, are surpassed in ethanol solution
Sound is uniformly dispersed, and stirs 4h, dries 6h at room temperature, obtains carbon silicon based composite material.
Embodiment 2
A kind of preparation method of New Type of Carbon silicon based composite material, is as follows：
S1,3.2g sucrose is added in 200mL distilled water, obtains the aqueous sucrose solution of a concentration of 0.016g/mL；
In the aqueous sucrose solution that S2, the S1 that 0.1g silica flours are added to 50mL are obtained, ultrasonic disperse is uniform, will be scattered
Solution is placed in porcelain boat, stirs 15h, preliminarily dried 12h, obtains reactant at room temperature；
S3, the reactant that S2 is obtained calcined to 2.5h under high pure nitrogen atmosphere in tube furnace under 1123K, washed,
After centrifugation, 10h is dried under 373K in vacuum drying chamber, obtains primary carbon-silicon composite；
S4,0.12g graphite fibres are added in 0.24g primary carbon-silicon composite that S3 is obtained, in ethanol solution
Ultrasonic disperse is uniform, stirs 11h, dries 10h at room temperature, obtains carbon silicon based composite material.
Embodiment 3
A kind of preparation method of New Type of Carbon silicon based composite material, is as follows：
S1,6g sucrose is added in 300ml distilled water, obtains the aqueous sucrose solution of a concentration of 0.02g/mL；
In the aqueous sucrose solution that S2, the S1 that 0.1g silica flours are added to 80mL are obtained, ultrasonic disperse is equal in ethanol solution
It is even, scattered solution is placed in porcelain boat, stirs 12h, preliminarily dried 8h, obtains reactant at room temperature；
S3, the reactant that S2 is obtained calcined to 2h under high pure nitrogen atmosphere in tube furnace under 1273K, it is washed, from
After the heart, 12h is dried under 363K in vacuum drying chamber, obtains primary carbon-silicon composite；
S4,0.6g graphite fibres being added in 0.3g primary carbon-silicon composite that S3 is obtained, ultrasonic disperse is uniform,
10h is stirred, drying at room temperature 10h obtains carbon silicon based composite material.
Embodiment 4
A kind of preparation method of New Type of Carbon silicon based composite material, is as follows：
S1,4g sucrose is added in 800ml distilled water, obtains the aqueous sucrose solution of a concentration of 0.005g/mL；
In the aqueous sucrose solution that S2, the S1 that 0.1g silica flours are added to 400mL are obtained, ultrasonic disperse is uniform, will be scattered
Solution be placed in porcelain boat, stir 12h, preliminarily dried 12h, obtains reactant at room temperature；
S3, the reactant that S2 is obtained calcined to 2.6h under high pure nitrogen atmosphere in tube furnace under 1273K, washed,
After centrifugation, 9h is dried under 353K in vacuum drying chamber, obtains primary carbon-silicon composite；
S4,0.75g graphite fibres are added in 0.25g primary carbon-silicon composite that S3 is obtained, ultrasonic disperse is equal
It is even, 9h is stirred, drying at room temperature 10h obtains carbon silicon based composite material.
We carry out pattern and Electrochemical Properties by taking embodiment 2 as an example, to the New Type of Carbon silicon based composite material of preparation
Fig. 1 is the transmission electron microscope picture of carbon silicon based composite material.From figure 1 it appears that the deeper part of color is in figure
Nano silicon particles, the shallower and part with certain transparency of silicon particle surface color is carbon-coating, and therefore, Fig. 1 shows by forging
Firing technique has obtained the composite material of carbon-coating coated Si.
Electrochemical property test
By carbon silicon based composite material, carbon black, binder according to 7：2：It is ground after 1 quality proportioning mixing, obtains electricity
Electrode material coater is coated on copper foil by pole material, and 373K dries 10h in vacuum drying chamber, and it is negative to obtain carbon silicon substrate
Pole material, using prepared carbon silicon based anode material as working electrode in glove box, lithium piece is to electrode, 1M LiPF6(1:
1:Ethylene carbonate, dimethyl carbonate and the diethyl carbonate of 1 volume ratio are mixed solvent) it is electrolyte, Celgard 2500
For diaphragm, it is assembled into the button cell of CR2025 models jointly.
Fig. 2 is carbon silicon based composite material first charge-discharge curve graph under 50mA/g current densities.It can from Fig. 2
Go out, discharge capacity is 1300mAh/g for the first time, and initial charge capacity is 900mAh/g.
Fig. 3 is the chemical property curve graph that carbon silicon based composite material recycles 20 times under 50mA/g current densities.From Fig. 3
In as can be seen that cycle 20 times after, reversible capacity is still maintained at 900mAh/g, capacity retention ratio 100%, cyclic process
Middle performance is stablized, and excellent cycle performance is shown, and is found in addition, further measuring, and the capacity in cyclic process than battery does not have
Have downward trend, there is ascendant trend by a small margin instead, show the material have stronger high power capacity play potential, have compared with
Good cycle performance.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, since the step method of use is identical as embodiment,
It repeats in order to prevent, the present invention describes preferred embodiment and its effect, and once a person skilled in the art knows bases
This creative concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of preparation method of New Type of Carbon silicon based composite material, which is characterized in that include the following steps：
S1, sucrose is added in distilled water, obtains aqueous sucrose solution；
S2, silica flour is added in the aqueous sucrose solution that S1 is obtained, ultrasonic disperse is uniform, stirs 12~20h, at room temperature tentatively
Dry 8~12h, obtains reactant, wherein the mass ratio of sucrose is 1 in the silica flour and S1 used in S2:8~20；
S3, the reactant for obtaining S2 calcine 2~3h under the conditions of protective atmosphere under 773~1473K, after washed, centrifugation,
Dry 8~12h, obtains primary carbon-silicon composite at 353K~373K；
S4, graphite fibre is added in primary carbon-silicon composite that S3 is obtained, ultrasonic disperse is uniform, stirs 4~8h, does
It is dry, obtain carbon silicon based composite material, wherein the mass ratio of the primary carbon-silicon composite and graphite fibre is 1:0.5~
3。
2. a kind of preparation method of New Type of Carbon silicon based composite material according to claim 1, which is characterized in that in S4, institute
It states graphite fibre method is prepared by the following procedure and be prepared：Using pitch as raw material, pitch-based fiber is prepared with melt spinning method,
Then 30min is handled in 523K under hot-air atmosphere, is then sintered 15min in 1273K under atmosphere of inert gases, finally exists
In graphitization temperature 3073K heat treatment 15min to get to graphite fibre under atmosphere of inert gases.
3. a kind of preparation method of New Type of Carbon silicon based composite material according to claim 2, which is characterized in that the inertia
Atmosphere is argon gas atmosphere.
4. a kind of preparation method of New Type of Carbon silicon based composite material according to claim 1, which is characterized in that in S1, institute
State a concentration of 0.005~0.04g/mL of sucrose in aqueous sucrose solution.
5. a kind of preparation method of New Type of Carbon silicon based composite material according to claim 1, which is characterized in that in S3, institute
It is high pure nitrogen to state protective gas.
6. a kind of preparation method of New Type of Carbon silicon based composite material according to claim 1, which is characterized in that in S4, institute
The mass ratio for stating primary carbon-silicon composite and graphite fibre is 2:1.
7. the New Type of Carbon silicon based composite material prepared by any one of claim 1~6 method is in lithium ion battery negative material
Application.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022000589A1 (en) * | 2020-06-29 | 2022-01-06 | 瑞声声学科技(深圳)有限公司 | Method for preparing silicon-based composite negative electrode material |
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