CN109524635A - A kind of preparation method and applications of the silicon carbon composite for negative electrode of lithium ion battery - Google Patents
A kind of preparation method and applications of the silicon carbon composite for negative electrode of lithium ion battery Download PDFInfo
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- CN109524635A CN109524635A CN201811077874.1A CN201811077874A CN109524635A CN 109524635 A CN109524635 A CN 109524635A CN 201811077874 A CN201811077874 A CN 201811077874A CN 109524635 A CN109524635 A CN 109524635A
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
A kind of preparation method and applications of the silicon carbon composite for negative electrode of lithium ion battery, are related to field of lithium ion battery.First uniformly disperse the silicon powder of certain mass in hydrocarbon material, then it instills in the reacting furnace for being raised to target temperature in atmosphere of inert gases in advance, the pyrolysis of hydrocarbon material chemical gaseous phase is coated on silicon face and forms clad, and silicon carbon composite is made.The material is the core-shell structure with spherical morphology to have in spherical concentric arrangement of multilayer carbon shell as shell using silicon particle as core, between 0.1-30 μm of diameter.The material uses capacity with higher and good cyclical stability as lithium ion battery negative material.Preparation method provided by the invention have it is easy to operate, quickly and effectively, the advantages that being produced on a large scale.
Description
Technical field
The present invention relates to field of lithium ion battery, in particular to a kind of silicon carbon composite for negative electrode of lithium ion battery
Preparation method.
Background technique
The continuous intensification of social process of industrialization, the needs of to meet sustainable economic development and protection of natural resources and environment,
More stringent requirements are proposed to energy storage device by people, and in numerous energy storage devices, lithium ion battery is close with its excellent energy
Degree and power density are widely used in various portable electronic devices (such as smart phone, laptop and video camera)
With the fields such as communications and transportation (such as electric car), and have extensive market.With the development of society, electronic product is quick
Update and electric vehicle industry rapid development so that people propose higher expectation to lithium ion battery, it is desirable to lithium from
Sub- battery possesses outstanding energy density, power density and cycle life.
Cathode material of lithium ion battery is mostly graphite material currently on the market, but with the development of society, graphite material
Material is not able to satisfy the demand of people's high-energy density, at the same time, some alloys due to low theoretical capacity (about 372mAh/g)
Class material becomes the hot spot of research due to high theoretical capacity and lower de- lithium voltage platform, and wherein silica-base material is considered
It is next-generation lithium ion battery negative material [Wu, Hui, and Yi the Cui. " Designing for being most hopeful to replace conventional graphite
nanostructured Si anodes for high energy lithium ion batteries."Nano Today
7.5(2012):414-429.].As the ion cathode material lithium of a new generation, the theoretical capacity of silicon is 4200mAh/g, is business
About 10 times for changing conventional graphite material, and there is relatively low de- lithium voltage platform to receive significant attention.But simultaneously there is also
Some fatal defective effects its further apply with commercialization, silicon materials application when be primarily present following problems: 1. filling
It is expanded in discharge process along with about 300% enormousness, it is difficult to form stable SEI film, while inevitably cause
The collapsing of electrode structure, breaking and Dusting simultaneously fall off from electrode slice, cause capacity to be decayed rapidly, the circulation for seriously affecting battery is steady
It is qualitative；2. silicon is semiconductor, electric conductivity is poor, causes irreversible degree during lithium ion deintercalation big, to reduce library for the first time
Human relations efficiency, battery cycle life are deteriorated.Silicon materials there are aiming at the problem that, research both domestic and external is concentrated mainly on following side
Face: 1. nanosizing alleviates expansion bring bulk effect, such as nano particle by reducing the size of silicon materials, and nano wire is received
Mitron etc.；2. porous, alleviated using the pore structure of material internal prosperity the volume expansion in charge and discharge process [Du,
Fei-Hu,et al."Surface Binding of Polypyrrole on Porous Silicon Hollow
Nanospheres for Li-Ion Battery Anodes with High Structure Stability."Advanced
materials 26.35(2014):6145-6150.]；3. composite material is prepared, such as the compound core-shell structure of silicon charcoal, yolk egg
[Zhang, Miao, et al. " the Latest development of nanostructured such as shell structure, sandwich structure
Si/C materials for lithium anode studies and applications."Energy Storage
Materials 4 (2016): 1-14.], carbon material has certain mechanical strength and higher electric conductivity, can alleviate silicon material
The expansion of material also can increase the electric conductivity of composite material.
In recent years, it prepares silicon carbon composite to have been a hot spot of research, Jingang Qin et al. passes through high mechanical strength
Silicon particle is coated with the extremely strong graphene sheet layer of electric conductivity, under the current density of 400mA/g, is kept after 200 circle of circulation
Capacity [Qin J, Wu M, Feng T, the et al.High rate capability and long cycling of 660mAh/g
life of graphene-coated silicon composite anodes for lithium ion batteries
[J].Electrochimica Acta,2017,256:259-266.].Inspiration of the Quan Xu et al. by watermelon structure, passes through
By nano silica fume, polyvinylpyrrolidone, glucose sugar, carboxymethyl cellulose etc. stirring after with flake graphite ball milling, it
Afterwards by spray drying, it is multiple up to watermelon shape silicon charcoal in its surface one layer of pyrolytic carbon of deposition that carbonization a period of time reuses CVD method
Condensation material, the material are also able to maintain the reversible capacity of about 500mAh/g by 250 cycle charge-discharges later.[Xu Q,Li J
Y,Sun J K,et al.Watermelon-Inspired Si/C Microspheres with Hierarchical
Buffer Structures for Densely Compacted Lithium-Ion Battery Anodes[J]
.Advanced Energy Materials,2017,7(3):1601481.].But current preparation method process flow is multiple
Miscellaneous, higher cost is unfavorable for industrialized realization.
Summary of the invention
In view of the above problems in the prior art, the object of the present invention is to provide a kind of silicon charcoals for negative electrode of lithium ion battery
Composite material and preparation method.
Silicon carbon composite of the invention, which is characterized in that using several silicon charcoal particles or its aggregation as core, with concentric rows
The multilayer carbon shell of column is the silicon carbon composite of the multi-layer core-shell structure of shell；Corresponding silicon charcoal particle is core-shell structure.Further
Using silicon particle as core, the surface that pyrolysis of hydrocarbons is deposited on silicon particle forms cladding carbon-coating to obtain core-shell structure silicon charcoal
Grain seed, these seeds melt in warm-up movement and are formed aggregation, while continuing in concentric circles in aggregate surface
Pyrolytic carbon layer is deposited as shell, is formed later using several silicon charcoal grain seeds or its aggregation as core, with concentric arrangement of multilayer
Carbon shell is the silicon carbon composite of the multi-layer core-shell structure of shell, and the silicon carbon composite of multi-layer core-shell structure has spherical morphology,
The material diameter be 0.1-30 μm between,
It is made as follows:
Step 1: it disperses the silicon powder of certain mass in liquid hydrocarbonaceous feedstock；
Step 2: taking liquid mixture obtained by step 1, continuously instills dropwise and is raised to the anti-of target temperature in advance
It answers in furnace, is pyrolyzed under an inert atmosphere, subsequent continuation of insurance temperature a period of time is added dropwise to get silicon charcoal composite wood in liquid mixture
Material.
The dosage relation of silicon powder of the present invention and liquid hydrocarbonaceous feedstock there is not limitation substantially, and the present invention is further preferred
Scheme is: every 0.5g silicon powder corresponds to 1-30ml or other higher volume of liquid hydrocarbonaceous feedstocks.
The further preferred embodiment of the present invention is: the silicon powder is having a size of between 10-2000nm.
The further preferred embodiment of the present invention is: the liquid hydrocarbonaceous feedstock be phenolic resin, pyridine, toluene,
One of quinoline, coal tar asphalt, coal tar, asphalt, ethylene bottom oil, mesophase pitch, aromatic hydrocarbons heavy oil or they
Mixture.
The further preferred embodiment of the present invention is: the target temperature is 600-1800 DEG C.
The further preferred embodiment of the present invention is: the soaking time is 0.5-5h.
The further preferred embodiment of the present invention is: the inert atmosphere be hydrogen, nitrogen, helium, neon, argon gas or they
Mixture.
The present invention using high temperature make hydrocarbon material after Pintsch process and heat polymerization to be dispersed in it
In silicon particle be that the poly- surface for being attached to silicon particle of core liquefaction forms clad to obtain core-shell structure silicon charcoal grain seed,
Continue to be added dropwise with raw material, these silicon charcoal grain seeds melt in warm-up movement and and form aggregation, while pyrolytic carbon layer after
It is continuous to be deposited in a manner of nearly concentric circles on its surface, it is formed later using several silicon charcoal particles or its aggregation as core, with concentric rows
The multilayer carbon shell of column is the silicon carbon composite of the multi-layer core-shell structure of shell, and the silicon carbon composite of multi-layer core-shell structure has ball
Shape pattern, the material diameter are between 0.1-30 μm, and preparation process is simple, are suitble to hydrocarbonization in industrialized production and preparation process
It closes object all to complete to coat layer by layer in the gas phase, so that the silicon charcoal compound particle clad is complete, structure is unified, therefore has good
Cyclical stability.
Detailed description of the invention
The scanning electron microscope (SEM) photograph of gained silicon carbon composite at a temperature of attached drawing 1 is 900 DEG C.
Attached drawing 2 is the chemical property curve of silicon carbon composite prepared by case study on implementation 3.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples, but the present invention is not limited to following embodiments.
Embodiment 1
Chemical gas phase reaction furnace is warming up to 900 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 5ml pyridine solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, and 30min is kept the temperature after being added dropwise, system
Obtain silicon carbon composite.According to lithium ion battery negative material button cell test method (active material powder, conduction
Agent, binder according to mass ratio 8:1:1 after evenly mixing, on sized mixing using water painting and copper foil, after dry cut-parts
Constant current charge-discharge test is carried out at button cell as electrode assembling) it is tested.
It is the shape appearance figure for preparing sample as shown in 1 scanning electron microscope of attached drawing (SEM).
The electrode material is under 50mA/g current density, first discharge specific capacity 1008.8mAh/g, charge specific capacity
805.6mAh/g initial coulomb efficiency 79.86%.Under the current density of 200mA/g, first discharge specific capacity 906.8mAh/
G, charge specific capacity 722.9mAh/g, initial coulomb efficiency 79.72%, and after 200 circulations, still have
The reversible capacity of 703.6mAh/g recycles conservation rate 97.3%.
Embodiment 2
Chemical gas phase reaction furnace is warming up to 1000 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 4ml pyridine solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, 30min is kept the temperature after being added dropwise,
Silicon carbon composite is made.Test method is the same as embodiment 1.
The electrode material is under 50mA/g current density, first discharge specific capacity 1063.5mAh/g, charge specific capacity
881.3mAh/g initial coulomb efficiency 82.87%.Under the current density of 200mA/g, first discharge specific capacity 917.0mAh/
G, charge specific capacity 764.5mAh/g, initial coulomb efficiency 83.37%, and after 100 circulations, still have
The reversible capacity of 674.4mAh/g recycles conservation rate 88.2%.
Embodiment 3
Chemical gas phase reaction furnace is warming up to 900 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 3ml pyridine solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, and 30min is kept the temperature after being added dropwise, system
Obtain silicon carbon composite.Test method is the same as embodiment 1.
The electrode material is under the current density of 200mA/g, first discharge specific capacity 2170.5mAh/g, charge specific capacity
1846.0mAh/g, initial coulomb efficiency 85.01%, and after 50 circulations, it is still reversible with 1606.4mAh/g
Capacity, recycles conservation rate 86.99%, and test result is shown in attached drawing 2.
Embodiment 4
Chemical gas phase reaction furnace is warming up to 900 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 20ml benzene solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, and 30min is kept the temperature after being added dropwise, system
Obtain silicon carbon composite.Test method is the same as embodiment 1.
The electrode material is under 50mA/g current density, first discharge specific capacity 673.5mAh/g, charge specific capacity
519.2mAh/g initial coulomb efficiency 77.09%.Under the current density of 200mA/g, first discharge specific capacity 550.7mAh/
G, charge specific capacity 393.2mAh/g, initial coulomb efficiency 71.40%, and after 200 circulations, still have
The reversible capacity of 463.8mAh/g is not decayed substantially with comparing for the first time.
Embodiment 5
Chemical gas phase reaction furnace is warming up to 900 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 20ml asphalt solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, is kept the temperature after being added dropwise
Silicon carbon composite is made in 30min.Test method is the same as embodiment 1.
The electrode material is under 50mA/g current density, first discharge specific capacity 707.2mAh/g, charge specific capacity
507.8mAh/g initial coulomb efficiency 71.80%.Under the current density of 200mA/g, first discharge specific capacity 591.5mAh/
G, charge specific capacity 425.9mAh/g, initial coulomb efficiency 72.72%, and after 200 circulations, still have
The reversible capacity of 420.5mAh/g is not decayed substantially with comparing for the first time.
Embodiment 6
Chemical gas phase reaction furnace is warming up to 900 DEG C in advance in argon atmosphere, disperses 0.5g silicon powder (100nm) in
In 20ml coal-tar solvent, then ultrasonic disperse 30min is instilled chemical gas phase reaction furnace, is kept the temperature after being added dropwise
Silicon carbon composite is made in 30min.Test method is the same as embodiment 1.
The electrode material is under 50mA/g current density, first discharge specific capacity 749.6mAh/g, charge specific capacity
553.0mAh/g initial coulomb efficiency 73.77%.Under the current density of 200mA/g, first discharge specific capacity 697.6mAh/
G, charge specific capacity 509.3mAh/g, initial coulomb efficiency 73.27%, and after 200 circulations, still have
The reversible capacity of 498.5mAh/g is not decayed substantially with comparing for the first time.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent variation or replacement on the premise of without prejudice to spirit of the invention,
These equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (9)
1. a kind of silicon carbon composite, which is characterized in that using several silicon charcoal particles or its aggregation as core, with concentric arrangement of more
Layer carbon shell is the silicon carbon composite of the multi-layer core-shell structure of shell, and corresponding silicon charcoal particle is core-shell structure.
2. a kind of silicon carbon composite described in accordance with the claim 1, which is characterized in that the silicon charcoal composite wood of multi-layer core-shell structure
Material has spherical morphology, which is between 0.1-30 μm.
3. the preparation method of silicon carbon composite of any of claims 1 or 2, which is characterized in that be made as follows:
Step 1: it disperses the silicon powder of certain mass in liquid hydrocarbonaceous feedstock；
Step 2: taking liquid mixture obtained by step 1, continuously instills the reacting furnace for being raised to target temperature in advance dropwise
In, it is pyrolyzed under an inert atmosphere, subsequent continuation of insurance temperature a period of time is added dropwise to get silicon carbon composite in liquid mixture.
4. the preparation method of silicon carbon composite described in accordance with the claim 3, it is characterised in that: the size of the silicon powder is
Between 10-2000nm.
5. the preparation method of silicon carbon composite described in accordance with the claim 3, it is characterised in that: the hydrocarbon material
Selected from phenolic resin, pyridine, toluene, quinoline, coal tar asphalt, coal tar, asphalt, ethylene bottom oil, mesophase pitch, virtue
One of hydrocarbon heavy oil or their mixture.
6. the preparation method of silicon carbon composite described in accordance with the claim 3, it is characterised in that: the target temperature is 600-
1800℃。
7. the preparation method of silicon carbon composite described in accordance with the claim 3, it is characterised in that: the soaking time is 0.5-
5h。
8. the preparation method of silicon carbon composite described in accordance with the claim 3, it is characterised in that: silicon powder and liquid hydrocarbon
The dosage relation of raw material is that every 0.5g silicon powder corresponds to 1-30ml liquid hydrocarbonaceous feedstock.
9. application of the silicon carbon composite of any of claims 1 or 2 as lithium ion battery negative material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| NO20190791A1 (en) * | 2019-06-24 | 2020-12-25 | Inst Energiteknik | Electric energy storage device & method |
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| CN102244240A (en) * | 2011-06-15 | 2011-11-16 | 中南大学 | Lithium ion battery composite anode material and preparation method thereof |
| CN103094533A (en) * | 2012-11-26 | 2013-05-08 | 中南大学 | Multi-core core-shell-structure silicon carbon composite negative pole material and preparation method thereof |
| CN103346293A (en) * | 2013-06-28 | 2013-10-09 | 中国科学院宁波材料技术与工程研究所 | Lithium ion battery cathode material and preparation method thereof as well as lithium ion battery |
| CN106602018A (en) * | 2016-12-21 | 2017-04-26 | 上海杉杉科技有限公司 | Anode material for lithium ion batteries, preparation method and battery containing anode material |
| WO2017099456A1 (en) * | 2015-12-07 | 2017-06-15 | 강원대학교산학협력단 | Negative electrode active material for lithium secondary battery comprising core composed of carbon, manufacturing method therefor, and lithium secondary battery including same |
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| CN102244240A (en) * | 2011-06-15 | 2011-11-16 | 中南大学 | Lithium ion battery composite anode material and preparation method thereof |
| CN103094533A (en) * | 2012-11-26 | 2013-05-08 | 中南大学 | Multi-core core-shell-structure silicon carbon composite negative pole material and preparation method thereof |
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| NO20190791A1 (en) * | 2019-06-24 | 2020-12-25 | Inst Energiteknik | Electric energy storage device & method |
| NO347199B1 (en) * | 2019-06-24 | 2023-07-03 | Inst Energiteknik | Electric energy storage device & method |
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