CN108963201A - A kind of silicon-carbon self-supporting composite negative pole material and the preparation method and application thereof - Google Patents
A kind of silicon-carbon self-supporting composite negative pole material and the preparation method and application thereof Download PDFInfo
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- CN108963201A CN108963201A CN201810522471.7A CN201810522471A CN108963201A CN 108963201 A CN108963201 A CN 108963201A CN 201810522471 A CN201810522471 A CN 201810522471A CN 108963201 A CN108963201 A CN 108963201A
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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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- 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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- 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 present invention relates to a kind of silicon-carbon self-supporting composite negative pole material and the preparation method and application thereof, the silicon on the surface or inside that are attached to carbon fiber supporter by porous carbon fiber supporter and infiltration is formed.The present invention first uses method of electrostatic spinning to prepare the macromolecular fibre shape supporter containing silicon source；Then Fibrous support body is obtained into lithium ion battery silicon-carbon self-supporting composite negative pole material by heat treatment process.Carbon fiber structural can provide conductive network and self-supporting skeleton, make up the low disadvantage of silicon conductivity, and silicon is active material.Silicon self-supporting electrode, which can be removed from, is added adhesive and conductive carbon material, and the three-dimensional network of itself can also provide a large amount of removal lithium embedded channel, have excellent chemical property.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of silicon-carbon self-supporting composite negative pole material and its system
Preparation Method and application.
Background technique
The rapid development of the novel industrial technology such as electric car in recent years, the demand to high-performance power lithium-ion battery
It is more more and more urgent.The improvement of performance of lithium ion battery depends greatly on embedding lithium metal material energy densities and circulation longevity
The raising of life.The theoretical lithium storage content for the graphite-like carbon negative pole material that commercial Li-ion battery is widely used at present is lower (only
Have 372m Ah/g), become the main bottleneck of limiting lithium ion cell energy density.
In recent years, very active to the research of lithium ion battery new electrode materials in the world.Lithium material is stored up in low potential
Material aspect, as silicon, tin, aluminium etc. can cathode made from the metal and its alloy material with lithium alloyage, reversible removal lithium embedded
Amount is far longer than graphite.
In these systems, silicon is increasingly looked steadily because of having the embedding lithium capacity of highest theory (4200m Ah g-1)
Mesh.But there is serious volume expansion under the conditions of high level removal lithium embedded in silica-base material, cause the circulation of electrode steady
Qualitative sharp fall.How to improve bring mechanical instability during embedding de- lithium, makes the material of these storage lithium function admirables
Material tends to the practical key points and difficulties for having become such investigation of materials.
Conventional Si-C composite material is usually prepared by the methods of pyrolysis, mechanical mixture/high-energy ball milling, described multiple
Object is closed to be constituted by inlaying silicon particle in dense carbon matrix.However, the silicon-carbon compound of such method preparation, when in the charge and discharge phase
Between silicon materials structure in be embedded in lithium ion when, be easy to happen structure breaking and powdered, therefore the circulation ability of battery is very
Difference.
In addition, the combination electrode formed with rigid copper current collector layer prior art discloses silicon-carbon active layer is for being similar to
For this lithium ion battery negative material with large volume effect of silicon, in charge and discharge process, silicon-carbon active layer occurs huge
Big volume change not only causes very strong mechanical stress inside active layer, also in silicon-carbon active layer and rigid copper current collector
Mechanical stress is generated between layer, silicon materials dusting is caused to be peeled off, is disengaged between material granule and between coating and copper current collector
Electrical contact is lost, so that charge/discharge capacity sharply declines, battery is quickly invalidated.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of energy density and surely
Qualitative good silicon-carbon self-supporting composite negative pole material and the preparation method and application thereof.
The purpose of the present invention can be achieved through the following technical solutions: a kind of silicon-carbon self-supporting composite negative pole material, should
Material includes carbon skeleton and the silicon powder that is carried in carbon skeleton duct, and the carbon skeleton is in self-supporting fibrous reticular structure,
In, the silicon powder accounts for the 10%~90% of material gross mass.
The present invention loads silicon powder by the carbon skeleton of self-supporting fibrous reticular structure, and the internal gutter of carbon skeleton and surface are all
Silicon powder can be loaded, so comparing general spinning carbon fibre material can the compound silicon compared with weight；Meanwhile except carbon fiber itself
Except elasticity, the volume expansion that the duct inside carbon fiber can also alleviate silicon well is influenced to overall structure bring, is changed
Kind electric conductivity.
The partial size of the silicon powder is 10~150nm.
A kind of preparation method of silicon-carbon self-supporting composite negative pole material as described above, comprising the following steps:
(1) polyacrylonitrile, polystyrene and silicon powder are added into n,N-Dimethylformamide, stirring and dissolving forms transparent
Solution；
(2) clear solution is prepared into the macromolecular fibre shape supporter containing silicon source by method of electrostatic spinning, it is then hot
Processing obtains the silicon-carbon self-supporting composite negative pole material.
Carbon source material of the polyacrylonitrile as electrostatic spinning of the present invention, spinning property is stablized, easily controllable.Polystyrene
As spinning material, not exclusively dissolves each other with polyacrylonitrile, is present in polyacrylonitrile solution with the form stable of drop bead,
And the fusing point of polystyrene is lower, so during heat treatment, polystyrene, which first melts, forms hole channel type cavity.
The mass ratio of the polyacrylonitrile, polystyrene and silicon powder is (0.1~0.9): (0.1~0.5): (0.05~
0.4)。
The stirring and dissolving carries out at a temperature of 60~70 DEG C, and mixing time is greater than 5h.
The process conditions of the method for electrostatic spinning are as follows: the voltage of 10~20KV, and syringe is 8 at a distance from receiving screen
~15cm, receiving screen are metal foil or metal mesh.It is easy to operate that method of electrostatic spinning prepares macromolecular fibre supporter, in spinning work
There are good Equipment Foundations in industry, and has the potentiality of industrial-scale popularization.
The heat treatment at 200~250 DEG C the following steps are included: pre-oxidize 2~4h, then again under an inert atmosphere
500~1200 DEG C are warming up to the heating rate of 3-5 DEG C/min, and keeps the temperature and is greater than 3h.
The inert atmosphere is nitrogen atmosphere.
A kind of application of silicon-carbon self-supporting composite negative pole material as described above, the negative electrode material are used for lithium ion battery anode material
Material.
Compared with prior art, the beneficial effects of the present invention are embodied in: negative electrode material of the invention can either load more
The silicon of weight, and the volume expansion of silicon can be inhibited well, improve electric conductivity, to guarantee electrode slice close with higher-energy
Degree, and electrode slice does not need have more excellent cyclical stability using conductive carbon and binder.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) figure of silicon-carbon self-supporting composite negative pole material in embodiment 3；
Fig. 2 is thermogravimetric (TG) curve graph of embodiment 1-4 and comparative example.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
Use 0.9g polyacrylonitrile for template, 0.5g polystyrene is as pore creating material, 5mL n,N-Dimethylformamide
Solvent is added 0.05g nano silica fume, mixes to solution stable homogeneous, obtain spinning solution.Using electrostatic spinning process,
Spinning solution is spun into containing silicon source fibrous polypropylene nitrile/polystyrene supporter；
To remove containing silicon source fibrous polypropylene nitrile/polystyrene support film monolith, be put into Muffle furnace 250 DEG C it is pre-
Aoxidize 3h；Then 3h is kept the temperature at 1200 DEG C in a nitrogen atmosphere again, heating rate is 3 DEG C/min, obtains silicon-carbon self-supporting electrode.
Its hot weight curve is silicone content 34wt% shown in the 0.05g Si curve in Fig. 2.
Embodiment 2
Use 0.1g polyacrylonitrile for template, 0.1g polystyrene is as pore creating material, 5mL n,N-Dimethylformamide
Solvent is added 0.1g nano silica fume, mixes to solution stable homogeneous, obtain spinning solution.It, will using electrostatic spinning process
Spinning solution is spun into containing silicon source fibrous polypropylene nitrile/polystyrene supporter.
To remove containing silicon source fibrous polypropylene nitrile/polystyrene support film monolith, be put into Muffle furnace 200 DEG C it is pre-
Aoxidize 4h；Then 8h is kept the temperature at 500 DEG C in a nitrogen atmosphere again, heating rate is 4 DEG C/min, obtains silicon-carbon self-supporting electrode.
Its hot weight curve is silicone content 31wt% shown in the 0.1g Si curve in Fig. 2.
Embodiment 3
Use 0.5g polyacrylonitrile for template, 0.3g polystyrene is as pore creating material, 5mL n,N-Dimethylformamide
Solvent is added 0.2g nano silica fume, mixes to solution stable homogeneous, obtain spinning solution.It, will using electrostatic spinning process
Spinning solution is spun into containing silicon source fibrous polypropylene nitrile/polystyrene supporter.
To remove containing silicon source fibrous polypropylene nitrile/polystyrene support film monolith, be put into Muffle furnace 220 DEG C it is pre-
Aoxidize 2h；Then 3h is kept the temperature at 700 DEG C in a nitrogen atmosphere again, heating rate is 5 DEG C/min, obtains silicon-carbon self-supporting electrode.
Its transmission electron microscope picture is as shown in Figure 1, the partial size of its internal gutter is 10nm~30nm.Its hot weight curve is the 0.2g in Fig. 2
Shown in Si curve, silicone content 51wt%.
Embodiment 4
Use 0.75g polyacrylonitrile for template, 0.45g polystyrene is as pore creating material, 7.5mL N, N- dimethyl formyl
Amine is solvent, and 0.4g nano silica fume is added, mixes to solution stable homogeneous, obtains spinning solution.Using electrostatic spinning work
Spinning solution is spun into containing silicon source fibrous polypropylene nitrile/polystyrene supporter by skill.
To remove containing silicon source fibrous polypropylene nitrile/polystyrene support film monolith, be put into Muffle furnace 220 DEG C it is pre-
Aoxidize 3h；Then 5h is kept the temperature at 800 DEG C in a nitrogen atmosphere again, heating rate is 5 DEG C/min, obtains silicon-carbon self-supporting electrode.
Its hot weight curve is silicone content 64wt% shown in the 0.4g Si curve in Fig. 2.
Comparative example 1
Use 0.5g polyacrylonitrile for template, 0.3g polystyrene is as pore creating material, 5mL n,N-Dimethylformamide
Solvent mixes to solution stable homogeneous, obtains spinning solution.Using electrostatic spinning process, spinning solution is spun into and is free of
There is fibrous polypropylene nitrile/polystyrene supporter of silicon source；
Fibrous polypropylene nitrile/polystyrene support film monolith without containing silicon source is removed, is put into 260 in Muffle furnace
DEG C pre-oxidation 2h；Then 3h is kept the temperature at 700 DEG C in a nitrogen atmosphere again, heating rate is 5 DEG C/min, obtains porous carbon self-supporting
Electrode.
Then the electrode assembling that Examples 1 to 4 and comparative example 1 are prepared carries out lithium ion at lithium ion battery
Cycle performance comparison, the results are shown in Table 1, wherein discharge capacity is that the gross mass of carbon silicon composite cathode material is calculated.
1 Examples 1 to 4 of table and the comparison of 1 lithium ion cycle performance of comparative example
As can be seen from the above table, using porous carbon of the invention/silicon composite structure negative electrode material, it can guarantee high capacity
While performance, the effective capacity retention ratio for improving battery makes lithium ion obtain good cyclical stability.
Claims (9)
1. a kind of silicon-carbon self-supporting composite negative pole material, which is characterized in that the material includes carbon skeleton and is carried on carbon skeleton
Silicon powder in duct, the carbon skeleton be in self-supporting fibrous reticular structure, wherein the silicon powder account for material gross mass 10%~
90%.
2. a kind of silicon-carbon self-supporting composite negative pole material according to claim 1, which is characterized in that the partial size of the silicon powder
For 10~150nm.
3. a kind of preparation method of silicon-carbon self-supporting composite negative pole material as claimed in claim 1 or 2, which is characterized in that including
Following steps:
(1) polyacrylonitrile, polystyrene and silicon powder are added into n,N-Dimethylformamide, stirring and dissolving forms transparent molten
Liquid；
(2) clear solution is prepared into the macromolecular fibre shape supporter containing silicon source by method of electrostatic spinning, it is subsequently heat-treated
Obtain the silicon-carbon self-supporting composite negative pole material.
4. a kind of preparation method of silicon-carbon self-supporting composite negative pole material according to claim 3, which is characterized in that described
Polyacrylonitrile, polystyrene and silicon powder mass ratio be (0.1~0.9): (0.1~0.5): (0.05~0.4).
5. a kind of preparation method of silicon-carbon self-supporting composite negative pole material according to claim 3, which is characterized in that described
Stirring and dissolving carried out at a temperature of 60~70 DEG C, mixing time be greater than 5h.
6. a kind of preparation method of silicon-carbon self-supporting composite negative pole material according to claim 3, which is characterized in that described
Method of electrostatic spinning process conditions it is as follows: the voltage of 10~20KV, syringe at a distance from receiving screen be 8~15cm, receive
Screen is metal foil or metal mesh.
7. a kind of preparation method of silicon-carbon self-supporting composite negative pole material according to claim 3, which is characterized in that described
Heat treatment the following steps are included: at 200~250 DEG C pre-oxidize 2~4h, then again under an inert atmosphere with 3-5 DEG C/min
Heating rate be warming up to 500~1200 DEG C, and keep the temperature and be greater than 3h.
8. a kind of preparation method of silicon-carbon self-supporting composite negative pole material according to claim 7, which is characterized in that described
Inert atmosphere is nitrogen atmosphere.
9. a kind of application of silicon-carbon self-supporting composite negative pole material as claimed in claim 1 or 2, which is characterized in that the cathode
Material is used for lithium cell cathode material.
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Cited By (10)
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| CN110112405A (en) * | 2019-05-29 | 2019-08-09 | 哈尔滨理工大学 | A kind of core-shell structure silicon/carbon fiber flexible combination electrode material and the preparation method and application thereof |
| CN111074382A (en) * | 2019-12-20 | 2020-04-28 | 银隆新能源股份有限公司 | Silicon-carbon composite material, preparation method thereof, silicon-based negative electrode for lithium ion battery and lithium ion battery |
| WO2020132057A1 (en) * | 2018-12-21 | 2020-06-25 | Enevate Corporation | Silicon-based energy storage devices with anhydride containing electrolyte additives |
| CN111525114A (en) * | 2020-05-09 | 2020-08-11 | 四川聚创石墨烯科技有限公司 | Method for continuously preparing current collector-free silicon-carbon negative electrode paper |
| CN112186141A (en) * | 2019-07-04 | 2021-01-05 | 天津工业大学 | Flexible self-supporting carbon fiber negative electrode material of lithium/sodium ion battery and preparation method |
| CN112582615A (en) * | 2020-12-10 | 2021-03-30 | 广东凯金新能源科技股份有限公司 | One-dimensional porous silicon-carbon composite negative electrode material, preparation method and application thereof |
| CN112886007A (en) * | 2021-01-19 | 2021-06-01 | 广东工业大学 | Cobalt ditelluride/carbon nanofiber material and preparation method and application thereof |
| CN113097469A (en) * | 2021-03-22 | 2021-07-09 | 湖北工程学院 | Preparation method of Si/SiC/C nanofiber membrane, battery cathode and lithium ion battery |
| CN113422009A (en) * | 2021-06-01 | 2021-09-21 | 广东工业大学 | Lithium ion battery cathode material and preparation method and application thereof |
| CN113471399A (en) * | 2021-06-24 | 2021-10-01 | 湖北工程学院 | Preparation method and application of high-conductivity Si/C nano-film |
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| CN112186141A (en) * | 2019-07-04 | 2021-01-05 | 天津工业大学 | Flexible self-supporting carbon fiber negative electrode material of lithium/sodium ion battery and preparation method |
| CN111074382A (en) * | 2019-12-20 | 2020-04-28 | 银隆新能源股份有限公司 | Silicon-carbon composite material, preparation method thereof, silicon-based negative electrode for lithium ion battery and lithium ion battery |
| CN111525114A (en) * | 2020-05-09 | 2020-08-11 | 四川聚创石墨烯科技有限公司 | Method for continuously preparing current collector-free silicon-carbon negative electrode paper |
| CN112582615B (en) * | 2020-12-10 | 2022-09-06 | 广东凯金新能源科技股份有限公司 | One-dimensional porous silicon-carbon composite negative electrode material, preparation method and application thereof |
| CN112582615A (en) * | 2020-12-10 | 2021-03-30 | 广东凯金新能源科技股份有限公司 | One-dimensional porous silicon-carbon composite negative electrode material, preparation method and application thereof |
| CN112886007A (en) * | 2021-01-19 | 2021-06-01 | 广东工业大学 | Cobalt ditelluride/carbon nanofiber material and preparation method and application thereof |
| CN112886007B (en) * | 2021-01-19 | 2022-07-29 | 广东工业大学 | Cobalt ditelluride/carbon nanofiber material and preparation method and application thereof |
| CN113097469A (en) * | 2021-03-22 | 2021-07-09 | 湖北工程学院 | Preparation method of Si/SiC/C nanofiber membrane, battery cathode and lithium ion battery |
| CN113422009B (en) * | 2021-06-01 | 2022-03-18 | 广东工业大学 | Lithium ion battery cathode material and preparation method and application thereof |
| CN113422009A (en) * | 2021-06-01 | 2021-09-21 | 广东工业大学 | Lithium ion battery cathode material and preparation method and application thereof |
| CN113471399A (en) * | 2021-06-24 | 2021-10-01 | 湖北工程学院 | Preparation method and application of high-conductivity Si/C nano-film |
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