CN106025211A - Preparation method of high-capacity silicon-based negative electrode material of lithium-ion battery - Google Patents
Preparation method of high-capacity silicon-based negative electrode material of lithium-ion battery Download PDFInfo
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- CN106025211A CN106025211A CN201610393161.0A CN201610393161A CN106025211A CN 106025211 A CN106025211 A CN 106025211A CN 201610393161 A CN201610393161 A CN 201610393161A CN 106025211 A CN106025211 A CN 106025211A
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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
The invention discloses a preparation method of a high-capacity silicon-based negative electrode material of a lithium-ion battery. The method comprises the preparation processes of: mixing nano silicon, graphite and a pyrolytic carbon organic matter precursor to obtain composite material precursor slurry; and carrying out spray drying to obtain precursor powder; and finally carrying out roasting treatment in an inert atmosphere and then carrying out grinding to obtain an organic matter pyrolytic carbon-coated nano silicon/graphite composite material. According to the preparation method, the dispersity of the nano silicon in the silicon-carbon negative electrode material can be improved; the structure stability of the material in a lithium intercalation and deintercalation process is improved; the condition that the material has relatively high conductivity is ensured; a pyrolytic carbon coating layer effectively coats the surfaces of material particles; the interface characteristic of the material can be effectively improved; and the electrochemical properties of the silicon-carbon negative electrode material are improved.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, be specifically related to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material.
Background technology
Lithium rechargeable battery has become the electrochmical power source of main flow the most, it is widely used in overwhelming majority mobile terminal device, compared to ni-mh, NI-G and lead-acid battery, lithium rechargeable battery has the advantages such as running voltage is high, specific energy is high and has extended cycle life, being developed rapidly in recent years, the application in the mobile devices such as notebook computer, digital camera, mobile phone, MP3 and MP4 is more and more extensive.Along with mobile device develops to miniaturization and multifunction direction, energy density and service life to lithium rechargeable battery are had higher requirement, also due to the fast development of various portable electric appts and electric automobile and extensively application, the demand of lithium ion battery high for energy, that have extended cycle life is the most urgent.The main negative material of commercial Li-ion battery is graphite at present, and due to its theoretical capacity low (372mAh/g), high-rate charge-discharge capability is poor, limits the further raising of lithium ion battery energy.
Owing to silicon has the highest theoretical specific capacity (4200mAh/g) and relatively low de-lithium current potential (less than 0.5V), become one of lithium ion battery negative material of the most potential replacement graphite in recent years.Li and Si can form LixSi (0 < x≤4.4) alloy, it is considered that at normal temperatures, and the rich lithium product that silicium cathode produces with lithium alloyage is mainly Li3.7Si5Phase, capacity is up to 3572mAh/g, and much larger than the theoretical capacity of graphite, but in charge and discharge process, silicon can occur huge change in volume, causes material efflorescence, peels off, loses electrical contact, and capacity attenuation is quickly.By using the particle diameter reducing silicon materials, silicon is made porous material, reducing the dimension of silicon materials, prepare the modes such as Si-C composite material and improve cyclical stability and the first charge-discharge efficiency of silicon-based anode to a certain extent in prior art, but, these Improving Measurements need higher cost mostly, need to mate corresponding electrolyte and could preferably play its performance, and the long-term cycle performance of material is the most poor.Therefore, it is a kind of good with compatibility of electrolyte to research and develop, good cycle, and the silicon based anode material of advantage of lower cost is significant to the performance improving lithium ion battery.
Summary of the invention
The technical problem to be solved is, overcomes deficiency of the prior art, it is provided that the preparation method of a kind of high-capacity lithium ion cell silicon based anode material, this negative material the capacity of lithium ion battery prepared is high, good cycle.
The preparation method of a kind of high-capacity lithium ion cell silicon based anode material, comprises the following steps:
(1) nano-silicon is joined in solvent and carry out ultrasonic disperse, be subsequently adding graphite and carry out mix and blend, add pyrolytic carbon organic matter precursor and continue mix and blend, obtain precursor pulp；
(2) precursor pulp in step (1) is spray-dried, obtains presoma powder body；
(3) the presoma powder body that step (2) obtains is carried out under an inert atmosphere calcination process, the most polished nano-silicon/graphite composite material obtaining organic matter pyrolysis carbon cladding.
Above-mentioned preparation method, in step (1), the mass ratio of nano-silicon and graphite is (1～10): 100, and described nano-silicon is graininess, and particle diameter is 5nm～100nm；Described graphite one or two kinds of in Delanium, native graphite, described graphite is graininess, and mean diameter D50 is 0.5 μm～20 μm.
In step (1), solvent is deionized water, methanol, ethanol, ethylene glycol, propanol or N-Methyl pyrrolidone, ultrasonic disperse time a length of 10～120 minutes, add and carry out mix and blend 30～120 minutes after graphite.
In step (1), pyrolytic carbon organic matter precursor is the one in phenolic resin, citric acid, glucose, sucrose, chitosan, polyvinylidene fluoride, Colophonium, and the addition of pyrolytic carbon organic matter precursor accounts for nano-silicon and the 5 of graphite gross mass～10%.Add and continue mix and blend 60～100 minutes after pyrolytic carbon organic matter precursor.
The inlet temperature of the hot-air being spray-dried in step (2) is 150 DEG C～250 DEG C, and outlet temperature is 40 DEG C～90 DEG C.
In step (3), inert atmosphere is argon, helium or nitrogen, particularly preferably argon, and sintering temperature is 600 DEG C～1000 DEG C, during roasting a length of 3～12 hours.
The present invention prepares nano-silicon/graphite composite by being scattered between graphite space by nano-silicon or being attached to the surface of graphite, then nano-silicon/graphite composite is carried out high temperature pyrolysis carbonization treatment, prepare the nano-silicon/graphite composite material of pyrolytic carbon cladding, obtain the high-capacity lithium ion cell silicon based anode material of the present invention.This preparation method can improve nano-silicon dispersibility in silicon-carbon cathode material, improve material structural stability during removal lithium embedded, ensure that material has higher conductivity, the surface of material granule effectively it is wrapped at pyrolytic carbon clad, the interfacial characteristics of material can be effectively improved, improve the chemical property of silicon-carbon cathode material.
Compared with prior art, the invention have the advantages that
(1) nano-silicon is dispersed between graphite by the present invention, effectively improves the reuniting effect of nano-silicon, provides space for nano-silicon volumetric expansion in charge and discharge process, it is to avoid nano-silicon ruptures and causes performance degradation；
(2) present invention uses organic matter pyrolysis carbon to be coated on silicon and graphite granule surface, improves the electric conductivity of composite, also makes nano-silicon and graphite contact more tight simultaneously, reduces the contact resistance between nano-silicon and graphite, be conducive to improving the electric conductivity of material；
(3) amorphous carbon that pyrolytic carbon organic matter precursor is formed after high temperature cabonization, electrolyte is had stronger corrosion resistance ability, simultaneously, the interlamellar spacing of amorphous carbon is bigger, lithium ion can quickly pass in and out, meeting the requirement of lithium ion battery high power charging-discharging, the hole and the space that are formed after carbonization can buffer the bulk effect that silica flour produces when discharge and recharge, it is ensured that the overall stability of material.
Accompanying drawing explanation
Fig. 1 is the cycle performance figure of the embodiment of the present invention 1.
Fig. 2 is the gram volume conservation rate figure of the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the preferably embodiment of the present invention is described in further detail.
Embodiment 1
The preparation method of a kind of high-capacity lithium ion cell silicon based anode material, comprises the following steps:
(1) 5g nano-silicon (particle diameter is 50nm) is joined in alcohol solvent, ultrasonic disperse 60min, it is subsequently adding 100g Delanium, mix and blend 30min, adds 8g phenolic resin afterwards, continue mix and blend 60min；
(2) by the slurry of mix homogeneously by being spray-dried, presoma powder body is obtained；
(3) powder body step (2) obtained, under argon shield, is warming up to 800 DEG C, and the time is 8h, grinds, obtain the nano-silicon/graphite composite material of organic matter pyrolysis carbon cladding after cooling down to room temperature.
With obtained composite, PVDF, the mass ratio of conductive carbon black is that 85:10:5 is coated in Copper Foil as negative pole, and using metal lithium sheet as to electrode, the hexafluoro phosphorus lithium of 1mol/L, as electrolyte, is assembled into button cell.Button cell under the electric current density of 200mA/g, the cycle performance figure of this electrode material as it is shown in figure 1, capability retention as shown in Figure 2.Can be seen that the discharge capacity first of this composite reaches 825mAh/g, the capacity after 100 circulations still has 660mAh/g, and conservation rate is 80%, and cyclic curve figure is shown in accompanying drawing 1.
Embodiment 2
The preparation method of a kind of high-capacity lithium ion cell silicon based anode material, comprises the following steps:
(1) 10g nano-silicon (particle diameter is 50nm) is joined in alcohol solvent, ultrasonic disperse 60min, it is subsequently adding 100g native graphite, mix and blend 45min, adds 10g phenolic resin afterwards, continue mix and blend 60min；
(2) by the slurry of mix homogeneously by being spray-dried, presoma powder body is obtained；
(3) powder body step (2) obtained, under argon shield, is warming up to 900 DEG C, and the time is 10h, grinds, obtain the nano-silicon/graphite composite material of organic matter pyrolysis carbon cladding after cooling down to room temperature.
With obtained composite, PVDF, the mass ratio of conductive carbon black is that 85:10:5 is coated in Copper Foil as negative pole, and using metal lithium sheet as to electrode, the hexafluoro phosphorus lithium of 1mol/L, as electrolyte, is assembled into button cell.Button cell is under the electric current density of 200mA/g, and the discharge capacity first of this electrode material reaches 990mAh/g, and the capacity after 100 circulations still has 772mAh/g, and conservation rate is 78%.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (6)
1. a preparation method for high-capacity lithium ion cell silicon based anode material, comprises the following steps:
(1) nano-silicon is joined in solvent and carry out ultrasonic disperse, be subsequently adding graphite and carry out mix and blend, add pyrolytic carbon organic matter precursor and continue mix and blend, obtain precursor pulp；
(2) precursor pulp in step (1) is spray-dried, obtains presoma powder body；
(3) the presoma powder body that step (2) obtains is carried out under an inert atmosphere calcination process, the most polished nano-silicon/graphite composite material obtaining organic matter pyrolysis carbon cladding.
2. according to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material described in claim 1, it is characterized in that: in step (1), the mass ratio of nano-silicon and graphite is (1～10): 100, described nano-silicon is graininess, and particle diameter is 5nm～100nm；Described graphite one or two kinds of in Delanium, native graphite, described graphite is graininess, and mean diameter D50 is 0.5 μm～20 μm.
3. according to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material described in claim 1, it is characterized in that: in step (1), solvent is deionized water, methanol, ethanol, ethylene glycol, propanol or N-Methyl pyrrolidone, ultrasonic disperse time a length of 10～120 minutes, add and carry out mix and blend 30～120 minutes after graphite.
4. according to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material described in claim 1, it is characterized in that: in step (1), pyrolytic carbon organic matter precursor is the one in phenolic resin, citric acid, glucose, sucrose, chitosan, polyvinylidene fluoride, Colophonium, the addition of pyrolytic carbon organic matter precursor accounts for nano-silicon and the 5 of graphite gross mass～10%, continues mix and blend 60～100 minutes after adding pyrolytic carbon organic matter precursor.
5. according to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material described in claim 1, it is characterized in that: the inlet temperature of the hot-air being spray-dried in step (2) is 150 DEG C～250 DEG C, and outlet temperature is 40 DEG C～90 DEG C.
6. according to the preparation method of a kind of high-capacity lithium ion cell silicon based anode material described in claim 1, it is characterized in that: in step (3), inert atmosphere is argon, helium or nitrogen, particularly preferably argon, sintering temperature is 600 DEG C～1000 DEG C, during roasting a length of 3～12 hours.
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Cited By (20)
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| CN106654220A (en) * | 2017-01-11 | 2017-05-10 | 湘潭大学 | Preparation method of high-capacity carbon-silicon composite negative material |
| CN107346822A (en) * | 2017-04-25 | 2017-11-14 | 山东玉皇新能源科技有限公司 | A kind of method that solvent-thermal method prepares graphene silicon composite cathode material |
| CN107863507A (en) * | 2017-01-21 | 2018-03-30 | 福建金山锂科新材料有限公司 | The method that Suspended Emulsion Polymerization method prepares silicon-carbon cathode material |
| CN107994213A (en) * | 2017-11-10 | 2018-05-04 | 北京圣比和科技有限公司 | The method and device of double consumable rotation electrode arc-plasma synthesis silicon carbon materials |
| CN109301224A (en) * | 2018-10-16 | 2019-02-01 | 中航锂电技术研究院有限公司 | A kind of preparation method and application of silicon-based composite anode material for Li-ion battery |
| CN109461890A (en) * | 2017-09-06 | 2019-03-12 | 丰域科技（北京）有限公司 | Silicon-carbon cathode material, preparation method and lithium ion battery |
| CN109565036A (en) * | 2018-09-28 | 2019-04-02 | 香港应用科技研究院有限公司 | Active material of positive electrode for lithium ion battery |
| CN110416513A (en) * | 2019-07-23 | 2019-11-05 | 中国恩菲工程技术有限公司 | Preparation method, carbon silicon combination electrode and the battery comprising it of carbon-silicon composite material |
| CN110416515A (en) * | 2019-07-24 | 2019-11-05 | 东莞东阳光科研发有限公司 | Lithium ion battery, lithium ion battery negative material and preparation method |
| CN110571409A (en) * | 2018-06-05 | 2019-12-13 | 微宏动力系统（湖州）有限公司 | preparation method of negative electrode material, negative electrode material and lithium battery |
| CN110600684A (en) * | 2018-09-12 | 2019-12-20 | 湖北万润新能源科技发展有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| WO2020062354A1 (en) * | 2018-09-28 | 2020-04-02 | Hong Kong Applied Science and Technology Research Institute Company Limited | Anode Active Materials for Lithium-ion Batteries |
| CN111573662A (en) * | 2020-05-21 | 2020-08-25 | 北京蒙京石墨新材料科技研究院有限公司 | Method for preparing high-capacity negative electrode material by utilizing recovered graphite |
| CN111584856A (en) * | 2020-04-14 | 2020-08-25 | 合肥国轩电池材料有限公司 | High-performance silicon-carbon negative electrode material and preparation method thereof |
| CN111697206A (en) * | 2019-03-14 | 2020-09-22 | 吉林聚能新型炭材料股份有限公司 | Preparation method of silicon-carbon negative electrode material |
| CN112582591A (en) * | 2020-12-01 | 2021-03-30 | 桐乡市昇威电子商务服务有限公司 | Porous nano silicon-carbon composite lithium ion battery cathode material and preparation method thereof |
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| CN111573662A (en) * | 2020-05-21 | 2020-08-25 | 北京蒙京石墨新材料科技研究院有限公司 | Method for preparing high-capacity negative electrode material by utilizing recovered graphite |
| CN112582591A (en) * | 2020-12-01 | 2021-03-30 | 桐乡市昇威电子商务服务有限公司 | Porous nano silicon-carbon composite lithium ion battery cathode material and preparation method thereof |
| CN112803005A (en) * | 2021-03-04 | 2021-05-14 | 合肥国轩高科动力能源有限公司 | Preparation method and application of silicon-carbon negative electrode material of lithium ion battery |
| CN112803005B (en) * | 2021-03-04 | 2022-05-13 | 合肥国轩高科动力能源有限公司 | Preparation method and application of silicon-carbon negative electrode material of lithium ion battery |
| CN114744178A (en) * | 2022-04-29 | 2022-07-12 | 中国有色桂林矿产地质研究院有限公司 | Nano silicon-graphite composite negative electrode material with carbon-coated and aluminum metaphosphate composite modification layer on surface and preparation method thereof |
| WO2023206673A1 (en) * | 2022-04-29 | 2023-11-02 | 中国有色桂林矿产地质研究院有限公司 | Nano silicon-graphite composite negative electrode material with carbon coating and aluminum metaphosphate composite modification layer on surface, and preparation method therefor |
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