CN104916835A - Preparation method of lithium titanate silicon-based composite anode material - Google Patents
Preparation method of lithium titanate silicon-based composite anode material Download PDFInfo
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- CN104916835A CN104916835A CN201510404666.8A CN201510404666A CN104916835A CN 104916835 A CN104916835 A CN 104916835A CN 201510404666 A CN201510404666 A CN 201510404666A CN 104916835 A CN104916835 A CN 104916835A
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- 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
- H01M4/364—Composites as mixtures
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- 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
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- H—ELECTRICITY
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- 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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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- 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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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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
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Abstract
The invention discloses a preparation method of a lithium titanate silicon-based composite anode material. According to the preparation method, nano silicon is coated with a resin carbon precursor, porous carbon formed after the carbonization of resin carbon precursor is used as a carrier of fixed nano silicon, can effectively alleviate the volume expansion effect of silicon, is compounded with lithium titanate, and is subjected to the asphalt coating modification treatment, so as to solve the defects of too large specific surface area of resin material and low capacity of lithium titanate, avoid large irreversible capacity loss, and improve the specific capacity of the material; therefore, the finally obtained material has the advantages of low specific surface area, excellent processing performance, high specific capacity, long periodic cycle and the like. Meanwhile, according to the invention, the preparation method is simple to operate, easy to control, low in production cost, and suitable for industrial production.
Description
Technical field
The present invention relates to lithium ion battery negative material field, be specifically related to the preparation method of the silica-based composite negative pole material of a kind of lithium ion battery lithium titanate.
Background technology
At present continuous deterioration with climatic environment in short supply along with global petroleum resources, human social development is faced with stern challenge.The new-energy automobile of development clean energy-saving is subject to the great attention of countries in the world.The development of new-energy automobile, crucial in its electrical source of power.Lithium ion battery has the advantages such as energy density is large, self discharge is little, memory-less effect, operating voltage range are wide, long service life, non-environmental-pollution, is the main electrical source of power of current new-energy automobile.And the crucial electrode material of lithium ion battery is the final deciding factor of battery performance, wherein the raising of negative material to performance of lithium ion battery plays vital effect.Therefore, high-performance, cheap negative material is developed to promoting that the development of new-energy automobile and relevant new industry has great importance.
Current negative material is mainly graphite, and its specific capacity, close to the theoretical value of 372mAh/g, is difficult to have the space of lifting again, and therefore finding the height ratio capacity negative material substituting carbon becomes an important developing direction.Li4Ti5O12 is as a kind of novel ion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolyte, security performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.Compared with carbon negative electrode material, lithium titanate has a lot of advantages, wherein, the deintercalation of lithium ion in lithium titanate is reversible, and lithium ion is embedding or is deviating from the process of lithium titanate, its crystal formation does not change, change in volume is less than 1%, therefore be called as " zero strain material ", can avoid causing structural damage due to the flexible back and forth of electrode material in charge and discharge cycles, thus improve cycle performance and the useful life of electrode, decrease and increase with cycle-index and bring specific capacity significantly to decay, there is the cycle performance more excellent than Carbon anode; But, because lithium titanate is a kind of insulating material, its conductivity is low, thus cause the application in lithium electricity to there is the poor problem of high rate performance, lithium titanate material theoretical specific capacity is 175 mAh/g simultaneously, and actual specific capacity is greater than 160mAh/g, has the shortcomings such as gram volume is lower, therefore, it is very necessary for carrying out modification for lithium titanate.
And silicon-based anode has unique advantage and potential, silicium cathode material, in charge and discharge process, can form Li with lithium
12si
7, Li
13si
4, Li
7si
3, Li
15si
4, Li
22si
5deng alloy, there is high power capacity (Li
22si
5, the highest 4200mAh/g), the voltage of removal lithium embedded is low, with the advantage such as electrolyte reactivity is low, security performance is good.But violent volumetric expansion (0 ~ 300%) can occur silicon in removal lithium embedded course of reaction, thus causes destruction and the efflorescence of material structure, causes capacity to be decayed rapidly, cycle performance worsens.In addition, also there is the defects such as conductivity is low, and high rate performance is not good enough, and coulombic efficiency is lower in silicium cathode.
Research show metal dust and silica flour and lithium titanate compound to prepare obtain the performance that negative material can greatly improve lithium titanate anode material.The advantages such as metal itself has good ductility, high conductivity, and mechanical strength is high, therefore select suitable metal and silicon to form silicon-carbon, effectively can overcome the bulk effect of silicon in charge and discharge process, improve the cyclical stability of material, conductivity is also necessarily improved.But current existing silicon-carbon cathode material capacity and head are imitated generally on the low side, and the material consistency of preparation is poor.
Therefore, the lithium titanate composite anode material developing a kind of high conductivity, high power capacity, high first charge-discharge efficiency and good cycling stability is the technical barrier of field of lithium ion battery.
Summary of the invention
For prior art Problems existing, an object of the present invention is the preparation method providing the silica-based composite negative pole material of a kind of lithium titanate, the method first adopts resinae carbon matrix precursor to carry out coated to nano-silicon, carbon matrix precursor forms loose structure after high temperature cabonization, effectively can alleviate the Volumetric expansion of silicon, again by pulverizing, submicron powder is obtained to the material after coated carbonization, after mixing with lithium titanate, pitch class carbon matrix precursor again, pass through high-temperature process, cooling is sieved, and obtains the silica-based composite negative pole material of lithium titanate of the present invention.
A preparation method for the silica-based composite negative pole material of lithium titanate, concrete preparation process is as follows:
(1) by the dispersion of resinae carbon matrix precursor in a solvent, add nano-silicon, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, high temperature cabonization, obtains materials A;
(2) by materials A by pulverizing, obtain particle diameter D50 between the submicron order powder B of 0.1 ~ 1 μm;
(3) powder B and lithium titanate, pitch class carbon matrix precursor are carried out solid phase mixing, then under inert gas shielding, high temperature cabonization, cooling is sieved.
Further, resinae carbon matrix precursor refers to the combination of in furfural resin, epoxy resin, phenolic resins, polyethylene glycol, polyvinyl chloride, polyvinyl butyral resin, polyacrylonitrile, polyacrylic acid a kind or at least 2 kinds in step (1).
Further, in step (1), the ratio of resinae carbon matrix precursor and nano-silicon is 1:(0.05 ~ 0.15).
Further, in step (1), the temperature of high temperature cabonization is 650 ~ 850 DEG C, and heating rate is 1 ~ 5 DEG C/min, and temperature retention time is 0.5 ~ 3h.
Further, step (2) is pulverized and is referred to by the one or more kinds of combinations in ball milling, mechanical crushing or air-flow crushing mode.
Further, the weight ratio of step (3) powder B and lithium titanate is (0.1 ~ 0.5): 1, and pitch class carbon matrix precursor accounts for 10 ~ 30% of powder B and lithium titanate total weight.
Further, step (3) medium pitch class carbon forerunner refers to the combination of in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier a kind or at least 2 kinds.
Further, diameter of particle D50≤3 μm of step (3) medium pitch class carbon forerunner.
Further, in step (3), the temperature of high temperature cabonization is 850 ~ 1000 DEG C, and heating rate is 5 ~ 20 DEG C/min, and temperature retention time is 0.5 ~ 4h.
The loose structure carbon formed after the carbonization of resinae carbon matrix precursor is as the carrier of fixing nano-silicon, utilize the characteristic that organic molecule in resin is many, when high temperature, Small molecular therefrom overflows, form micropore, nano-silicon is evenly embedded in micropore, the method can improve the dispersiveness of silicon nanoparticle in silica-based composite negative pole material, alleviate material take off/embedding lithium time volumetric expansion and contraction, enhance the structural stability of material, ensure that material has higher conductance, improve chemical property and the cyclical stability thereof of material.
Again by after carrying out compound with lithium titanate, through pitch-coating modification, solve the shortcoming that resinous material specific area is excessive and lithium titanate capacity is on the low side, avoid large irreversible capacity loss, gram specific capacity of the material improved, the material of final gained has low specific area, good processing characteristics and the advantage such as Gao Ke specific capacity and long period circulation.
Meanwhile, method of the present invention is simple to operate, be easy to control, and production cost is low, be applicable to suitability for industrialized production.
Embodiment
In order to understand the present invention better, illustrate technical scheme of the present invention below by specific embodiment.
Embodiment 1
Epoxy resin is dispersed in acetone solvent, in epoxy resin: the ratio of nano-silicon=1:0.1 adds silica flour, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 750 DEG C are risen to the heating rate of 2 DEG C/min, insulation 2h, utilize air-flow crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.3:1 by powder and lithium titanate again, the petroleum asphalt (D50=2.15 μm) simultaneously adding 15% of powder and lithium titanate total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 850 DEG C with the heating rate of 10 DEG C/min, insulation 3h, after being cooled to room temperature, sieve and obtain the silica-based composite negative pole material of lithium titanate prepared by the present invention.
Embodiment 2
By phenolic resin dispersion in spirit solvent, in phenolic resins: the ratio of nano-silicon=1:0.15 adds silica flour, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 800 DEG C are risen to the heating rate of 3 DEG C/min, insulation 3h, utilize ball mill grinding that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.4:1 by powder and lithium titanate again, the coal tar pitch (D50=2.15 μm) simultaneously adding 20% of powder and lithium titanate total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 1000 DEG C with the heating rate of 10 DEG C/min, insulation 0.5h, after being cooled to room temperature, sieve and obtain the silica-based composite negative pole material of lithium titanate prepared by the present invention.
Embodiment 3
Polyethylene glycol is dispersed in deionization, in polyethylene glycol: the ratio of nano-silicon=1:0.05 adds silica flour, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 850 DEG C are risen to the heating rate of 5 DEG C/min, insulation 1h, utilize mechanical crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.5:1 by powder and lithium titanate again, the mesophase pitch (D50=2.15 μm) simultaneously adding 30% of powder and lithium titanate total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 900 DEG C with the heating rate of 15 DEG C/min, insulation 1.5h, after being cooled to room temperature, sieve and obtain the silica-based composite negative pole material of lithium titanate prepared by the present invention.
Embodiment 4
By phenolic resin dispersion in spirit solvent, in resin: the ratio of nano-silicon=1:0.1 adds silica flour, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 850 DEG C are risen to the heating rate of 2 DEG C/min, insulation 0.5h, utilize air-flow crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.25:1 by powder and lithium titanate again, the modified coal tar pitch (D50=2.15 μm) simultaneously adding 20% of powder and lithium titanate total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 850 DEG C with the heating rate of 5 DEG C/min, insulation 2.5h, after being cooled to room temperature, sieve and obtain the silica-based composite negative pole material of lithium titanate prepared by the present invention.
Comparative example 1
One-component lithium titanate in embodiment 1.
Comparative example 2
According to the preparation flow in embodiment 1, difference is not add the negative material that silica flour finally obtains.
Half-cell detects
For the electrical property of negative material prepared by inspection the inventive method, test by half-cell method of testing, negative material with above embodiment and comparative example: acetylene black: PVDF(Kynoar)=93:3:4(weight ratio), add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 1.0 ~ 2.5V, and charge-discharge velocity is 0.5C, and carry out testing to battery performance, test result is in table 1.
Full battery testing
Negative material with embodiment and comparative example: SP:SBR(solid content 50%): CMC=94:2.5:1.5:2(weight ratio), add appropriate amount of deionized water and mix furnishing pulpous state, be applied on Copper Foil, at 90 DEG C, vacuumize drying; By LiCoO
2powder: SP:KS-6:PVDF=94:1.5:2:2.5(weight ratio), do after solvent evenly sizes mixing with NMP, be applied on aluminium foil, at 100 DEG C, vacuumize drying; By dried positive and negative electrode pole piece through roll-in, cut-parts, winding, fluid injection, sealing, formation process, make 18650 cylindrical batteries, barrier film is Celgard2400, electrolyte is 1M LiPF6 ∕ DMC:EC:DEC, use battery check device to carry out the detection of cycle performance, test result is in table 1.
The Performance comparision of negative material in the different embodiment of table 1 and comparative example
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. a preparation method for the silica-based composite negative pole material of lithium titanate, concrete preparation process is as follows:
(1) by the dispersion of resinae carbon matrix precursor in a solvent, add nano-silicon, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, high temperature cabonization, obtains materials A;
(2) by materials A by pulverizing, obtain particle diameter D50 between the submicron order powder B of 0.1 ~ 1 μm;
(3) powder B and lithium titanate, pitch class carbon matrix precursor are carried out solid phase mixing, then under inert gas shielding, high temperature cabonization, cooling is sieved.
2. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, is characterized in that resinae carbon matrix precursor in step (1) refers to the combination of in furfural resin, epoxy resin, phenolic resins, polyethylene glycol, polyvinyl chloride, polyvinyl butyral resin, polyacrylonitrile, polyacrylic acid a kind or at least 2 kinds.
3. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, is characterized in that the ratio of resinae carbon matrix precursor and nano-silicon in step (1) is 1:(0.05 ~ 0.15).
4. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, it is characterized in that the temperature of high temperature cabonization in step (1) is 650 ~ 850 DEG C, heating rate is 1 ~ 5 DEG C/min, and temperature retention time is 0.5 ~ 3h.
5. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, is characterized in that step (2) is pulverized and refers to by the one or more kinds of combinations in ball milling, mechanical crushing or air-flow crushing mode.
6. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, it is characterized in that the weight ratio of step (3) powder B and lithium titanate is for (0.1 ~ 0.5): 1, pitch class carbon matrix precursor accounts for 10 ~ 30% of powder B and lithium titanate total weight.
7. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, it is characterized in that step (3) medium pitch class carbon forerunner refers to the combination of in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier a kind or at least 2 kinds, diameter of particle D50≤3 μm of pitch class carbon forerunner.
8. the preparation method of the silica-based composite negative pole material of a kind of lithium titanate according to claim 1, it is characterized in that the temperature of high temperature cabonization in step (3) is 850 ~ 1000 DEG C, heating rate is 5 ~ 20 DEG C/min, and temperature retention time is 0.5 ~ 4h.
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| CN201510404666.8A CN104916835A (en) | 2015-07-10 | 2015-07-10 | Preparation method of lithium titanate silicon-based composite anode material |
| PCT/CN2016/087172 WO2017008624A1 (en) | 2015-07-10 | 2016-06-25 | Method for fabricating lithium titanate silicon-based composite negative-electrode material |
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| WO2017008624A1 (en) * | 2015-07-10 | 2017-01-19 | 田东 | Method for fabricating lithium titanate silicon-based composite negative-electrode material |
| CN109326788A (en) * | 2018-11-20 | 2019-02-12 | 青海大学 | Negative electrode material and lithium ion battery and preparation method thereof |
| CN112467096A (en) * | 2020-10-30 | 2021-03-09 | 安普瑞斯（南京）有限公司 | Negative electrode material, preparation method thereof, electrode and secondary battery |
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| CN110247009A (en) * | 2019-07-03 | 2019-09-17 | 珠海冠宇电池有限公司 | A kind of anti-overcharge diaphragm and preparation method thereof and lithium ion battery |
| CN113800510A (en) * | 2021-09-07 | 2021-12-17 | 广东凯金新能源科技股份有限公司 | Graphite negative electrode material and preparation method thereof |
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| CN101244814A (en) * | 2007-02-13 | 2008-08-20 | 深圳市比克电池有限公司 | Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material |
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| CN102013487A (en) * | 2010-10-29 | 2011-04-13 | 济南大学 | Carbon/silicon composite lithium ion battery negative material and preparation method thereof |
| CN103022444A (en) * | 2012-12-05 | 2013-04-03 | 上海锦众信息科技有限公司 | Preparation method of carbon silicon composite material |
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| CN104916835A (en) * | 2015-07-10 | 2015-09-16 | 田东 | Preparation method of lithium titanate silicon-based composite anode material |
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| CN101244814A (en) * | 2007-02-13 | 2008-08-20 | 深圳市比克电池有限公司 | Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017008624A1 (en) * | 2015-07-10 | 2017-01-19 | 田东 | Method for fabricating lithium titanate silicon-based composite negative-electrode material |
| CN109326788A (en) * | 2018-11-20 | 2019-02-12 | 青海大学 | Negative electrode material and lithium ion battery and preparation method thereof |
| CN112467096A (en) * | 2020-10-30 | 2021-03-09 | 安普瑞斯（南京）有限公司 | Negative electrode material, preparation method thereof, electrode and secondary battery |
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Application publication date: 20150916 |