CN104993118A - Synthesizing method for lithium-ion negative electrode material of Li4Ti5O12/C - Google Patents

Synthesizing method for lithium-ion negative electrode material of Li4Ti5O12/C Download PDF

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Publication number
CN104993118A
CN104993118A CN201510333725.7A CN201510333725A CN104993118A CN 104993118 A CN104993118 A CN 104993118A CN 201510333725 A CN201510333725 A CN 201510333725A CN 104993118 A CN104993118 A CN 104993118A
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lithium
titanium dioxide
cathode material
synthetic method
powder
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田东
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Priority to PCT/CN2016/083771 priority patent/WO2016202162A1/en
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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
    • 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
    • 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
    • H01M4/48—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
    • 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
    • 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 synthesizing method for a lithium-ion negative electrode material of Li4Ti5O12/C. The synthesizing method is characterized by comprising the following steps that firstly, titanium dioxide and an organic carbon source are mixed with added water, spray granulation is conducted after ball grinding treatment is conducted, obtained powder is pretreated in the inert atmosphere, and carbon-covering titanium dioxide powder is obtained; secondly, a lithium source is dissolved into water, the titanium dioxide powder obtained in the first step is added, spray granulation is conducted after ball grinding treatment is conducted, and the dried powder is obtained; thirdly, the dried powder obtained in the second step is treated in the inert atmosphere, high-temperature heat treatment is conducted, and the lithium-ion negative electrode material of Li4Ti5O12/C is obtained through airflow classification. Carbon covering is conducted on the titanium dioxide firstly, lithium titanate agglomeration caused by high-temperature treatment in the later period is avoided, lithium titanate grains are prevented from being excessively produced, the spreading speed of lithium ions in the charging and discharging process can be effectively increased, the electric conduction performance of the material is improved, and development of the electric performance of lithium titanate is ensured.

Description

A kind of ion cathode material lithium Li 4ti 5o 12the synthetic method of/C
Technical field
The present invention relates to lithium ion battery negative material, especially relate to a kind of ion cathode material lithium Li adopted prepared by carbon cladding titanium dioxide technique 4ti 5o 12the synthetic method of/C.
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.Li 4ti 5o 12as 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.
Summary of the invention
The object of this invention is to provide process route simple, be applicable to large-scale industrial production, adopt a kind of ion cathode material lithium Li prepared by carbon cladding titanium dioxide technique 4ti 5o 12the synthetic method of/C.
The present invention includes following steps:
1) add water titanium dioxide and organic carbon source mixing, mist projection granulating after ball-milling treatment, and the powder obtained preliminary treatment in an inert atmosphere, obtains carbon cladding titanium dioxide powder;
2) by soluble in water for lithium source, add the titanium dioxide powder that step 1) obtains, then mist projection granulating after ball-milling treatment, obtain dry powder;
3) by step 2) the dry powder that obtains processes in an inert atmosphere, then carries out high-temperature heat treatment, namely obtains ion cathode material lithium Li through air current classifying 4ti 5o 12/ C.
In step 1), described titanium dioxide is the one in anatase titanium dioxide or metal and stone type titanium dioxide.
In step 1), described organic carbon source can adopt the one in water-soluble organic substance, and described water-soluble organic substance can be selected from the one in glucose, sucrose, fructose, polyethylene glycol, polyacrylic acid, shitosan etc.; The time of described ball-milling treatment is 5 ~ 10h; Described pretreated temperature is 400 ~ 500 DEG C, and the pretreated time is 5 ~ 8h.
In step 2) in, described lithium source can adopt the one in water-soluble lithium salts lithium acetate, lithium hydroxide; The time of described ball-milling treatment is 2 ~ 3h.
In step 1) and 2) in, described titanium dioxide, lithium source are n(Li by element molal quantity): n(Ti)=0.84 ~ 0.87; In step 1), the quality of described organic carbon source is 10% ~ 15% of titanium dioxide quality; In step 1) and 2) in, described hydromining salt-free water, wherein in step 1), the addition of water can be 3 ~ 4 times of titanium dioxide in mass ratio, step 2) in the addition of water be 3 ~ 4 times of carbon cladding titanium dioxide powder quality in mass ratio.
In step 1) and 3) in, described inert atmosphere can adopt nitrogen or argon gas etc.
In step 3), the temperature of described process is 500 ~ 600 DEG C, and the time of process is 10 ~ 20h; The temperature of described high-temperature heat treatment is 750 ~ 850 DEG C, and the time of high-temperature heat treatment is 2 ~ 20h.
With existing ion cathode material lithium Li 4ti 5o 12synthetic method compare, the invention has the advantages that: first carbon carried out to synthesis material titanium dioxide coated, avoid the later stage to cause the reunion of lithium titanate because of high-temperature process, prevent lithium titanate crystal grain from producing excessive, effectively can improve lithium ion and cross diffusion rate in title in discharge and recharge.Have employed water-soluble organic carbon source, make carbon source evenly be coated on particle surface, the conductivity height nano-carbon coated layer that organic substance is formed after oversintering pyrolysis, greatly improves the electric conductivity of material, ensures the performance of lithium titanate electrical property.
Embodiment
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
According to n(Li): n(Ti)=0.84, take 694g lithium acetate and 1000g titanium dioxide, organic carbon source glucose 100g is added according to the weight of titanium dioxide 10%, titanium dioxide and glucose are added 3L salt-free water mix, ball-milling treatment 8h, mist projection granulating, the powder obtained, in an inert atmosphere in 500 DEG C of preliminary treatment 7h, obtains carbon cladding titanium dioxide powder.Be dissolved in by lithium acetate in 3.5L salt-free water, add carbon cladding titanium dioxide powder and stir, ball-milling treatment 3h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2650 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 5h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.2%.
Embodiment 2
According to n(Li): n(Ti)=0.87, take 261g lithium hydroxide and 1000g titanium dioxide, organic carbon source sucrose 150g is added according to the weight of titanium dioxide 15%, titanium dioxide and sucrose are added 3.5L salt-free water mix, ball-milling treatment 8h, mist projection granulating, the powder obtained, in an inert atmosphere in 500 DEG C of preliminary treatment 8h, obtains carbon cladding titanium dioxide powder.Be dissolved in by lithium hydroxide in 3.5L salt-free water, add carbon cladding titanium dioxide powder and stir, ball-milling treatment 3h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2600 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 4h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 1.6%.
Embodiment 3
According to n(Li): n(Ti)=0.85, take 255g lithium hydroxide and 1000g titanium dioxide, organic carbon source polyethylene glycol 100g is added according to the weight of titanium dioxide 10%, titanium dioxide and polyethylene glycol are added 3.0L salt-free water mix, ball-milling treatment 3h, mist projection granulating, the powder obtained, in an inert atmosphere in 500 DEG C of preliminary treatment 8h, obtains carbon cladding titanium dioxide powder.Be dissolved in by lithium hydroxide in 3.5L salt-free water, add carbon cladding titanium dioxide powder and stir, ball-milling treatment 3h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2650 DEG C of sintering 8h in atmosphere, then after being warming up to 820 DEG C of sintering 6h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 2.3%.
Embodiment 4
According to n(Li): n(Ti)=0.86, take 710g lithium acetate and 1000g titanium dioxide, organic carbon source polyacrylic acid 150g is added according to the weight of titanium dioxide 15%, titanium dioxide and polypropylene are added 3.6L salt-free water mix, ball-milling treatment 8h, mist projection granulating, the powder obtained, in an inert atmosphere in 500 DEG C of preliminary treatment 8h, obtains carbon cladding titanium dioxide powder.Be dissolved in by lithium acetate in 3.5L salt-free water, add carbon cladding titanium dioxide powder and stir, ball-milling treatment 3h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2650 DEG C of sintering 8h in atmosphere, then after being warming up to 880 DEG C of sintering 8h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 2.6%.
Embodiment 5
According to n(Li): n(Ti)=0.87, take 261g lithium hydroxide and 1000g titanium dioxide, organic carbon source glucose 100g is added according to the weight of titanium dioxide 10%, titanium dioxide and glucose are added 3.6L salt-free water mix, ball-milling treatment 8h, mist projection granulating, the powder obtained, in an inert atmosphere in 500 DEG C of preliminary treatment 8h, obtains carbon cladding titanium dioxide powder.Be dissolved in by lithium hydroxide in 4.0L salt-free water, add carbon cladding titanium dioxide powder and stir, ball-milling treatment 3h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2650 DEG C of sintering 8h in atmosphere, then after being warming up to 880 DEG C of sintering 5h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 2.3%.
Comparative example 1
According to n(Li): n(Ti)=0.84, takes 694g lithium acetate and 1000g titanium dioxide, and add 3L salt-free water and mix, ball-milling treatment 8h, mist projection granulating obtains dry powder.This powder is joined in rotary furnace, at N 2650 DEG C of sintering 8h in atmosphere, then after being warming up to 800 DEG C of sintering 5h, cooling, sieves, air current classifying and obtain product.
Products obtained therefrom carbon content is 0.
Electrochemical property test
For the performance of modification lithium-ion battery lithium titanate anode 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.
Table 1 is the Performance comparision of negative material in different embodiment and comparative example
More than show and describe general principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection range is defined by appending claims and equivalent thereof.

Claims (10)

1. an ion cathode material lithium Li 4ti 5o 12the synthetic method of/C, is characterized in that comprising the following steps:
1) add water titanium dioxide and organic carbon source mixing, mist projection granulating after ball-milling treatment, and the powder obtained preliminary treatment in an inert atmosphere, obtains carbon cladding titanium dioxide powder;
2) by soluble in water for lithium source, add the titanium dioxide powder that step 1) obtains, then mist projection granulating after ball-milling treatment, obtain dry powder;
3) by step 2) the dry powder that obtains processes in an inert atmosphere, then carries out high-temperature heat treatment, namely obtains ion cathode material lithium Li through air current classifying 4ti 5o 12/ C.
2. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1), and described titanium dioxide is the one in anatase titanium dioxide or metal and stone type titanium dioxide.
3. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1), and described organic carbon source adopts the one in water-soluble organic substance, and described water-soluble organic substance is selected from the one in glucose, sucrose, fructose, polyethylene glycol, polyacrylic acid, shitosan.
4. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1), and the time of described ball-milling treatment is 5 ~ 10h; Described pretreated temperature is 400 ~ 500 DEG C, and the pretreated time is 5 ~ 8h.
5. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 2) in, described lithium source can adopt the one in water-soluble lithium salts lithium acetate, lithium hydroxide; The time of described ball-milling treatment is 2 ~ 3h.
6. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1) and 2) in, described titanium dioxide, lithium source are n(Li by element molal quantity): n(Ti)=0.84 ~ 0.87.
7. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1), and in step 1), the quality of described organic carbon source is 10% ~ 15% of titanium dioxide quality.
8. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, it is characterized in that in step 1) and 2) in, in step 1) and 2) in, described hydromining salt-free water, wherein in step 1), the addition of water is 3 ~ 4 times of titanium dioxide in mass ratio, step 2) in the addition of water be 3 ~ 4 times of carbon cladding titanium dioxide powder quality in mass ratio.
9. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 1) and 3) in, described inert atmosphere adopts nitrogen or argon gas.
10. a kind of ion cathode material lithium Li as described in claim 1 4ti 5o 12the synthetic method of/C, is characterized in that in step 3), and the temperature of described process is 500 ~ 600 DEG C, and the time of process is 10 ~ 20h; The temperature of described high-temperature heat treatment is 750 ~ 850 DEG C, and the time of high-temperature heat treatment is 2 ~ 20h.
CN201510333725.7A 2015-06-16 2015-06-16 Synthesizing method for lithium-ion negative electrode material of Li4Ti5O12/C Pending CN104993118A (en)

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PCT/CN2016/083771 WO2016202162A1 (en) 2015-06-16 2016-05-28 Method for synthesizing lithium-ion negative-electrode material li4ti5o12/c

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WO2016202162A1 (en) * 2015-06-16 2016-12-22 田东 Method for synthesizing lithium-ion negative-electrode material li4ti5o12/c
CN106328891A (en) * 2016-08-29 2017-01-11 深圳博磊达新能源科技有限公司 Nano lithium titanate composite, preparation method thereof and lithium titanate battery
CN106784693A (en) * 2016-12-26 2017-05-31 上海中聚佳华电池科技有限公司 A kind of surface has the preparation method of the rich nitrogen nano lithium titanate electrode material of uniform carbon coating layer
CN107528057A (en) * 2017-08-31 2017-12-29 北方奥钛纳米技术有限公司 The preparation method of carbon coating lithium titanate and carbon coating lithium titanate and application
CN108963198A (en) * 2017-05-22 2018-12-07 动力专家有限公司 Anode, cathode, preparation method and the lithium ion battery including it

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CN111943259B (en) * 2020-08-24 2022-12-06 合肥工业大学 Carbon-coated mesoporous dual-phase titanium dioxide and preparation method and energy storage application thereof
CN113571677A (en) * 2021-05-17 2021-10-29 兰州大学 Modification method for improving first coulombic efficiency of carbon-based negative electrode material
CN115571908A (en) * 2022-10-18 2023-01-06 深圳电网智慧能源技术有限公司 Lithium titanate electrode material and application thereof in composite battery and standby power supply

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CN106784693A (en) * 2016-12-26 2017-05-31 上海中聚佳华电池科技有限公司 A kind of surface has the preparation method of the rich nitrogen nano lithium titanate electrode material of uniform carbon coating layer
CN108963198A (en) * 2017-05-22 2018-12-07 动力专家有限公司 Anode, cathode, preparation method and the lithium ion battery including it
CN107528057A (en) * 2017-08-31 2017-12-29 北方奥钛纳米技术有限公司 The preparation method of carbon coating lithium titanate and carbon coating lithium titanate and application

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Application publication date: 20151021