CN103840146A - Preparation method of high-tap-density lithium titanate material - Google Patents
Preparation method of high-tap-density lithium titanate material Download PDFInfo
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- CN103840146A CN103840146A CN201210487143.0A CN201210487143A CN103840146A CN 103840146 A CN103840146 A CN 103840146A CN 201210487143 A CN201210487143 A CN 201210487143A CN 103840146 A CN103840146 A CN 103840146A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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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
- H01M4/48—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
- 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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- 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
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Abstract
The invention relates to a preparation method of a high-tap-density lithium titanate material. The method comprises the following steps: (a), mixing a lithium compound, a titanium compound and a substance providing a carbon source according to the mass ratio Li to Ti to C of (0.1-0.2):1:(0-6), and ball-milling and mixing by taking deionized water as a medium; (b), spraying and drying the ball-milled slurry; and (c), calcining dried powder in an inert atmosphere at high temperature, so as to obtain the spherical lithium titanate material. The invention has the technical effects that the potential safety hazards and the environmental problem in the drying process of alcohol system slurry can be avoided by adopting a water-based slurry spraying and drying method; mixed powder good in sphericity, strong in mobility and uniform in particle size distribution can be obtained; in addition, after the powder is processed at the high temperature, the spherical lithium titanate material high in tap density and good in rate capability can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of lithium titanate, especially a kind of preparation method of high-tap density lithium titanate material.
Background technology
Spinelle Li
4ti
5o
12be that a kind of " zero strain " inserts material, embed crystal structure in the process of deviating from lithium ion and can keep the stability of height, and make it have good cycle performance and discharge voltage stably.Li
4ti
5o
12there is relatively high electrode potential (1.55Vvs.Li/Li+), make this material to obtain in burning voltage interval and to use at most liquid electrolyte, thereby avoided the generation of electrolyte decomposition phenomenon or protective layer (film).Li
4ti
5o
12there is platform in voltage in the time being charged to spinel structure and rock salt structure two-phase section, utilizes this point to can be used as the indication that charging finishes, and solved the security hidden trouble that carbon negative pole exists.Although Li
4ti
5o
12theoretical capacity only have 175mAh/g, but because its reversible lithium ion deintercalation ratio approaches 100%, therefore its actual capacity generally remains on 150~160mAh/g, and concentrate on land regions.Li
4ti
5o
12large 1 order of magnitude of chemical diffusion coefficient ratio carbon negative pole material at normal temperatures, discharges and recharges speed very fast.Li
4ti
5o
12compared with commercial carbon negative pole material, conventionally there is better chemical property and fail safe; Compared with alloy type negative material, more easily preparation, cost is lower.Along with popularizing gradually of new-energy automobile, Li
4ti
5o
12material will replace graphite with the cycle performance of the security performance of its almost Perfect and overlength, becomes the main product of power battery cathode material.But Li
4ti
5o
12the use of poor, shortcoming all limited this material such as tap density is lower of conductivity.
Summary of the invention
For the deficiencies in the prior art, the invention provides that a kind of tap density is high, the preparation method of the spherical lithium titanate of good rate capability.
Technical scheme of the present invention is: a kind of preparation method of high-tap density lithium titanate material, comprises the following steps:
A) with mass ratio Li: Ti: C=0.1~0.2: 1: 0~6 ratio mixed lithiated compound, titanium compound, provide the material of carbon source, take deionized water as medium, carry out ball mill mixing;
B) the good slurry of ball milling is sprayed and be dried;
C) by the high-temperature calcination under inert atmosphere of dried powder, obtain spherical lithium titanate material.
Feature of the present invention and further improvement are:
Described step is a) before carrying out ball mill mixing and add dispersant.
Described dispersant is absolute ethyl alcohol, isopropyl alcohol or acetone.
Described lithium compound is lithium carbonate, lithium hydroxide or lithia.
Described titanium compound is titanium dioxide, titanium trichloride or metatitanic acid.
The described material that carbon source is provided is Super-P, glucose, sucrose or ascorbic acid.
Described step Ball-milling Time a) is 1-10 hour.
Described step b) spray-dired inlet temperature is 100~250 ℃, and outlet temperature is 80~150 ℃.
The gas pressure that described step b) is sprayed while being dried is 0.1~0.5MPa.
Described step calcining heat c) is 600~1000 ℃, and calcination time is 10~30 hours.
Technique effect of the present invention is: by adopting water-based slurry spray-dired method, avoided potential safety hazard and environmental problem in alcohol system slurry drying process, can obtain good sphericity, mobility is strong, particle diameter is evenly distributed mixed powder.This powder can obtain after high-temperature process that tap density is high, the spherical lithium titanate material of good rate capability.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further details.
Fig. 1 is the Electronic Speculum picture that embodiment 2 prepares material.
Fig. 2 is the electrical property figure that embodiment 2 prepares material.
Fig. 3 is the XRD figure that embodiment 2 prepares material.
Embodiment
Comparative example 1:
Lithium carbonate 39.41g, titanium dioxide 100g, glucose 8.26g are mixed, add absolute ethyl alcohol, ball milling 4h on planetary ball mill, forms mixture.This mixture is placed in to 85 ℃ of baking ovens dries.Dried mixture hardens, and in 800 ℃ of nitrogen atmosphere stoves, sintering 20 hours, obtains Powdered spinel lithium titanate.Sample is through test, and tap density is only 0.76g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 170.2mAh/g.
Embodiment 1:
Lithium carbonate 39.41g, titanium dioxide 100g, glucose 8.26g are mixed in deionized water, add a certain amount of absolute ethyl alcohol to make dispersant, on planetary ball mill, ball milling 4 hours, obtains uniform slurry, slurry is sprayed dry.130 ℃ of spray dryer inlet temperatures, 85 ℃ of outlet temperatures, gas pressure 0.2MPa.Spray-dried material pattern spherical in shape, good fluidity, under 750 ℃ of nitrogen atmospheres, sintering 20 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.26g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 165.6mAh/g.
Embodiment 2:
Lithium carbonate 78.82g, titanium dioxide 200g, glucose 16.52g are mixed in deionized water, add a certain amount of absolute ethyl alcohol to make dispersant, ball milling 4h on planetary ball mill, obtains uniform slurry, slurry is sprayed dry.130 ℃ of spray dryer inlet temperatures, 95 ℃ of outlet temperatures, gas pressure 0.2MPa.Spray-dried material pattern spherical in shape, good fluidity, under 800 ℃ of nitrogen atmospheres, sintering 20 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.32g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12h, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 168mAh/g.
Embodiment 3:
Lithium carbonate 38.94g, titanium dioxide 100g, glucose 13.76g are mixed in deionized water, add a certain amount of acetone to make dispersant, on planetary ball mill, ball milling 6 hours, obtains uniform slurry, slurry is sprayed dry.140 ℃ of spray dryer inlet temperatures, 105 ℃ of outlet temperatures, gas pressure 0.3MPa.Spray-dried material pattern spherical in shape, good fluidity, under 800 ℃ of nitrogen atmospheres, sintering 17 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.21g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 172.3mAh/g.
Embodiment 4:
Lithium carbonate 78.82g, titanium dioxide 200g, glucose 16.52g are mixed in deionized water, add a certain amount of isopropyl alcohol to make dispersant, on planetary ball mill, ball milling 6 hours, obtains uniform slurry, slurry is sprayed dry.150 ℃ of spray dryer inlet temperatures, 115 ℃ of outlet temperatures, gas pressure 0.25MPa.Spray-dried material pattern spherical in shape, good fluidity, sintering 17h under 800 ℃ of nitrogen atmospheres, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.14g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 163.4mAh/g.
Embodiment 5
Lithium carbonate 39.41g, titanium dioxide 100g, glucose 8.26g are mixed in deionized water, add a certain amount of absolute ethyl alcohol to make dispersant, on planetary ball mill, ball milling 1 hour, obtains uniform slurry, slurry is sprayed dry.100 ℃ of spray dryer inlet temperatures, 80 ℃ of outlet temperatures, gas pressure 0.1MPa.Spray-dried material pattern spherical in shape, good fluidity, under 600 ℃ of nitrogen atmospheres, sintering 10 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.26g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 164.6mAh/g.
Embodiment 6
Lithium carbonate 74g, titanium dioxide 233g, glucose 525g are mixed in deionized water, add a certain amount of absolute ethyl alcohol to make dispersant, on planetary ball mill, ball milling 10 hours, obtains uniform slurry, slurry is sprayed dry.150 ℃ of spray dryer inlet temperatures, 100 ℃ of outlet temperatures, gas pressure 0.4MPa.Spray-dried material pattern spherical in shape, good fluidity, under 950 ℃ of nitrogen atmospheres, sintering 28 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.25g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 178.1mAh/g.
Embodiment 7
Lithium carbonate 74g, titanium dioxide 233g are mixed in deionized water, add a certain amount of absolute ethyl alcohol to make dispersant, on planetary ball mill, ball milling 2 hours, obtains uniform slurry, slurry is sprayed dry.125 ℃ of spray dryer inlet temperatures, 90 ℃ of outlet temperatures, gas pressure 0.3MPa.Spray-dried material pattern spherical in shape, good fluidity, under 750 ℃ of nitrogen atmospheres, sintering 16 hours, obtains spherical lithium titanate material.Sample is through test, and tap density is 1.27g/cm
3.
By the lithium titanate synthesizing, acetylene black and PVDF, ((Kynoar) adds appropriate NMP to mix in mass ratio at 85: 8: 7, is coated on aluminium foil.In vacuum drying oven, toast after 12 hours, take out compressing tablet, cut-parts.Take lithium titanate as anodal, metal lithium sheet is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC (volume ratio is 1: 1), assembled battery in the glove box that is full of argon gas, and use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 1~3V, and charge-discharge magnification is 0.2C, and recording first discharge specific capacity is 175.1mAh/g.
More than show and described basic 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; that in above-described embodiment and specification, describes 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, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. a preparation method for high-tap density lithium titanate material, is characterized in that, comprises the following steps:
A) with mass ratio Li: Ti: C=0.1~0.2: 1: 0~6 ratio mixed lithiated compound, titanium compound, provide the material of carbon source, take deionized water as medium, carry out ball mill mixing;
B) the good slurry of ball milling is sprayed and be dried;
C) by the high-temperature calcination under inert atmosphere of dried powder, obtain spherical lithium titanate material.
2. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described step is a) before carrying out ball mill mixing and add dispersant.
3. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described dispersant is absolute ethyl alcohol, isopropyl alcohol or acetone.
4. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, lithium compound is lithium carbonate, lithium hydroxide or lithia.
5. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described titanium compound is titanium dioxide, titanium trichloride or metatitanic acid.
6. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, the described material that carbon source is provided is Super-P, glucose, sucrose or ascorbic acid.
7. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described step Ball-milling Time a) is 1-10 hour.
8. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described step b) spray-dired inlet temperature is 100~250 ℃, and outlet temperature is 80~150 ℃.
9. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, the gas pressure that described step b) is sprayed while being dried is 0.1~0.5MPa.
10. the preparation method of a kind of high-tap density lithium titanate material according to claim 1, is characterized in that, described step calcining heat c) is 600~1000 ℃, and calcination time is 10~30 hours.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104393272A (en) * | 2014-10-22 | 2015-03-04 | 中国石油大学(北京) | Lithium titanate cathode composite material and preparation method |
CN106159249A (en) * | 2015-04-09 | 2016-11-23 | 中信国安盟固利动力科技有限公司 | A kind of preparation method of the nano lithium titanate of applicable industrialized production |
CN107215891A (en) * | 2017-06-28 | 2017-09-29 | 福建师范大学 | A kind of porous Li4Ti5O12The ultrasonic atomizatio preparation method of hollow ball |
CN110407248A (en) * | 2019-08-06 | 2019-11-05 | 南京兴旺新能源有限公司 | The method that anatase titanium dioxide prepares lithium titanate lithium cell cathode material |
CN110422875A (en) * | 2019-08-06 | 2019-11-08 | 南京兴旺新能源有限公司 | The preparation method of high-tap density high compacted density lithium titanate lithium cell cathode material |
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CN102074689A (en) * | 2010-12-23 | 2011-05-25 | 天津巴莫科技股份有限公司 | Method for preparing lithium iron phosphate composite material |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104393272A (en) * | 2014-10-22 | 2015-03-04 | 中国石油大学(北京) | Lithium titanate cathode composite material and preparation method |
CN106159249A (en) * | 2015-04-09 | 2016-11-23 | 中信国安盟固利动力科技有限公司 | A kind of preparation method of the nano lithium titanate of applicable industrialized production |
CN107215891A (en) * | 2017-06-28 | 2017-09-29 | 福建师范大学 | A kind of porous Li4Ti5O12The ultrasonic atomizatio preparation method of hollow ball |
CN107215891B (en) * | 2017-06-28 | 2019-04-09 | 福建师范大学 | A kind of porous Li4Ti5O12The ultrasonic atomizatio preparation method of hollow sphere |
CN110407248A (en) * | 2019-08-06 | 2019-11-05 | 南京兴旺新能源有限公司 | The method that anatase titanium dioxide prepares lithium titanate lithium cell cathode material |
CN110422875A (en) * | 2019-08-06 | 2019-11-08 | 南京兴旺新能源有限公司 | The preparation method of high-tap density high compacted density lithium titanate lithium cell cathode material |
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Application publication date: 20140604 |