CN102931388A - Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery - Google Patents

Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery Download PDF

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Publication number
CN102931388A
CN102931388A CN2012104814669A CN201210481466A CN102931388A CN 102931388 A CN102931388 A CN 102931388A CN 2012104814669 A CN2012104814669 A CN 2012104814669A CN 201210481466 A CN201210481466 A CN 201210481466A CN 102931388 A CN102931388 A CN 102931388A
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rare earth
lithium titanate
earth oxide
lithium
anode material
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CN102931388B (en
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袁中直
邱彩霞
刘金成
吕正中
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Eve Energy Co Ltd
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Abstract

The invention relates to a rare earth oxide clad lithium titanate anode material, which is prepared by lithium titanate and rare earth oxide, wherein the rare earth oxide is uniformly clad on the surface of the lithium titanate. By adopting the preparation method, the rare earth oxide clad lithium titanate anode material with uniform particle size distribution can be prepared and the reaction between the lithium titanate negative electrode and an electrolyte is inhibited, so that the decomposition of the electrolyte organic solvent is prevented, flatulence problem of a lithium titanate battery is effectively solved, and the cyclicity and the multiplying power performance of the lithium titanate battery are remarkably improved.

Description

Rare earth oxide coats lithium titanate anode material and its preparation method and lithium ion battery
Technical field
The present invention relates to electrode material for lithium ion cell, particularly a kind of rare earth oxide coats lithium titanate anode material and preparation method thereof, and uses the lithium ion battery that this rare earth oxide coats the lithium titanate inorganic material.
Background technology
Lithium ion battery as one of new forms of energy is widely used in electronic product, electric motor car and the implantable medical devices owing to advantages such as having energy density height and long service life.Along with the expansion of lithium ion battery applications scope, fail safe, useful life and the high rate performance of battery material are had higher requirement.At present the conventional commercial lithium ion battery negative material mostly is greatly graphite material, but at circulation time first, the formation of graphite surface SEI film causes the loss of irreversible capacity, simultaneously, lithium ion generates Li dendrite easily in telescopiny, cause battery short circuit, brings safety problem.
Adopt spinel lithium titanate Li 4Ti 5O 12The theoretical capacity of the lithium titanate battery of making is 175mAh/g, owing to Li in charge and discharge process 4Ti 5O 12Skeleton structure changes hardly and is called as " zero strain " material.Lithium titanate battery has high (the 1. 55 V vs Li/Li of embedding lithium current potential +), the advantage that charge and discharge platform is stable, thus the generation of SEI film and separating out of Li dendrite avoided, the fail safe of Effective Raise lithium ion battery.Therefore, Li 4Ti 5O 12Very likely become one of lithium ion battery negative material of new generation.
Yet Li 4Ti 5O 12Material is as a kind of insulator, and himself lower electronic conductivity (10-9 S/cm) has limited its extensive use.In addition, the lithium ion battery ubiquity flatulence problem take lithium titanate as negative pole has also affected the application of lithium titanate battery.
Summary of the invention
Based on this, be necessary to provide a kind of rare earth oxide that has good conductivity, effectively solves the flatulence problem to coat lithium titanate anode material.
A kind of rare earth oxide coats lithium titanate anode material, and it is to be prepared from by lithium titanate and rare earth oxide, and rare earth oxide is coated on the lithium titanate surface equably.
Preferably, described rare earth oxide is at least a in lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, the gadolinium oxide.
In addition, also be necessary to provide a kind of rare earth oxide to coat lithium titanate anode material preparation method, this preparation method may further comprise the steps:
1) with lithium titanate nano particle and surfactant-dispersed in the aqueous solution, add again the nitric acid rare earth compound, obtain colloidal sol after fully stirring, obtain gel after the drying, the mol ratio of its rare earth elements and lithium titanate is 0.01:1 to 0.08:1;
2) place high temperature furnace under air atmosphere, to calcine described gel, obtain being coated with the lithium titanate anode material of rare earth oxide.
Preferably, a kind of for in lauryl sodium sulfate, sodium hexadecyl sulfate and the sodium stearyl sulfate of described surfactant.Described nitric acid rare earth compound is one or more in lanthanum nitrate, cerous nitrate, praseodymium nitrate, neodymium nitrate, samaric nitrate, europium nitrate, the gadolinium nitrate.Step 2) in, the high temperature furnace calcining heat is 700-800 ° of C, and calcination time is 1-2 hour, and the increasing extent of temperature of high temperature furnace is 2-10 ° of C/min.
In addition, also be necessary to provide a kind of lithium ion battery that adopts rare earth oxide to coat lithium titanate anode material, its positive electrode active materials is a kind of in LiMn2O4, LiFePO4 and the nickle cobalt lithium manganate ternary material, and binding agent is Kynoar, is added with conductive agent; The percentage by weight of positive active material, binding agent, conductive agent is 80-90%: 5-10%: 5-10%.
Preferably, the percentage by weight of lithium titanate, binding agent and the conductive agent of rare earth oxide coating is 85-95%: 3-10%: 1-5%.Electrolyte adopts organic mixed solution of the lithium salts of 1mol/L, lithium salts adopts lithium hexafluoro phosphate, and organic solvent is ethylene carbonate, propene carbonate, methyl ethyl carbonate is formulated, and the volume ratio of ethylene carbonate, propene carbonate, methyl ethyl carbonate is 1: 1: 1.
Utilize rare earth oxide of the present invention to coat lithium titanate anode material preparation method and can prepare the lithium titanate electrode material that rare earth oxide that particle diameter is evenly distributed coats, suppressed the reaction of lithium titanate anode and electrolyte, thereby stop the electrolyte organic solvent to decompose, efficiently solve the flatulence problem of lithium titanate.In addition, the rare earth oxide of synthesis of nano size coats the contact area that lithium titanate anode material can increase electrode and electrolyte, embed fast with embedding so that under the high magnification condition, be conducive to lithium ion, can make the cyclicity of lithium titanate electrode and forthright being significantly improved doubly.Therefore this electrode material has good conductivity, higher specific capacity and the superior cycle performance of charging and discharging.
Description of drawings
Fig. 1 is the TEM figure of embodiment 1 preparation product.
Embodiment
Below in conjunction with drawings and Examples rare earth oxide of the present invention being coated lithium titanate anode material and preparation method thereof describes.Rare earth oxide of the present invention coats lithium titanate anode material preparation method and mainly may further comprise the steps:
1) with lithium titanate nano particle and surfactant-dispersed in the aqueous solution, add again the nitric acid rare earth compound, obtain colloidal sol after fully stirring, obtain gel after dry (for example can carry out drying in baking oven), the mol ratio of its rare earth elements and lithium titanate is 0.01:1 to 0.08:1;
2) place high temperature furnace under air atmosphere, to calcine described gel, remove surfactant and acid ion, obtain being coated with the lithium titanate anode material of rare earth oxide.Preferably, the high temperature furnace calcining heat is 700-800 ° of C, and calcination time is 1-2 hour, and the increasing extent of temperature of high temperature furnace is 2-10 ° of C/min, can comparatively fast obtain the lapping of high-quality.
Wherein, surfactant can be in lauryl sodium sulfate, sodium hexadecyl sulfate and the sodium stearyl sulfate one or more.The nitric acid rare earth compound is one or more in lanthanum nitrate, cerous nitrate, praseodymium nitrate, neodymium nitrate, samaric nitrate, europium nitrate, the gadolinium nitrate.Adding surfactant can make the rare earth oxide that forms in the course of reaction be wrapped in the lithium titanate material surface, rather than be entrained in the lithium titanate material and form a kind of novel substance, its essence or bi-material, lithium titanate anode and electrolyte react to have wrapped up rear establishment, thereby stop the electrolyte organic solvent to decompose, efficiently solve the flatulence problem of lithium titanate.
Embodiment 1
With lithium titanate Li 4Ti 5O 12Nano particle and Surfactant SDS are dispersed in the aqueous solution, add lanthanum nitrate again, control La 3+With Li 4Ti 5O 12Mol ratio be 0.04:1.Obtain colloidal sol after fully stirring, dry formation gel is placed in the high temperature furnace calcines 2 hours (h) under 750 ° of C air atmospheres, removes surfactant and acid ion, obtains lanthana and coats Li 4Ti 5O 12Negative material.
Fig. 1 is the TEM figure of embodiment 1 preparation product, and the visible material surface uniform covers one deck lanthana.
Embodiment 2
With Li 4Ti 5O 12Nano particle and surfactant sodium hexadecyl sulfate are dispersed in the aqueous solution, add cerous nitrate again, control Ce 3+With Li 4Ti 5O 12Mol ratio be 0.02:1.Dry formation gel is placed in the high temperature furnace calcines 1h under 700 ° of C air atmospheres, removes surfactant and acid ion, obtains cerium oxide and coats Li 4Ti 5O 12Negative material.
Embodiment 3
With Li 4Ti 5O 12Nano particle and surfactant sodium stearyl sulfate are dispersed in the aqueous solution, add europium nitrate again, control Eu 3+With Li 4Ti 5O 12Mol ratio be 0.03:1.Dry formation gel is placed in the high temperature furnace calcines 2h under 700 ° of C air atmospheres, removes surfactant and acid ion, obtains europium oxide and coats Li 4Ti 5O 12Negative material.
Embodiment 4
Take LiMn2O4 as anodal, the lanthana for preparing with embodiment 1 coats Li 4Ti 5O 12Material is negative pole, is assembled into lithium-ion-power cell.
LiMn2O4, conductive agent Super P and binding agent polyvinylidene fluoride are pressed the 90:5:5 mass ratio to add in the blender, stir take 1-METHYLPYRROLIDONE as dispersant, scattered slurry is coated in the aluminium foil two sides, through baking, roll-in, cut and make anodal utmost point pole piece.Lanthana is coated Li 4Ti 5O 12Pressing the 95:3:2 mass ratio for negative material, conductive agent Super P and binding agent polyvinylidene fluoride adds in the blender, stir take 1-METHYLPYRROLIDONE as dispersant, scattered slurry is coated in the Copper Foil two sides, through baking, roll-in, cut and make cathode pole piece.Positive/negative plate and barrier film are carried out lamination and packaging technology, obtain battery core.Pour into electrolyte in dry air, sealing obtains lithium-ion-power cell.Battery is behind forming and capacity dividing, and in 25 ° of C of normal temperature, the 0.5C multiplying power is carried out the charge and discharge cycles test.Battery testing the results are shown in following table:
Cycle-index Capability retention Thickness swelling
1000 96% Less than 1.5%
Embodiment 5
Be anodal with LiFePO4, the cerium oxide for preparing with embodiment 2 coats Li 4Ti 5O 12Material is negative pole, is assembled into lithium-ion-power cell.
LiMn2O4, conductive agent Super P and binding agent polyvinylidene fluoride are pressed the 85:10:5 mass ratio to add in the blender, stir take 1-METHYLPYRROLIDONE as dispersant, scattered slurry is coated in the aluminium foil two sides, through baking, roll-in, cut and make anodal utmost point pole piece.Cerium oxide is coated Li 4Ti 5O 12Negative material, conductive agent Super P and binding agent polyvinylidene fluoride are pressed the 90:5:5 mass ratio and are added in the blender, stir take 1-METHYLPYRROLIDONE as dispersant, scattered slurry is coated in the Copper Foil two sides, through baking, roll-in, cut and make cathode pole piece.Positive/negative plate and barrier film are carried out lamination and packaging technology, obtain battery core.Pour into electrolyte in dry air, sealing obtains lithium-ion-power cell.Battery is behind forming and capacity dividing, and in 25 ° of C of normal temperature, the 0.5C multiplying power is carried out the charge and discharge cycles test.Battery testing the results are shown in following table:
Cycle-index Capability retention Thickness swelling
1000 97% Less than 1.5%
The result shows, uses the rare earth oxide of the inventive method preparation to coat Li 4Ti 5O 12The flatulence phenomenon of the lithium-ion-power cell that negative material is assembled into improves.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.

Claims (9)

1. the negative material of a rare earth oxide coating lithium titanate is characterized in that be prepared from by lithium titanate and rare earth oxide, rare earth oxide is coated on the lithium titanate surface equably.
2. rare earth oxide according to claim 1 coats lithium titanate anode material, it is characterized in that, described rare earth oxide is at least a in lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, the gadolinium oxide.
3. a rare earth oxide claimed in claim 1 coats lithium titanate anode material preparation method, it is characterized in that, may further comprise the steps:
1) with lithium titanate nano particle and surfactant-dispersed in the aqueous solution, add again the nitric acid rare earth compound, obtain colloidal sol after fully stirring, obtain gel after the drying, the mol ratio of its rare earth elements and lithium titanate is 0.01:1 to 0.08:1;
2) place high temperature furnace under air atmosphere, to calcine described gel, obtain being coated with the lithium titanate anode material of rare earth oxide.
4. rare earth oxide according to claim 3 coats lithium titanate anode material preparation method, it is characterized in that a kind of for in lauryl sodium sulfate, sodium hexadecyl sulfate and the sodium stearyl sulfate of described surfactant.
5. rare earth oxide according to claim 3 coats lithium titanate anode material preparation method, it is characterized in that described nitric acid rare earth compound is one or more in lanthanum nitrate, cerous nitrate, praseodymium nitrate, neodymium nitrate, samaric nitrate, europium nitrate, the gadolinium nitrate.
6. rare earth oxide according to claim 3 coats lithium titanate anode material preparation method, it is characterized in that step 2) in, the high temperature furnace calcining heat is 700-800 ° of C, and calcination time is 1-2 hour, and the increasing extent of temperature of high temperature furnace is 2-10 ° of C/min.
7. a right to use requires 1 described a kind of rare earth oxide to coat the lithium ion battery of lithium titanate anode material, it is characterized in that, positive electrode active materials is a kind of in LiMn2O4, LiFePO4 and the nickle cobalt lithium manganate ternary material, and binding agent is Kynoar, is added with conductive agent; The percentage by weight of positive active material, binding agent, conductive agent is 80-90%: 5-10%: 5-10%.
8. lithium ion battery according to claim 7 is characterized in that, in negative plate, the percentage by weight of lithium titanate, binding agent and conductive agent that rare earth oxide coats is 85-95%: 3-10%: 1-5%.
9. lithium ion battery according to claim 7, it is characterized in that, electrolyte adopts organic mixed solution of the lithium salts of 1mol/L, lithium salts adopts lithium hexafluoro phosphate, organic solvent is ethylene carbonate, propene carbonate, methyl ethyl carbonate is formulated, and the volume ratio of ethylene carbonate, propene carbonate, methyl ethyl carbonate is 1: 1: 1.
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Cited By (16)

* Cited by examiner, † Cited by third party
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CN103456944A (en) * 2013-09-04 2013-12-18 中国海洋石油总公司 Modifying method of ternary anode material
CN103682301A (en) * 2013-12-04 2014-03-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of nanometer lithium titanate covered with double highly-conductive materials
CN104112860A (en) * 2013-04-22 2014-10-22 万向电动汽车有限公司 Preparation method of lithium ion battery positive electrode modified material
CN104505502A (en) * 2014-12-26 2015-04-08 宁夏共享新能源材料有限公司 Lithium titanate composite negative material for lithium ion battery and preparation method of lithium titanate composite negative material
CN104779364A (en) * 2015-03-31 2015-07-15 中新能科技发展有限公司 Anode of lithium ion battery, preparation method of anode and lithium ion battery
CN104966822A (en) * 2015-06-16 2015-10-07 东莞市翔丰华电池材料有限公司 Multilayer coated lithium titanate cathode material of lithium ion battery and preparation method of multilayer coated lithium titanate cathode material
CN105336939A (en) * 2015-09-30 2016-02-17 中国科学院过程工程研究所 Coating modification method of lithium titanate and lithium ion battery thereof
US20160218355A1 (en) * 2015-01-27 2016-07-28 Dongfang Electric Corporation Method for Preparing Carbon-Coated Lithium Titanate
CN105932238A (en) * 2016-05-11 2016-09-07 新疆大学 Preparation method of lithium ion battery negative electrode material lithium titanate coated by spherical rare earth metal oxide
CN106920952A (en) * 2017-04-29 2017-07-04 合肥国轩高科动力能源有限公司 Preparation method of modified lithium nickel manganese oxide positive electrode material
CN109384457A (en) * 2018-09-30 2019-02-26 镇江华智睿安物联科技有限公司 A kind of electrode material and preparation method thereof for mass spectrum ionization source
CN110854383A (en) * 2019-11-08 2020-02-28 昆山宝创新能源科技有限公司 Modified ternary cathode material and preparation method thereof
CN111477859A (en) * 2020-05-09 2020-07-31 宁波锋成纳米科技有限公司 Composite positive electrode material, preparation method thereof and water-based secondary battery
CN112054181A (en) * 2020-09-28 2020-12-08 珠海冠宇电池股份有限公司 Lithium supplement agent and application thereof
CN114583126A (en) * 2022-02-24 2022-06-03 北京工业大学 La2O3-Co/AB composite material and preparation method and application thereof
CN115275170A (en) * 2022-09-02 2022-11-01 永州昊利新材料科技有限公司 Preparation method of cerium dioxide modified lithium manganese iron phosphate electrode material

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CN101764209A (en) * 2010-01-04 2010-06-30 苏州星恒电源有限公司 Lithium titanate composite electrode material with surface coating layer

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CN104112860A (en) * 2013-04-22 2014-10-22 万向电动汽车有限公司 Preparation method of lithium ion battery positive electrode modified material
CN104112860B (en) * 2013-04-22 2017-02-08 万向电动汽车有限公司 Preparation method of lithium ion battery positive electrode modified material
CN103456944B (en) * 2013-09-04 2015-11-11 中国海洋石油总公司 A kind of method of modifying of tertiary cathode material
CN103456944A (en) * 2013-09-04 2013-12-18 中国海洋石油总公司 Modifying method of ternary anode material
CN103682301A (en) * 2013-12-04 2014-03-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of nanometer lithium titanate covered with double highly-conductive materials
CN103682301B (en) * 2013-12-04 2015-10-28 上海纳米技术及应用国家工程研究中心有限公司 The preparation method of the nano lithium titanate that a kind of pair of high conductive material is coated
CN104505502A (en) * 2014-12-26 2015-04-08 宁夏共享新能源材料有限公司 Lithium titanate composite negative material for lithium ion battery and preparation method of lithium titanate composite negative material
US9923199B2 (en) * 2015-01-27 2018-03-20 Dongfang Electric Corporation Method for preparing carbon-coated lithium titanate
US20160218355A1 (en) * 2015-01-27 2016-07-28 Dongfang Electric Corporation Method for Preparing Carbon-Coated Lithium Titanate
CN104779364A (en) * 2015-03-31 2015-07-15 中新能科技发展有限公司 Anode of lithium ion battery, preparation method of anode and lithium ion battery
CN104966822A (en) * 2015-06-16 2015-10-07 东莞市翔丰华电池材料有限公司 Multilayer coated lithium titanate cathode material of lithium ion battery and preparation method of multilayer coated lithium titanate cathode material
CN105336939A (en) * 2015-09-30 2016-02-17 中国科学院过程工程研究所 Coating modification method of lithium titanate and lithium ion battery thereof
CN105932238A (en) * 2016-05-11 2016-09-07 新疆大学 Preparation method of lithium ion battery negative electrode material lithium titanate coated by spherical rare earth metal oxide
CN106920952A (en) * 2017-04-29 2017-07-04 合肥国轩高科动力能源有限公司 Preparation method of modified lithium nickel manganese oxide positive electrode material
CN106920952B (en) * 2017-04-29 2019-03-29 合肥国轩高科动力能源有限公司 Preparation method of modified lithium nickel manganese oxide positive electrode material
CN109384457A (en) * 2018-09-30 2019-02-26 镇江华智睿安物联科技有限公司 A kind of electrode material and preparation method thereof for mass spectrum ionization source
CN110854383A (en) * 2019-11-08 2020-02-28 昆山宝创新能源科技有限公司 Modified ternary cathode material and preparation method thereof
CN111477859A (en) * 2020-05-09 2020-07-31 宁波锋成纳米科技有限公司 Composite positive electrode material, preparation method thereof and water-based secondary battery
CN112054181A (en) * 2020-09-28 2020-12-08 珠海冠宇电池股份有限公司 Lithium supplement agent and application thereof
CN114583126A (en) * 2022-02-24 2022-06-03 北京工业大学 La2O3-Co/AB composite material and preparation method and application thereof
CN114583126B (en) * 2022-02-24 2023-11-24 北京工业大学 La (La) 2 O 3 Co/AB composite material and preparation method and application thereof
CN115275170A (en) * 2022-09-02 2022-11-01 永州昊利新材料科技有限公司 Preparation method of cerium dioxide modified lithium manganese iron phosphate electrode material

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