CN101431154B - Lithium titanate/C composite electrode material and method for producing the same - Google Patents

Lithium titanate/C composite electrode material and method for producing the same Download PDF

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CN101431154B
CN101431154B CN2008103065271A CN200810306527A CN101431154B CN 101431154 B CN101431154 B CN 101431154B CN 2008103065271 A CN2008103065271 A CN 2008103065271A CN 200810306527 A CN200810306527 A CN 200810306527A CN 101431154 B CN101431154 B CN 101431154B
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lithium
electrode material
combination electrode
lithium titanate
polymeric carboxylic
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CN101431154A (en
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潘中来
刘力
林子吉
杨克润
胡学步
邓正华
索继栓
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Sichuan Yindile Materials Science and Technology Group Co., Ltd.
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CHENGDU ZHONGKE LAIFANG ENERGY TECHNOLOGY Co Ltd
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a lithium titanate/C composite electrode material and a preparation method thereof, belonging to the field of electrochemical power sources. The technical problem to be solved by the invention is that the Li4Ti5O12/C composite electrode material with the simple preparation method and the high charge-discharge rate is provided. The technical proposal is as follows: titanium dioxide is taken as a titanium source, polymeric lithium carboxylic salt is taken as a lithium source and a carbon source, and the Li4Ti5O12/C composite electrode material with the high charge-discharge rate performance is prepared by solid phase reaction. The method has low cost and simple process, and the prepared Li4Ti5O12/C composite material has high charge-discharge rate performance and greater gram capacity, thereby being capable of being widely applied in lithium-ion batteries which are needed by mobile communication, various portable electronic devices and various electric cars.

Description

Lithium titanate/C combination electrode material and preparation method thereof
Technical field
The present invention relates to a kind of lithium titanate/C combination electrode material and preparation method thereof, lithium titanate electrode composite material of particularly a kind of high charge-discharge magnification that is used for lithium ion battery and preparation method thereof belongs to field of electrochemical power source.
Background technology
Along with electronic equipment develops to miniaturization and microminiaturization, the research of lithium ion battery more and more obtains paying attention to application.Along with the development of electric automobile, the high power type electrokinetic cell also becomes the focus of Study on Li-ion batteries using.Spinel type lithium titanate Li 4Ti 5O 12Electrode material as novel energy storage cell comes into one's own day by day, and this is because spinel-type Li 4Ti 5O 12Be a kind of " zero strain " material, it can keep the high stability of crystal structure in lithium ion embedding-Tuo embedding process.Li 4Ti 5O 12Its specific structure characteristics have been avoided in charge and discharge cycles making Li owing to the flexible repeatedly of electrode material causes structural damage 4Ti 5O 12Has excellent cycle performance.
Restriction Li 4Ti 5O 12The major obstacle that material is used is that high-rate charge-discharge capability is poor, and the battery capacity decay is bigger under the high power charging-discharging condition.Therefore to make Li 4Ti 5O 12Can reach practicability, need to improve the high rate capability that discharges and recharges of lithium titanate material, also will keep its high reversible electrochemical capacity and good cyclical stability simultaneously.
Can improve Li at present 4Ti 5O 12The method of high rate performance mainly contains: preparation nanometer particle size Li 4Ti 5O 12, Li 4Ti 5O 12Bulk doped and introducing conductive phase.
1. synthesis of nano size Li 4Ti 5O 12, can increase the contact area of electrode active material and electrolyte, help lithium ion and embed fast and deviate from, can shorten the migration path of lithium ion simultaneously, reduce the diffusional resistance of lithium ion, guarantee that lithium ion can embed and deviate from fast under the high magnification condition.At present Li that adopt sol-gel process to prepare nanometer particle size more 4Ti 5O 12Sol-gel process have that chemical uniformity is good, heat treatment temperature is low, the powder granule particle diameter is little and be evenly distributed, the powder sintering performance is good, course of reaction is easy to control, equipment is simple, but contraction is big when dry, the suitability for industrialized production difficulty is big, synthesis cycle is long, is difficult to realize that large-scale industrial production is to satisfy a large amount of requirements of energy field.
2. to Li 4Ti 5O 12Carry out metal cation and mix, to improve Li 4Ti 5O 12The electronic conductivity of material.Studies show that, can better improve Li by cation doping 4Ti 5O 12Conductivity, but for improving Li 4Ti 5O 12Discharge and recharge the high rate capability DeGrain.Part is mixed and has also been reduced the chemical property of material to a certain extent simultaneously.
3. introduce high conductive phase, to Li 4Ti 5O 12Introduce higher second phase (as metal, carbon) of a small amount of conductivity in the powder and serve as conducting medium, evenly disperse or be coated on Li 4Ti 5O 12Particle surface, preparation Li 4Ti 5O 12/ high conductive phase composite material to strengthen the electron conduction ability between the principal phase particle, improves the electric conductivity of combination electrode material.Wen Zhaoyin (publication number: CN1588677A) disclose to Li 4Ti 5O 12The middle Ag that adds has improved its high rate capability effectively as the electron conduction agent.Yet, improve Li as additive with Ag 4Ti 5O 12Conductivity cost height, be difficult to satisfy a large amount of requirements of energy field.
In J.Power Sources 126 (2004) 163, A.Guerfi etc. adopt the higher material with carbon element of conductivity to Li by discovering 4Ti 5O 12Modification can improve its high rate performance, is to Li because of carbon 4Ti 5O 12Modifying function mainly show as: 1. make reducing agent, promote the reaction in the body powder, accelerate lithium ion at Li 4Ti 5O 12Interparticle diffusion; 2. high temperature suppresses the increase effect of particle down, and promotes to generate the small-particle aggregate of chain structure; 3. serve as conducting bridge, form the conductive network that connects the active particle material, improve electronic conductivity; 4. increase electrically contacting between particle and the particle, relax because the internal stress that particle is grown up and produced.Yue Min (publication number: CN 101000960A) disclose employing nano-sized carbon carbon coated material or doping vario-property agent doping vario-property Li 4Ti 5O 12, improved Li effectively 4Ti 5O 12Capacity performance and cycle performance.(publication number: CN1978524 A) disclose employing high conduction high-specific surface area coalescence benzene or phenolic resins Pintsch process, preparation carbon coats Li to Wang Rongshun 4Ti 5O 12Composite material, be 155-162mAh/g during its first discharge specific capacity 0.3C, be 140-150mAh/g during 2C, be 95-110mAh/g during 9C.Yet said method adopts additional carbon, and coats by physical method, and the carbon that is difficult to the processability homogeneous coats compound Li 4Ti 5O 12Electrode material, and, also increased the preparation difficulty owing to increased reacting phase.
Do not see that at present with the polymeric carboxylic lithium salts be lithium source and carbon source, the Li that the chemical method original position is synthetic 4Ti 5O 12The report of/C combination electrode material.
Summary of the invention
Technical problem to be solved by this invention provides the Li that a kind of preparation method simply has the high charge-discharge magnification performance 4Ti 5O 12/ C combination electrode material.
Technical scheme of the present invention: with titanium dioxide is the titanium source, and the polymeric carboxylic lithium salts is the lithium source, and the carbon skeleton pyrolysis product of polymeric carboxylic lithium salts is a carbon source, prepares the Li with high charge-discharge magnification performance by solid phase reaction 4Ti 5O 12/ C combination electrode material.
Particularly, the present invention mixes the polymeric carboxylic Aqueous Lithium Salts with titanium dioxide, adopts mechanical mixture to mill to make it to reach fully and is uniformly dispersed, and drying obtains presoma, carries out the synthetic Li of high temperature solid state reaction under inert atmosphere protection 4Ti 5O 12/ C combination electrode material.Wherein, the temperature of solid phase reaction is 600 ℃～900 ℃, and best temperature range is 750 ℃～850 ℃; Reaction time is 4～24 hours, and best time range is 10～18 hours.
Wherein, titanium dioxide is anatase crystal, and diameter of particle is 0.01～5.00 μ m.
Described polymeric carboxylic lithium salts is meant the lithium salts that the water soluble polymer carboxylic acid forms, as Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium or their copolymer, average molecular weight range is 2000～100000, and its optimum range is 5000～20000.
The mechanical mixture milling can be industry dispersion and crumbling methods commonly used such as ball milling, colloid mill, sand milling, does not have special appointment in the present invention.
Inert protective atmosphere can be inert gases such as nitrogen, argon gas.
Li prepared according to the methods of the invention 4Ti 5O 12/ C combination electrode material be the ash to black powder, carbon content is 1.0～15.0%, optimum range is 3.0～6.0%, the gram volume 〉=140mAh/g of material when 0.2C discharges and recharges, the gram volume 〉=100mAh/g of material when 8.0C discharges and recharges.
Adopt the prepared Li of preparation method provided by the invention 4Ti 5O 12/ C composite material has high charge, and has bigger gram volume.This method has characteristics such as cheap, that operation is simple, product property is good.The Li for preparing by this method 4Ti 5O 12/ C combination electrode material can be widely used in mobile communication and various portable electric appts and the required lithium ion battery of various electric motor car.
Embodiment
Li of the present invention 4Ti 5O 12The preparation method of/C combination electrode material is as follows:
A, preparation polymeric carboxylic lithium salts: in the polymeric carboxylic aqueous solution, add LiOHH 2O carries out neutralization reaction, obtains the aqueous solution of polymeric carboxylic lithium salts;
B, in lithium: titanium mol ratio is 4.0～4.2: 5 ratio, will add titanium dioxide in the polymeric carboxylic Aqueous Lithium Salts and mix, and adopts mechanical mixture to mill to make it to reach fully and is uniformly dispersed, and drying obtains presoma;
C, presoma carry out 4～24 hours synthetic Li of solid phase reaction under 600 ℃～900 ℃ inert atmosphere protections 4Ti 5O 12/ C combination electrode material.
Below by the more specifically detailed description of indefiniteness embodiment, will help understanding of the present invention, protection scope of the present invention is not subjected to the qualification of these embodiment, and protection scope of the present invention is decided by claim.
Embodiment 1 Li of the present invention 4Ti 5O 12The preparation of/C composite material
Taking by weighing 500 gram mean molecule quantities is that 10000 concentration is 30% the polyacrylic acid aqueous solution, adds 88 gram LiOHH 2O neutralizes, and obtains the Lithium polyacrylate aqueous solution, and then by stoichiometric proportion Li: Ti=4.02: 5 add 208 gram titanium dioxide (TiO 2) powder, stirring ball-milling disperseed 4 hours, obtained Lithium polyacrylate-titanium dioxide (PAALi-TiO 2) mixture predecessor slurry.Slurry obtains presoma after 120 ℃ of left and right sides temperature oven dry.Presoma placed carry out high temperature solid state reaction in the nitrogen atmosphere protection tube furnace, the control heating rate is 5 ℃/min, is warming up to 800 ℃ and be incubated 10 hours, takes out behind the natural cooling.
The electrochemical property test method: embodiment 1 prepared lithium titanate material, conductive carbon black and aqueous binder LA132 are evenly mixed by 85: 10: 5 mass ratioes, be coated on the Copper Foil, standby through vacuum tank oven dry 6 hours.In being filled with the glove box of argon gas, be assembled into button cell and carry out battery performance test, used electrolyte is 1mol/L LiPF6/EC+EMC+DMC (1: 1: 1), metal lithium sheet is to electrode and reference electrode, on Neware battery performance test instrument, carry out 0.2C, 1.0C, 2.0C, 4.0C, 8.0C the high rate performance test, the charging/discharging voltage scope is 1.0V～3.0V.
Lithium titanate material gram volume by embodiment 1 method and proportioning preparation is 162mAh/g, and the gram volume of material is 125mAh/g when 8.0C discharges and recharges, and carbon content is 4.86%.
Embodiment 2 Li of the present invention 4Ti 5O 12The preparation of/C composite material
Taking by weighing 500 gram mean molecule quantities is that 5000 concentration is 40% the poly aqueous solution, adds 145 gram LiOHH 2O neutralizes, and obtains the poly lithium aqueous solution, and then by stoichiometric proportion Li: Ti=4.02: 5 add 340 gram titanium dioxide (TiO 2) powder, stirring ball-milling disperseed 4 hours, obtained poly lithium-titanium dioxide (PMALi-TiO 2) mixture predecessor slurry.Slurry obtains presoma after 120 ℃ of left and right sides temperature oven dry.Presoma placed carry out high temperature solid state reaction in the nitrogen atmosphere protection tube furnace, the control heating rate is 5 ℃/min, is warming up to 800 ℃ and be incubated 10 hours, takes out behind the natural cooling.
The electric performance test method is identical with embodiment 1.
Lithium titanate material gram volume by embodiment 2 methods and proportioning preparation is 165mAh/g, and the gram volume of material is 122mAh/g when 8.0C discharges and recharges, and carbon content is 3.54%.
Embodiment 3 Li of the present invention 4Ti 5O 12The preparation of/C composite material
Other condition is identical with embodiment 1, and only different is that the polyacrylic acid that the polymeric carboxylic lithium salts needs replaces with poly-(acrylic acid-acrylonitrile) copolymer, wherein acrylic acid: acrylonitrile is 8: 2.
The electric performance test method is identical with embodiment 1.
Lithium titanate material gram volume by embodiment 3 methods and proportioning preparation is 160mAh/g, and the gram volume of material is 130mAh/g when 8.0C discharges and recharges, and carbon content is 5.63%.
Embodiment 4 Li of the present invention 4Ti 5O 12The preparation of/C composite material
Other condition is identical with embodiment 1, and only different is that polyacrylic mean molecule quantity is 50000.
The electric performance test method is identical with embodiment 1.
Lithium titanate material gram volume by embodiment 4 methods and proportioning preparation is 164mAh/g, and the gram volume of material is 124mAh/g when 8.0C discharges and recharges, and carbon content is 5.07%.
Embodiment 5 Li of the present invention 4Ti 5O 12The preparation of/C composite material
Other condition is identical with embodiment 2, and only different is that the polyacrylic acid that the polymeric carboxylic lithium salts needs replaces with poly-(maleic acid-acrylonitrile) copolymer, wherein maleic acid: acrylonitrile is 8: 2.
The electric performance test method is identical with embodiment 1.
Lithium titanate material gram volume by embodiment 5 methods and proportioning preparation is 163mAh/g, and the gram volume of material is 133mAh/g when 8.0C discharges and recharges, and carbon content is 6.05%.
Embodiment 6 Li4Ti of the present invention 5O 12The preparation of/C composite material
Other condition is identical with embodiment 1, and only different is that the polyacrylic acid that the polymeric carboxylic lithium needs replaces with polymethylacrylic acid, and its mean molecule quantity is 5000.
The electric performance test method is identical with embodiment 1.
Lithium titanate material gram volume by embodiment 6 methods and proportioning preparation is 155mAh/g, and the gram volume of material is 118mAh/g when 8.0C discharges and recharges, and carbon content is 4.05%.

Claims (7)

1. prepare the method for lithium titanate/C combination electrode material, it is characterized in that:
A, preparation polymeric carboxylic lithium salts: in the polymeric carboxylic aqueous solution, add LiOHH 2O carries out neutralization reaction, obtains the aqueous solution of polymeric carboxylic lithium salts; Described polymeric carboxylic lithium salts is meant the lithium salts that the water soluble polymer carboxylic acid forms;
B, in lithium: titanium mol ratio is 4.0～4.2: 5 ratio, will add titanium dioxide in the polymeric carboxylic Aqueous Lithium Salts and mix, and adopts mechanical mixture to mill to make it to reach fully and is uniformly dispersed, and drying obtains presoma;
C, presoma carry out 4～24 hours synthetic Li of solid phase reaction under 600 ℃～900 ℃ inert atmosphere protections 4Ti 5O 12/ C combination electrode material.
2. the method for preparing lithium titanate/C combination electrode material according to claim 1 is characterized in that:
The described polymeric carboxylic lithium salts of a step is Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium or their copolymer, and average molecular weight range is 2000～100000;
The described titanium dioxide of b step is anatase crystal, and diameter of particle is 0.01～5.00 μ m.
3. the method for preparing lithium titanate/C combination electrode material according to claim 2 is characterized in that: the average molecular weight range of described polymeric carboxylic lithium salts is 5000～20000.
4. the method for preparing lithium titanate/C combination electrode material according to claim 1 is characterized in that:
The described mechanical mixture milling of b step is ball milling, colloid mill or sand milling.
5. the method for preparing lithium titanate/C combination electrode material according to claim 1 is characterized in that:
The described inert protective atmosphere of c step is nitrogen or argon gas; The temperature of solid phase reaction is 750 ℃～850 ℃; Reaction time is 10～18 hours.
6. lithium titanate/C combination electrode material of preparing of each described method for preparing lithium titanate/C combination electrode material of claim 1-5, it is characterized in that: C content is 1.0～15.0wt%.
7. lithium titanate according to claim 6/C combination electrode material is characterized in that: C content is 3.0～6.0%.
CN2008103065271A 2008-12-25 2008-12-25 Lithium titanate/C composite electrode material and method for producing the same Active CN101431154B (en)

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US20120261622A1 (en) * 2009-12-22 2012-10-18 Masatoshi Honma Lithium titanate, manufacturing method therefor, slurry used in said manufacturing method, electrode active material containing said lithium titanate, and lithium secondary battery using said electrode active material
CN102299333A (en) * 2011-07-14 2011-12-28 上海微纳科技有限公司 Preparation method of carbon coated Li4Ti5O12 nano cathode material
CN102496704B (en) * 2011-12-08 2014-04-23 中信国安盟固利电源技术有限公司 Lithium titanate/titanium black anode material and preparation method thereof
CN103872305B (en) * 2014-03-24 2016-01-20 四川兴能新材料有限公司 The coated Li of polyelectrolyte 4ti 5o 12the preparation method of negative material
CN104466152B (en) * 2014-12-02 2018-02-23 赵县强能电源有限公司 A kind of preparation method of lithium ionic cell cathode material lithium titanate
CN104882589B (en) * 2015-05-28 2017-03-22 清华大学深圳研究生院 Carbon-coated ternary anode material and preparing method thereof, and lithium ion battery
CN104993118A (en) * 2015-06-16 2015-10-21 田东 Synthesizing method for lithium-ion negative electrode material of Li4Ti5O12/C
CN110534730A (en) * 2019-08-26 2019-12-03 高朗科技(湖州)有限公司 The preparation method of lithium titanate material
CN114171733B (en) * 2021-11-30 2024-02-13 中国科学院过程工程研究所 Coated lithium ion battery positive electrode material and preparation method and application thereof

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