CN103078087B - A kind of preparation method of lithium titanate/carbon nano tube composite cathode material - Google Patents
A kind of preparation method of lithium titanate/carbon nano tube composite cathode material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of lithium titanate/carbon nano tube composite cathode material, belong to battery material technical field.The present invention adopts chemical vapour deposition technique in lithium titanate superficial growth carbon nano-tube, its with directly in lithium titanate, there is compared with doped carbon nanometer pipe characteristics such as being uniformly dispersed, adhesion is strong, the carbon nano-tube simultaneously grown is easier forms network structure on lithium titanate surface, plays an important role to the Stability Analysis of Structures improving battery material under large multiplying power discharging condition.In the present invention lithium ion battery by the network configuration of the high conductivity and formation thereof that utilize carbon nano-tube to improve the contact probability with lithium titanate, reduce internal resistance, reduce polarization, the specific area that carbon nano-tube is larger simultaneously can improve again the imbibition liquid-keeping property of negative material, thus improves the large multiplying power discharging ability of battery and the circulation ability of battery.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, relate to a kind of preparation method of lithium titanate/carbon nano tube composite cathode material specifically, belong to battery material technical field.
Background technology
Lithium ion battery is a kind of novel energy storage cell grown up in recent years, advantages such as having extended cycle life with it, working voltage platform is steady, be cheap and pollution-free receives the concern of people, has now been widely used in the fields such as electric automobile, wind energy energy storage, mobile power station.
At present, lithium ion battery negative many employings graphite type material, but its extensive use in field of batteries due to drawbacks limit such as cycle life are poor, fail safe is low of graphite negative electrodes material.Spinel type lithium titanate is a kind of zero strain material, and having good cycle, do not react with electrolyte, charging/discharging voltage platform is steady, fail safe is high, price is low and the advantage such as easily prepare, is the desirable negative material preparing long-life, high security battery.But, point product stone-type lithium titanate material own electronic conductance and ionic conductance lower, when high current charge-discharge, capacity attenuation is fast, and high rate performance is poor, affect its application under high current charge-discharge condition, therefore improve the key that high rate performance becomes lithium titanate practicalization.
At present, Li is improved
4ti
50
12high rate performance is mainly through two approach: one is that lithium titanate is prepared into nano barium titanate lithium material; Two is doped conducting metal and material with carbon element.After Chinese patent (publication number: CN101630732A) discloses and adopts sol-gel process to be mixed with titanium, lithium compound and doped chemical solution by a certain proportion of carbon nano tube dispersion liquid, heat drying obtains gel precursor, and under inert atmosphere, sintering obtains the preparation method that the coated particle diameter of a kind of carbon nano-tube is nano level lithium titanate compound.Same Chinese patent (application number: 201110000627.3) also disclose one direct doped carbon nanometer pipe in lithium titanate and prepare anode material, thus improve the method for battery high rate performance.But, the composite negative pole material that said method is obtained, carbon nano-tube and lithium titanate just simply mix, wherein carbon nano-tube lithium titanate EDS maps uniformity and adhesion all poor, very limited to the increase rate of battery high rate performance.
Chinese patent (notification number: CN101969112A) discloses a kind of preparation method of negative material, be 100:(0.1 ~ 5 in mass ratio by negative material and catalyst) after mechanical mixture, add in thermal reaction apparatus, pass to carbon-source gas, and pass to protective gas as carrying source gas, after being warmed up to 400 ~ 900 DEG C, insulation cooling after 1 ~ 72 hour, forms the mixture of negative material, catalyst and carbon nano-tube; Be 1:(1 ~ 100 by mixture and oxidant according to mass ratio again) add in reactor, add water and stir into pastel; React 1 ~ 20 hour at again pastel being heated to 50 ~ 400 DEG C, the obtained composite negative pole material being coated with carbon nano-tube.But the method course of reaction is complicated, obtained negative material less stable, adopts oxidation step can destroy the rock-steady structure of lithium titanate self, finally affects the cycle performance of battery.
Summary of the invention
The object of this invention is to provide a kind of preparation method of lithium titanate/carbon nano tube composite cathode material, to improve high rate performance and the cycle performance of battery.
In order to realize above object, the technical solution adopted in the present invention is:
A kind of preparation method of lithium titanate/carbon nano tube composite cathode material; concrete steps are as follows: be add the catalyst fines mixing that particle diameter is 30 ~ 100nm in the lithium titanate powder of 0.3 ~ 10 μm at particle diameter; mixed-powder is heated to 600 ~ 800 DEG C under an atmosphere of hydrogen; then at temperature is 800 ~ 1200 DEG C, pass into acetylene gas; constant temperature 24 ~ 48 hours again; product after constant temperature is cooled to room temperature under inert gas shielding, removes catalyst and get final product.
Described catalyst is iron, cobalt, nickel, ferric nitrate, nickel nitrate, iron chloride or nickel chloride.
Described lithium titanate powder and the weight ratio of catalyst are lithium titanate powder: catalyst=10:(0.1 ~ 1).
Described inert gas is nitrogen, argon gas or helium.
Described lithium titanate powder can be prepared by a conventional method to obtain, and also can be commercial goods.The present invention only provides a kind of method preparing lithium titanate powder specifically; step is as follows: be lithium according to mol ratio: titanium: dispersant=1:(1.2 ~ 2): (3 ~ 8) get lithium source, titanium source and dispersant; being milled to particle size after mixing is 0.5 ~ 5 μm; dry; under inert gas shielding, dried powder is calcined 1 ~ 48 hour at 600 ~ 1000 DEG C, the powder after calcining is milled to granularity and is 0.3 ~ 10 μm and namely obtains lithium titanate powder.
Described lithium source is lithium carbonate, lithium acetate, lithium nitrate or lithium hydroxide.
Described titanium source is titanium dioxide.
Described dispersant is absolute ethyl alcohol.
Beneficial effect of the present invention:
The present invention adopts chemical vapour deposition technique in lithium titanate superficial growth carbon nano-tube, its with directly in lithium titanate, there is compared with doped carbon nanometer pipe characteristics such as being uniformly dispersed, adhesion is strong, the carbon nano-tube simultaneously grown is easier forms network configuration on lithium titanate surface, plays an important role to the Stability Analysis of Structures improving battery material under large multiplying power discharging condition.
Lithium ion battery of the present invention by the network configuration of the high conductivity and formation thereof that utilize carbon nano-tube to improve the contact probability with lithium titanate, reduce internal resistance, reduce polarization, the specific area that carbon nano-tube is larger simultaneously can improve again the imbibition liquid-keeping property of negative material, thus improves the large multiplying power discharging ability of battery and the circulation ability of battery.
In a word, adopt the composite negative pole material that chemical vapour deposition technique is prepared in lithium titanate superficial growth carbon nano-tube, the conductivity of lithium titanate and large multiplying power discharging ability can be improved, imbibition ability and the cyclical stability of battery can be improved again, good impetus is served to the extensive use of lithium titanate negative material; And preparation method is simple, quick, good stability, cost is low, is suitable for large-scale production and application.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure that the embodiment of the present invention 1 prepares negative material;
Fig. 2 is the multiplying power discharging figure of lithium ion battery in embodiment 1;
Fig. 3 is the cyclic curve figure of lithium ion battery in embodiment and comparative example.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
In the present embodiment, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:1.2:5 gets lithium carbonate, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 2 μm of powder, by powder freeze-day with constant temperature 2 hours at 100 DEG C, under argon shield, dried powder is calcined 12 hours at 800 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 1000 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 1 μm for 120 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 2 μm be that the iron catalyst of 50nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and iron is lithium titanate powder: iron=10:0.5, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 10 DEG C/min, the temperature in reactor is risen to 600 DEG C, then at temperature is 800 DEG C, pass into acetylene gas 100 minutes, constant temperature 24 hours, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, wash through the concentrated sulfuric acid afterwards, distilled water washs, 80 DEG C of dryings after 6 hours ball milling namely obtain lithium titanate/carbon nano tube composite cathode material.Surface Electronic Speculum figure refers to Fig. 1.
The negative material of the present embodiment lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1,2, and multiplying power discharging figure and cyclic curve refer to Fig. 2, Fig. 3.
Embodiment 2
In the present embodiment, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:2:3 gets lithium nitrate, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 5 μm of powder, by powder freeze-day with constant temperature 3 hours at 100 DEG C, under nitrogen protection dried powder is calcined 24 hours at 1000 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 2000 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 3 μm for 300 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 3 μm be that the Co catalysts of 100nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and cobalt is lithium titanate powder: cobalt=10:1, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 20 DEG C/min, the temperature in reactor is risen to 800 DEG C, then at temperature is 1000 DEG C, pass into acetylene gas 200 minutes, constant temperature 24 hours, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, wash through the concentrated sulfuric acid afterwards, distilled water washs, 80 DEG C of dryings after 6 hours ball milling namely obtain lithium titanate/carbon nano tube composite cathode material.
The negative material of the present embodiment lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
Embodiment 3
In the present embodiment, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:2:8 gets lithium acetate, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 0.5 μm of powder, by powder freeze-day with constant temperature 4 hours at 100 DEG C, under helium protection, dried powder is calcined 48 hours at 600 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 1500 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 0.3 μm for 200 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 0.3 μm be that the Raney nickel of 30nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and nickel is lithium titanate powder: nickel=10:0.1, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 20 DEG C/min, the temperature in reactor is risen to 600 DEG C, then at temperature is 900 DEG C, pass into acetylene gas 50 minutes, constant temperature 48 hours, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, wash through the concentrated sulfuric acid afterwards, distilled water washs, 60 DEG C of dryings after 8 hours ball milling namely obtain lithium titanate/carbon nano tube composite cathode material.
The negative material of the present embodiment lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
Embodiment 4
In the present embodiment, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:1.2:8 gets lithium hydroxide, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 0.5 μm of powder, by powder freeze-day with constant temperature 1 hour at 100 DEG C, under argon shield, dried powder is calcined 30 hours at 700 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 2000 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 1 μm for 200 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 1 μm be that the ferric nitrate catalyst of 50nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and ferric nitrate is lithium titanate powder: ferric nitrate=10:0.3, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 10 DEG C/min, the temperature in reactor is risen to 1000 DEG C, then at temperature is 850 DEG C, pass into acetylene gas 300 minutes, constant temperature 1 hour, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, wash through the concentrated sulfuric acid afterwards, distilled water washs, 60 DEG C of dryings after 8 hours ball milling namely obtain lithium titanate/carbon nano tube composite cathode material.
The negative material of the present embodiment lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
Embodiment 5
In the present embodiment, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:1.2:3 gets lithium hydroxide, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 5 μm of powder, by powder freeze-day with constant temperature 4 hours at 100 DEG C, under argon shield, dried powder is calcined 30 hours at 700 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 2000 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 10 μm for 200 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 10 μm be that the nickel chloride iron catalyst of 80nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and nickel chloride is lithium titanate powder: nickel chloride=10:0.5, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 10 DEG C/min, the temperature in reactor is risen to 800 DEG C, then at temperature is 1000 DEG C, pass into acetylene gas 60 minutes, constant temperature 24 hours, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, wash through the concentrated sulfuric acid afterwards, distilled water washs, 60 DEG C of dryings after 8 hours ball milling namely obtain lithium titanate/carbon nano tube composite cathode material.
The negative material of the present embodiment lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
Comparative example 1
The positive electrode of this comparative example lithium ion is pure lithium titanate, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
Comparative example 2
In this comparative example, lithium titanate/carbon nano tube composite cathode material is prepared by following method, and concrete steps are:
(1) preparation of lithium titanate powder: be lithium according to mol ratio: titanium: dispersant=1:1.2:3 gets lithium hydroxide, titanium dioxide and absolute ethyl alcohol, add after mixing in planetary ball mill, within 48 hours, obtaining particle diameter with the rotating speed wet ball grinding of speed 400 revs/min is 5 μm of powder, by powder freeze-day with constant temperature 10 hours at 100 DEG C, under argon shield, dried powder is calcined 30 hours at 700 DEG C, take out at powder after calcining is cooled to 100 DEG C, namely the rotating speed ball milling added again with 2000 revs/min in ultra-fine ball mill obtains the lithium titanate powder that particle diameter is 10 μm for 200 minutes,
(2) be that to add particle diameter in the lithium titanate powder of 10 μm be that the nickel chloride iron catalyst of 80nm mixes to obtain mixed-powder in step (1) particle diameter, the weight ratio of described lithium titanate powder and nickel chloride is lithium titanate powder: nickel chloride=10:0.5, mixed-powder is added in quartz tube reactor, and hydrogen is passed in described reactor, in the process passing into hydrogen, with the speed of 10 DEG C/min, the temperature in reactor is risen to 800 DEG C, then at temperature is 1000 DEG C, pass into acetylene gas 60 minutes, constant temperature 24 hours, product in constant temperature post-reactor is cooled to room temperature in a nitrogen atmosphere, again according to quality than product: concentrated hydrochloric acid, add water after the mixed acid=1:50 mixing of hydrofluoric acid and stir into starchiness, 300 DEG C of reactions 5 hours are heated to the programming rate of 5 DEG C/min, stirred once every 1 hour in course of reaction, after starchiness thing moved in centrifuge washing equipment continue to add the pH of water washing to slurry for neutral under the rotating speed of 300r/min, centrifugal dehydration makes moisture lower than 40%, dry at 100 DEG C again to moisture lower than 0.01% and get final product.
The negative material of this comparative example lithium ion adopts the above-mentioned lithium titanate/carbon nano tube composite cathode material prepared, and positive electrode is battery LiFePO4, and electrolyte is 1.0mol/LLiPF
6/ EC+DEC(V
eC: V
dEC=1: 1) (EC: ethylene carbonate, DEC: diethyl carbonate), barrier film is U.S. Celgard2300 barrier film, and the performance of obtained 2.5AH lithium ion battery refers to following table 1, and cyclic curve refers to Fig. 3.
The comparison of lithium ion battery high rate performance in table 1 embodiment and comparative example
The comparison of cycle performance of lithium ion battery in table 2 embodiment and comparative example
Claims (4)
1. the preparation method of a lithium titanate/carbon nano tube composite cathode material, it is characterized in that: concrete steps are as follows: be in the lithium titanate powder of 0.3 ~ 10 μm, add the catalyst fines mixing that particle diameter is 30 ~ 100nm at particle diameter, mixed-powder is heated to 600 ~ 800 DEG C under an atmosphere of hydrogen, then at temperature is 800 ~ 1200 DEG C, pass into acetylene gas, constant temperature 24 ~ 48 hours again, product after constant temperature is cooled to room temperature under inert gas shielding, remove catalyst and namely obtain the lithium titanate/carbon nano tube composite cathode material forming carbon nanotube network on lithium titanate surface,
Described catalyst is iron, cobalt, nickel, ferric nitrate, nickel nitrate, iron chloride or nickel chloride;
Described lithium titanate powder and the weight ratio of catalyst are lithium titanate powder: catalyst=10:(0.1 ~ 1);
The preparation process of described lithium titanate powder is as follows: be lithium according to mol ratio: titanium: dispersant=1:(1.2 ~ 2): (3 ~ 8) get lithium source, titanium source and dispersant; being milled to particle size after mixing is 0.5 ~ 5 μm; dry; under inert gas shielding, dried powder is calcined 1 ~ 48 hour at 600 ~ 1000 DEG C, the powder after calcining is milled to granularity and is 0.3 ~ 10 μm and namely obtains lithium titanate powder.
2. the preparation method of lithium titanate/carbon nano tube composite cathode material according to claim 1, is characterized in that: described lithium source is lithium carbonate, lithium acetate, lithium nitrate or lithium hydroxide.
3. the preparation method of lithium titanate/carbon nano tube composite cathode material according to claim 1, is characterized in that: described titanium source is titanium dioxide.
4. the preparation method of lithium titanate/carbon nano tube composite cathode material according to claim 1, is characterized in that: described dispersant is absolute ethyl alcohol.
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| CN103682296B (en) * | 2013-08-16 | 2015-12-09 | 东莞上海大学纳米技术研究院 | A kind of preparation method of nanoscale lithium titanate material with high specific capacity |
| CN105789620A (en) * | 2014-12-23 | 2016-07-20 | 深圳市比克电池有限公司 | Preparation method of lithium iron phosphate cathode material and lithium iron phosphate cathode material |
| CN104934589A (en) * | 2015-07-15 | 2015-09-23 | 田东 | Amorphous carbon deposit modified lithium titanate negative electrode material preparation method |
| CN106384819A (en) * | 2016-11-07 | 2017-02-08 | 珠海格力电器股份有限公司 | Carbon-coated lithium titanate material and preparation method thereof as well as lithium-ion battery |
| CN107275598B (en) * | 2017-05-27 | 2020-02-14 | 广东烛光新能源科技有限公司 | Lithium titanate negative electrode material and preparation method thereof |
| CN109980223A (en) * | 2017-12-28 | 2019-07-05 | 张家港市国泰华荣化工新材料有限公司 | A kind of lithium titanate/carbon/carbon nano tube composite material and preparation method and application |
| CN110620213B (en) * | 2018-06-20 | 2022-03-25 | 贝特瑞新材料集团股份有限公司 | Composite material of lithium tetrachloroaluminate and carbon nanotube coated lithium titanate, preparation method and application thereof |
| CN110459770A (en) * | 2019-07-31 | 2019-11-15 | 桑顿新能源科技(长沙)有限公司 | A kind of lithium titanate anode material, preparation method, cathode pole piece and lithium ion battery |
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