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Preparation method of lithium titanate-carbon nanotube electrode material

A technology of carbon nanotubes and electrode materials, which is applied in the direction of battery electrodes, nanotechnology, nanotechnology, etc., can solve the problems of large capacitance attenuation, pore blockage, difficulty in uniform dispersion of graphene, etc., to improve the performance of conductive electrons, reduce the Migration impedance, the effect of overcoming capacity fading and poor rate performance

Active Publication Date: 2019-12-24
ZHEJIANG FOLTA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, lithium titanate anode materials (Li 4 Ti 5 o 12 ), which has the advantages of high safety performance, good high-rate charge-discharge performance, excellent cycle performance, and stable charge-discharge voltage. However, Li 4 Ti 5 o 12 The electronic conductivity of the material itself (and the mobility of lithium ions) is low, so the capacitance attenuation is large and the rate performance is poor when charging and discharging at a high current.
[0003] In the existing technology, lithium titanate is mainly mixed with conductive agents with excellent conductivity, such as graphene and activated carbon, to prepare electrode materials, so as to make up for the defect of lithium titanate material's lack of electron conductivity.
Usually, the preparation of lithium titanate-activated carbon composite electrode materials will cause pore blockage, reduce the pore volume of activated carbon and the specific surface area of ​​the composite material, which is not conducive to the full play of adsorption performance.
In the preparation process of lithium titanate-graphene composite electrode, limited by the preparation method, graphene is difficult to disperse evenly in the slurry, and the battery capacity and charge-discharge rate of the electrode are not ideal.

Method used

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  • Preparation method of lithium titanate-carbon nanotube electrode material
  • Preparation method of lithium titanate-carbon nanotube electrode material
  • Preparation method of lithium titanate-carbon nanotube electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Weigh 3.1251g of carbon nanotubes (dispersed in NMP, the content is 4wt%) and NMP mixture and 12.5062g of ethylene glycol, and add them to a 100mL reaction kettle, and then add 4.457g in the glove box Isopropyl titanate; put it in a homogeneous reactor at 200°C for 12 hours at a rotation speed of 10r / min after ventilation to obtain slurry A;

[0035] (2) Cool the slurry A, then suction filter, wash with 10mL of methanol, take 2.0190g of the product and put it in the reaction kettle, then add 5.0746g of lithium hydroxide aqueous solution (1.0mol / L), and then place it at 200°C In a homogeneous reactor, the reaction speed was 10r / min for 12h; slurry B was obtained;

[0036] (3) Suction filter slurry B to separate the solid, take the solid and place it in a tube furnace, and heat it at 700°C 2 Sintering in the atmosphere for 4h to obtain the lithium titanate electrode material;

[0037] (4) placing the NMP solution (3wt%) of lithium titanate electrode material, PVDF, ...

Embodiment 2

[0048] The difference between the second embodiment and the first embodiment is that the sintering temperature in the step (3) of the second embodiment is changed to 400° C., and the others are the same as those of the first embodiment, which will not be repeated here.

Embodiment 3

[0050] The difference between the third embodiment and the first embodiment is that the sintering temperature in the step (3) of the second embodiment is changed to 500° C., and the others are the same as the first embodiment, and will not be repeated here.

[0051] Attached from the manual Figure 7 with Figure 8 It can be analyzed that in the comparison between the above-mentioned Example 2 and Example 3, the capacity of the material sintered at 500°C is higher than that at 400°C at different sintering temperatures, at 0.4A·g -1 When the current density, the former is 250mAh / g, and the latter is 200mAh / g. The lithium titanate-carbon nanotube material prepared by sintering at 500°C can maintain a capacity of 250mAh / g at a high rate current density, and the attenuation is small. In the existing commercial product Li 4 Ti 5 o 12 At 1C, it can only reach about 170mAh / g or even less.

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Abstract

The invention discloses a novel method for preparing a lithium titanate-carbon nanotube electrode material. The method comprises the steps that S1 an NMP mixture containing 4 wt% carbon nanotube, dioland titanate are added to a homogeneous reaction device, and stirred for polymerization reaction to form polymer mixed slurry A with the carbon nanotube and suction filtration slurry A, and washing with a methanol solution is carried out to acquire a polymer M with the carbon nanotube; S2 the carbon nanotube-containing polymer M and a lithium compound are mixed and dissolved in water, and then placed in a homogeneous reactor, and after stirring and hydrolysis reaction, mixture slurry B and suction filtration slurry B are acquired and washed with a methanol solution to acquire a solid N; and S3 after the solid N is sintered in an inert atmosphere in a high-temperature furnace, the lithium titanate-carbon nanotube electrode material is acquired. The lithium titanate-carbon nanotube electrode material prepared by the preparation method provided by the invention can realize charge and discharge under large current, and overcomes the problems of capacity attenuation and poor rate performance during charge and discharge under large current.

Description

technical field [0001] The invention relates to lithium titanate-carbon nanotube, a lithium ion battery negative electrode material with high capacity and deep charge and discharge capability, and a preparation method thereof. Background technique [0002] At present, lithium titanate anode materials (Li 4 Ti 5 o 12 ), which has the advantages of high safety performance, good high-rate charge-discharge performance, excellent cycle performance, and stable charge-discharge voltage. However, Li 4 Ti 5 o 12 The electronic conductivity of the material itself (and the mobility of lithium ions) is low, so the capacitance decays greatly and the rate performance is poor when charging and discharging with a large current. [0003] In the prior art, lithium titanate is mainly mixed with a conductive agent with excellent conductivity, such as graphene, activated carbon, etc., to prepare electrode materials, so as to make up for the defect of lithium titanate material's insufficient...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/485H01M4/625H01M10/0525Y02E60/10
Inventor 不公告发明人
Owner ZHEJIANG FOLTA TECH CO LTD
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