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Preparation method of lithium titanate negative electrode material with micro-nanostructure

A negative electrode material and micro-nano structure technology, applied in the field of preparation of lithium titanate negative electrode materials, can solve the problems of high raw material, solvent and operation requirements, complicated operation process, etc., and achieve good dispersion, high stability, and excellent large rate Effect of Discharge Characteristics

Inactive Publication Date: 2013-05-15
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this preparation method operation process is more complicated, and the raw material that needs, solvent and operating requirement are also higher

Method used

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  • Preparation method of lithium titanate negative electrode material with micro-nanostructure
  • Preparation method of lithium titanate negative electrode material with micro-nanostructure
  • Preparation method of lithium titanate negative electrode material with micro-nanostructure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Take 100ml of absolute ethanol into a 250ml three-necked flask, add 0.4ml of 0.1M PEG4000 solution to it, and then slowly drop 2ml of tetrabutyl titanate into it. Access N 2 , Under agitation, react for 2h, stand for 8h, filter to obtain white precipitate, wash the precipitate three times with absolute ethanol, and dry it in a vacuum oven at 60°C to prepare spherical titanium dioxide precursor. figure 1 It is the prepared spherical titanium dioxide precursor. Weigh 0.15g of titanium dioxide precursor, add it to 15ml of ethanol and water mixed solution (volume ratio is 1:1), then add 0.0629g of LiOH·H to it 2 O, after stirring for 15 minutes, transfer to a 50ml hydrothermal reactor, react at 180°C for 12 hours to obtain a white powder, and put it in a muffle furnace at 500°C for two hours to prepare pure phase lithium titanate with micro-nano structure Powder. figure 2 Shown is the XRD pattern of the obtained lithium titanate powder. It can be seen that the po...

Embodiment 2

[0027] Example 2: Take 100ml of absolute ethanol into a 250ml three-necked flask, add 0.4ml of 0.1M PEG1000 solution to it, and then slowly drop 2ml of isopropyl titanate into it. Access N 2 , Under agitation, react for 2h, stand for 8h, filter to obtain white precipitate, wash the precipitate three times with absolute ethanol, and dry it in a vacuum oven at 60°C to prepare spherical titanium dioxide precursor. Weigh 0.15g of titanium dioxide precursor, add it to 15ml of ethanol and water mixed solution (volume ratio is 3:2), then add 0.065g of LiOH·H to it 2 O, after stirring for 15 minutes, transfer to a 50ml hydrothermal reactor, react at 180°C for 5 hours to obtain a white powder, and place it in a muffle furnace at 500°C for 1 hour to prepare pure phase lithium titanate with micro-nano structure Powder.

Embodiment 3

[0028] Example 3: Take 100ml of absolute ethanol into a 250ml three-necked flask, add 0.4ml of 0.1M PEG10000 solution to it, and then slowly drop 2ml of butyl titanate into it. Access N 2 , Under stirring, react for 4h, stand for 2h, filter to obtain white precipitate, wash the precipitate three times with absolute ethanol, and dry it in a vacuum oven at 60°C to prepare spherical titanium dioxide precursor. Weigh 0.15g of titanium dioxide precursor, add it to 15ml of ethanol and water mixed solution (volume ratio 4:1), then add 0.0629g of LiOH·H to it 2 O, after stirring for 15 minutes, transfer to a 50ml hydrothermal reactor, react at 150°C for 12 hours to obtain a white powder, and place it in a muffle furnace at 450°C for 4 hours to prepare pure phase lithium titanate with micro-nano structure Powder.

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Abstract

The invention provides a preparation method of a lithium titanate negative electrode material with a micro-nanostructure. The method is characterized by comprising the steps of: a. preparing a titanium dioxide precursor; b. under a stirring state, adding the titanium dioxide precursor into water, or a mixed solution of water and ethanol, further adding lithium hydroxide under a stirring state, then transferring the solution into a hydrothermal reaction kettle to undergo a hydrothermal reaction, leaving the solution to natural cooling to room temperature, then carrying out filtering, washing, drying and calcination, thus obtaining the lithium titanate negative electrode material end product. The method adopts spherical titanium dioxide as an initial raw material, and takes water or ethanol as a reaction solvent to prepare plush-like hollow microspheres with an average diameter of 1.5-3 micrometers through a hydrothermal reaction and a calcination treatment. The microspheres are composed of nanosheets. The material also shows certain mesoporous characteristic, the inner micropores of the material have an average diameter of 5-15nm. The lithium titanate negative electrode material with a micro-nanostructure involved in the invention has the characteristic of excellent high-rate discharge, and is suitable for use by power batteries.

Description

Technical field [0001] The invention relates to a method for preparing battery electrode materials, in particular to a method for preparing lithium titanate negative electrode materials with a micro-nano structure. Background technique [0002] Recently, as a new type of negative electrode material, spinel-type lithium titanate has the advantages of "zero strain" and good cycle performance, and has gradually become a research focus. Compared with traditional carbon anode materials, the "zero strain" material-lithium titanate has a potential of 1.55V relative to lithium metal, which is much higher than the reduction voltage of most electrolytes, which can avoid electrolyte reduction and passivation film formation At the same time, it can prevent the generation of metallic lithium, and has very excellent cycle performance and safety performance. Therefore, lithium titanate material can be used as a negative electrode material for lithium-ion batteries and has been widely focused b...

Claims

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Application Information

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IPC IPC(8): H01M4/485
CPCY02E60/122Y02E60/10
Inventor 王瑾王丹何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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