Nano lithium titanate for Negative electrode material of cell or electrochemical vessel, and its and titanium dioxide composite preparing method

A technology of nano-lithium titanate and titanium dioxide, which is applied in the field of nano-materials, can solve the problems of difficulty in large-scale industrial production, large volume changes of alloy-type negative electrodes, and complicated preparation methods of carbon materials, and achieve good cycle stability and excellent electrochemical performance. , the effect of shortening the reaction time

Active Publication Date: 2007-11-14
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, commercialized lithium-ion battery negative electrode materials mostly use various lithium-intercalated carbon materials. Carbon materials have some disadvantages as lithium-ion battery negative electrode materials: First, the potential of carbon materials is very close to that of metal lithium. When the battery is overcharged, Metal lithium may precipitate on the surface of the carbon electrode to form lithium dendrites, which may cause a short circuit; second, the first charge and discharge efficiency is low; third, it interacts with the electrolyte; fourth, there is obvious voltage hysteresis; fifth, the carbon material preparation method It is more complicated; six is ​​that although the alloy negative electrode material generally has a high specific capacity, the repeated intercalation and desorption of lithium leads to a large volume change of the alloy negative electrode during the charging and discharging process, and gradually pulverizes and fails, so the cycle performance is poor
However, the sol-gel method requires expensive organic alkoxides as precursors, and the process is complex, so it is difficult to achieve large-scale industrial production to meet the large demand in the energy field

Method used

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  • Nano lithium titanate for Negative electrode material of cell or electrochemical vessel, and its and titanium dioxide composite preparing method
  • Nano lithium titanate for Negative electrode material of cell or electrochemical vessel, and its and titanium dioxide composite preparing method
  • Nano lithium titanate for Negative electrode material of cell or electrochemical vessel, and its and titanium dioxide composite preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1, get 3g TiO 2 , slowly add 300ml of NaOH solution with a concentration of 3mol / L into a polytetrafluoroethylene container, control the temperature at 120°C, stir and add a reflux condenser, react for 24 hours to obtain nanotube sodium titanate, wash the above titanate Sodium nanotubes to a pH of 13, then suction filtered, dried, mixed with 12g of lithium nitrate and ground, melted and heated at 500°C for 2.5 hours, washed and dried to obtain a spinel lithium titanate product; as shown in Figure 1, The diameter of the nano-lithium titanate is about 8-10nm, and the length is about 100nm.

Embodiment 2

[0032] Example 2, get 10g of metatitanic acid (industrial slurry, weight content 44.04%, produced by Yida Fine Chemical Co., Ltd.), and slowly add 100ml of KOH solution with a concentration of 10mol / L into a polytetrafluoroethylene reaction vessel, Put it in a microwave oven, set it to medium-low heat (750W, work for 10s, stop for 12s), mechanically stir, add a reflux condenser, react for 6 hours to get potassium titanate nanowires with a diameter of several nanometers, wash until the pH is 7 and dry , and then take 25g of lithium citrate and lithium chloride mixture (weight ratio is 1:3) mixed with dried potassium titanate / titanic acid composite fiber, and put it in a sintering furnace, under the protection of nitrogen, melt and heat at 1000°C Exchanged for 2 hours, the lithium titanate-titanium dioxide composite was obtained, the morphology of which is shown in Figure 2; the crystal structure is shown in Figure 3, which contains two different crystal forms: cubic spinel struc...

Embodiment 3

[0033] Embodiment 3, get 3g TiO 2 , slowly add 300ml of NaOH solution with a concentration of 10mol / L into a polytetrafluoroethylene container, control the temperature at 120°C, stir and add a reflux condenser, react for 24 hours to obtain nanotube sodium titanate, wash the above titanate Sodium nanotubes to a pH of 6, then suction filtered and dried; then ground with a mixture of 5 g of lithium hydroxide and lithium nitrate (1:5 by weight), melted, heated and exchanged at 451°C for 48 hours, washed and dried to obtain the product Composite of spinel lithium titanate and titanium dioxide.

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Abstract

This invention discloses nano lithium titanate for cell cathode material and compound with titanium dioxide, its preparation method is that: (1) compound containing titanium and sodium hydroxide (potassium) react by heating, cool, wash by water to different pH value, dry to obtain sodium(potassium) titanate or sodium (potassium) titanate compound; (2) mix the product from step (1) and inorganic lithium salt, heat it up to 451- 1,000 degree C to fuse exchange react for 30minute -48 hours, or mix the product from step (1) and organic or inorganic lithium salt under inert gas and heat it to150-1,000 degree C to fuse exchange react for30 minute - 48 hours, then wash by water and dry to obtain the finished product.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and relates to a method for preparing nanometer lithium titanate and its compound with titanium dioxide, which are used as battery or electrochemical container negative electrode materials. Background technique [0002] At present, commercialized lithium-ion battery negative electrode materials mostly use various lithium-intercalated carbon materials. Carbon materials have some disadvantages as lithium-ion battery negative electrode materials: First, the potential of carbon materials is very close to that of metal lithium. When the battery is overcharged, Metal lithium may precipitate on the surface of the carbon electrode to form lithium dendrites, which may cause a short circuit; second, the first charge and discharge efficiency is low; third, it interacts with the electrolyte; fourth, there is obvious voltage hysteresis; fifth, the carbon material preparation method It is more comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04C01G23/00C01G23/047
CPCY02E60/12Y02E60/10
Inventor 张经纬李明王晓冬张顺利金振声吴志申张治军
Owner HENAN UNIVERSITY
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