Method for preparing lithium titanate powder

A technology of lithium titanate and powder, which is applied in the field of preparation of lithium titanate powder, can solve the problems of difficult removal and high energy consumption, and achieve the effects of simple process, excellent electrochemical performance and low production cost

Inactive Publication Date: 2011-11-23
HUNAN UNIV OF HUMANITIES SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method adds molten salt impurities during the synthesis process, and these impurities are difficult to remove during washing
[0010] Other methods: such as Chinese patent CN101704681A, although the raw material cost of this method is low, but the preparation process requires freeze crystallization and high-energy ball milling, and the energy consumption is relatively high

Method used

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  • Method for preparing lithium titanate powder
  • Method for preparing lithium titanate powder
  • Method for preparing lithium titanate powder

Examples

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Effect test

Embodiment 1

[0028] Embodiment 1: the preparation method of lithium titanate powder described in this embodiment comprises the following steps:

[0029] 1), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh an excess of 0-5% lithium acetate, make a solution, and then add to Li + Add appropriate amount of complexing agent and burning agent EDTA to the solution to prepare uniform mixed solution A.

[0030] 2), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh metatitanic acid (H 2 TiO 3 ), and then add an appropriate amount of hydrogen peroxide (hydrogen peroxide, H 2 o 2 ) and excess ammonia (NH 3 ×H 2 O), after the metatitanic acid is completely dissolved, add a certain amount of citric acid to obtain a uniform mixed solution B.

[0031] 3) Mix the A and B solutions prepared above, then concentrate the mixed solution into a jelly, dry it at 100°C to make a powder, or make a powder by spray drying.

[0032] 4) Put the powder (or directly ...

Embodiment 2

[0034] 1), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh an excess of 0-5% lithium nitrate to make solution A.

[0035] 2), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh metatitanic acid (H 2 TiO 3 ), and then add an appropriate amount of hydrogen peroxide (hydrogen peroxide, H 2 o 2 ) and excess ammonia (NH 3 ×H 2 O), after the metatitanic acid is completely dissolved, add a certain amount of oxalic acid to obtain a uniform mixed solution B.

[0036] 3) Mix the A and B solutions prepared above, then concentrate the mixed solution to a jelly, and dry it at 120°C to make a powder, or make a powder by spray drying.

[0037] 4) Put the above-prepared powder (or the directly-prepared jelly) into a muffle furnace and calcinate at 800°C for 4 hours to obtain Li 4 Ti 5 o 12 Powder.

Embodiment 3

[0039] 1), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh an excess of 0-5% lithium acetate, make a solution, and then add to Li + Add appropriate amount of complexing agent and burning agent EDTA to the solution to prepare uniform mixed solution A.

[0040] 2), according to the chemical formula Li 4 Ti 5 o 12 Metering ratio Weigh metatitanic acid (H 2 TiO 3 ), and then add an appropriate amount of hydrogen peroxide (hydrogen peroxide, H 2 o 2 ) and excess ammonia (NH 3 ×H 2 O), after the metatitanic acid is completely dissolved, add a certain amount of citric acid to obtain a uniform mixed solution B.

[0041] 3) Mix the A and B solutions prepared above, then concentrate the mixed solution to a jelly, dry it at 100°C to make a powder, or make a powder by spray drying.

[0042] 4) Put the above-prepared powder (or the directly-prepared jelly) into a muffle furnace and calcinate at 800°C for 6 hours to obtain Li 4 Ti 5 o 12 Powder.

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Abstract

The invention discloses a method for preparing lithium titanate powder. The method comprises the following steps of: weighing an excessive amount of lithium salt (lithium nitrate or lithium acetate and the like) with the concentration 0-5 percent according to the metering ratio of a chemical formula Li4Ti5O12, preparing the lithium salt into a solution, and adding an appropriate amount of coordination agent and incendiary agent (such as citric acid or EDTA (Ethylene Diamine Tetraacetic Acid) or oxalic acid ) into the Li<+> solution to obtain a uniform mixed solution A; weighing metatitanic acid (H2TiO3) according to the metering ratio of a chemical formula Li4Ti5O12, adding an appropriate amount of hydrogen peroxide (oxyful, H2O2) and an excessive amount of ammonia water (NH3*H2O), and adding a certain amount of coordination agent and incendiary agent (such as citric acid or oxalic acid or EDTA and the like) after the metatitanic acid is fully dissolved to obtain a uniform mixed solution B; mixing the prepared solution A with the solution B, heating and concentrating into jelly (or drying into powder at a temperature between 50 DEG C and 200 DEG C); and putting the powder obtained by drying (or the directly prepared jelly) into a muffle furnace for calcining at a temperature between 500 DEG C and 900 DEG C for 1-10 hours to obtain Li4Ti5O12 powder. The method has the advantages of simple technical process, low cost of raw materials, easiness for control of stoichiometric ratio and excellent electrochemical performance of a product, and is suitable for mass production; and the particle diameter of the powder is between 50 nanometers and 500 nanometers.

Description

[0001] technical field [0002] The invention belongs to the technical field of preparation of negative electrode materials of lithium ion batteries, and relates to a preparation method of lithium titanate powder with a spinel structure. technical background [0003] Lithium titanate (LTO) is a highly stable and high rate lithium-ion secondary battery negative electrode material with a spinel structure. Lithium titanate is used as a lithium ion negative electrode material. During charging and discharging, lithium ion intercalation and deintercalation have almost no effect on the material structure, so it is called a "zero strain" material, and after 100 charge and discharge cycles, the capacity loss is very small . Moreover, lithium titanate does not react with the electrolyte, and the charge and discharge voltage platform is stable. Compared with the carbon anode materials that currently occupy a large market share, Li 4 Ti 5 o 12 The equilibrium potential is high, avoi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00
Inventor 彭秧锡
Owner HUNAN UNIV OF HUMANITIES SCI & TECH
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