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Method of producing spinel structured lithium titanate

A technology of structural lithium titanate and spinel, which is applied in chemical instruments and methods, lithium compounds, titanium oxide/hydroxide, etc., can solve the problems of difficult industrial transformation, complicated process, and high cost of raw materials, and achieve cheap raw materials, The effect of easy to obtain raw materials and simple process

Inactive Publication Date: 2008-05-07
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a complex aqueous solution sol with inorganic titanium, lithium compounds and cheap organic complexing agents as basic raw materials in order to overcome the shortcomings of the existing sol-gel method, such as high raw material cost, complicated process, and difficult industrial transformation. -The method of gel synthesis lithium titanate

Method used

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  • Method of producing spinel structured lithium titanate

Examples

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Embodiment 1

[0011] Commercially available analytically pure TiCl 4 (concentration is 99.9%) slowly add in ice-water bath 3mol / L hydrochloric acid solution and make TiCl 4 reserve solution. Separately take 5.0ml TiCl 4 Three parts of the stock solution were added to the TiO 2 ·nH 2 O precipitated completely. Filter with a medium-speed filter paper, wash until there is no chloride ion, dry the filter paper and the precipitate at 800°C for 4 hours, weigh after cooling, and determine the TiCl concentration in the standby solution accordingly. 4 The content is equivalent to 0.28g / ml titanium dioxide.

[0012] Take the above TiCl 4 15.3ml of stock solution, using the same steps as above to obtain TiO 2 ·nH 2 O, disperse with a small amount of water, add 12g citric acid, 1.700gLiOH·H 2 O, adjust pH ≈ 5 with commercially available analytically pure ammonia (concentration: 25% to 28%). Next, the mixture was stirred at about 80°C, and the TiO 2 ·nH 2 O gradually dissolves to form a solu...

Embodiment 2

[0018] Disperse 7.0g of titanium dioxide industrial intermediate metatitanic acid (moisture content 30%) in deionized water, add 10g of commercially available analytical pure reagent oxalic acid, 1.5g of commercially available analytical pure reagent lithium carbonate successively, and the rest of the operating steps are the same as in Example 1 same. Prepared Li 4 Ti 5 o 12 The average particle size of the powder is about 2.37 μm, and the XRD measurement results show that it has a spinel structure without other impurity phases. Charge and discharge at a constant current with a current rate of 0.5C. After 20 cycles, its specific capacity is greater than 122mAh / g.

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Abstract

The invention discloses a preparation method for spinel structure lithium titanate. The invention is characterized in that titanate and lithium inorganic compound and organic acid or ammonium salt with low cost is taken as the raw material; the gel precursor is compounded through simple composite water solution sol and gel route; the precursor reacts for 1 to 8 hours by ranging from 500 DEG C to 800DEG so as to obtain loosened porous nanometer spinel structure lithium titanate(Li4Ti5O12) with granularity range from 0.5 to 10 micrometers and without impurity. The granularity of the product reaches 100nm to 500nm after being grinded through a planetary ball mill. The performances such as the circulated volt-ampere characteristics, the high current performance and the Ohm essential resistance of products prepared with the invention are obviously superior to that of products prepared through solid state reaction, with circulated rate capability of 100mAh / g to 165mAh / g, thereby being high performance cathode materials for lithium ion battery. The invention has the advantages of low raw materials cost, simple procedure, suitable industrial transformation, and excellent product performance.

Description

technical field [0001] The invention relates to a method for preparing electrode materials, in particular to a method for preparing lithium titanate with a spinel structure. Background technique [0002] Lithium titanate is a high-performance lithium-ion battery anode material with long life, high-current charging and discharging, safety, and environmental protection. Using it to replace carbon anode materials can fundamentally eliminate the safety hazards of lithium-ion batteries and make lithium-ion batteries The cycle performance and fast charge and discharge performance of the ion battery are greatly improved. The solid-state reaction method is the main way to prepare lithium titanate, and its product is a micron or submicron powder with poor high-current performance. Sol-gel technology is an effective method to prepare high-performance spinel lithium titanate. The product has small particle size, concentrated particle size distribution, cycle life and electrochemical p...

Claims

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Application Information

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IPC IPC(8): C01G23/04C01D15/00
Inventor 杨建文钟海云钟晖赵绚戴艳阳
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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