Method of producing spinel structured lithium titanate

A technology for structural lithium titanate and spinel, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of long process, difficult control of reaction conditions, high cost of raw materials, etc.

Inactive Publication Date: 2009-04-08
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a one-step solid-phase reaction synthesis of lithium titanate using titanium dioxide, lithium carbonate and carbon black as raw materials in order to overcome the shortcomings of the existing lithium titanate synthesis method, which are difficult to control the reaction conditions, the process is long, and the cost of raw materials is high. Methods

Method used

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  • Method of producing spinel structured lithium titanate
  • Method of producing spinel structured lithium titanate
  • Method of producing spinel structured lithium titanate

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Accurately weigh 3.228g of commercially available analytical reagent titanium dioxide (mainly anatase, titanium dioxide ≥ 99.0%), lithium carbonate 0.762g (lithium carbonate ≥ 97.0%), carbon black 0.400g (ash content ≤ 0.2%), in 200mL agate Planetary ball milling in a tank for 2 hours, put the mixture in a 25mL corundum boat, place it in a tube furnace, feed in commercially available argon gas (Ar ≥ 99.996%) with a flow rate of 20L / h, react the material at 900°C for 30 hours, and cool naturally Take it out after reaching room temperature, transfer it to an agate ball mill jar and fill it with argon gas, and grind it with a planetary ball mill for 2 hours to obtain a dark blue spinel lithium titanate powder product. X-ray diffractometer measurement result shows that product is mainly spinel structure (see attached figure 1 ); its simulated battery Li / LiTi 2 o 4 There is a group of redox reversible peaks in the cyclic voltammetry curve, and the reaction potential is 1.3...

Embodiment 2

[0014] Accurately weigh 322.800g of commercially available analytical reagent titanium dioxide (mainly anatase, titanium dioxide ≥ 99.0%), lithium carbonate 76.200g (lithium carbonate ≥ 97.0%), carbon black 38.000g (ash content ≤ 0.2%), in 500mL agate Planetary ball milling in batches for 2 hours in a jar, put the mixture in a 500mL graphite crucible, put it in a SL63-7B vacuum carbon tube electric furnace (produced by Shanghai Electric Furnace Factory), and pump the vacuum to 10 -1 Pa, heated to 900°C for 8 hours, cooled to room temperature, taken out, transferred to an agate ball mill jar filled with argon, and ground for 2 hours with a planetary ball mill to obtain a dark blue spinel lithium titanate powder product. Its X-ray diffractometer measurement results and electrochemical performance are similar to those of Example 1, wherein the reversible lithium intercalation reaction potential is 1.34V, the specific capacity is 160mAh / g, and the charge and discharge performance i...

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Abstract

The invention discloses a method for preparing lithium titanate with a spinel structure. Lithium carbonate, titanium dioxide and carbon black which are low in price and easy to obtain are used as raw materials; the lithium titanate (LiTi2O4) is synthesized by a one-step solid phase reaction method. The raw materials are fully mixed and react for 4 to 36 hours at a temperature between 700 and 1,300 DEG C under an argon atmosphere or a vacuum atmosphere to prepare the lithium titanate (LiTi2O4) with the spinel structure which is pure or contains a little carbon black. A product is ground through a planetary ball mill; the granularity of the product reaches between 0.5 and 5 mu m; and the cycle ratio capacity of the product reaches between 100 and 160 mAh / g. The method has a simple process and low prices of raw materials and is suitable for industrial production; and the product has excellent electrochemical performance and can be used a material for the cathode of a high-performance lithium ion battery.

Description

technical field [0001] The present invention relates to a kind of preparation method of lithium-ion battery electrode material, especially refers to the synthesis of spinel structure lithium titanate (LiTiO) which can be used as lithium-ion battery negative electrode material by one-step solid phase reaction using cheap and easy-to-obtain raw materials. 2 o 4 )Methods. Background technique [0002] Lithium titanate refers to Li-Ti-O series oxygen compounds, wherein, the spinel structure ( ) LiTi 2 o 4 , Li 4 Ti 5 o 12 and Li of the orthorhombite structure (Pbnm) 2 Ti 3 o 7 All have good reversible lithium intercalation reaction characteristics, and can be used as anode materials for lithium-ion batteries. LiTi with spinel structure 2 o 4 It has the advantages of low lithium intercalation potential, stable charge and discharge performance, good conductivity, and high current performance, and is expected to be used as anode material for long-life and high-power li...

Claims

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Application Information

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IPC IPC(8): C01G23/00
Inventor 杨建文赵江陈永珍杨正晓
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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