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Method for preparing nano-crystal lithium-titanium composite oxide

A lithium-titanium composite and oxide technology, which is applied in the fields of titanium compounds, nanostructure manufacturing, chemical instruments and methods, etc., can solve the problems of complex cost process, industrialized amplification of material agglomeration, etc., and achieves abundant reserves, regular morphology, The obvious effect of the platform

Inactive Publication Date: 2007-10-24
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ohzuku, Nakahara et al. synthesized pure-phase spinel Li by a solid-state method 4 Ti 5 o 12 , Bach, Shen et al. used butyl titanate as raw material to synthesize nano-Li by sol-gel method. 4 Ti 5 o 12 Particles, Robertson, Chen, Sun, Guerfi ​​et al. for Li 4 Ti 5 o 12 Element doping has been carried out, but most of the above works cannot overcome technical problems such as high cost, complicated process, material agglomeration and industrial scale-up

Method used

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  • Method for preparing nano-crystal lithium-titanium composite oxide
  • Method for preparing nano-crystal lithium-titanium composite oxide
  • Method for preparing nano-crystal lithium-titanium composite oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Dissolve 5g of titanium powder in 30ml of 30% hydrogen peroxide solution at a temperature of 0-5°C, add 3.6g of lithium hydroxide monohydrate as an aqueous solution, and add a certain amount of activated carbon powder , stir well. After adding 5% ammonia water, it was transferred to a water bath at 50° C. and stirred thoroughly for 30 minutes, and the mixture was placed in an oven and dried directly to obtain a precursor. After the precursor was heat-treated at 300°C for 4 hours, it was heated to 800°C for 24 hours and then cooled and ground to obtain a nanocrystalline lithium-titanium composite oxide with a spinel structure, Li 4 Ti 5 o 12 The content is more than 99%. The average grain size of the lithium-titanium composite oxide is about 20nm, and the specific surface area is 70m 2 / g, under 0.1C charge and discharge conditions, its reversible lithium intercalation capacity is 165mAh / g, under 100C charge and discharge conditions, the capacity retention...

Embodiment 2

[0021] Embodiment 2: under the temperature environment of 3~8 ℃, 16g TiOSO 4 Dissolve in 50ml of 30% hydrogen peroxide solution, add 5.3g of lithium acetate as an aqueous solution, add a certain amount of starch, and stir thoroughly. After adding 5% ammonia water until the solution is alkaline, transfer it to a water bath at 100°C for a full reaction for 60 minutes, and place it in an oven to dry directly to obtain a precursor. The precursor was heat-treated at 200°C for 4 hours, heated to 900°C for 20 hours, cooled and ground to obtain a nanocrystalline lithium-titanium composite oxide with a spinel structure, Li 4 Ti 5 o 12 Content 92%. The average grain size of the nanocrystalline lithium-titanium composite oxide is about 50nm, and the specific surface area is 45m 2 / g, under 0.1C charge and discharge conditions, its reversible lithium intercalation capacity is 160mAh / g, and the capacity retention rate under 100C charge and discharge conditions is 62%.

Embodiment 3

[0022] Example 3: 10g TiO(OH) 2 Mix with 50ml of 30% hydrogen peroxide solution, add 6g of lithium nitrate as an aqueous solution, add a certain amount of polypropylene glycol, and stir well. After adding 5% ammonia water until the solution is alkaline, transfer it to a water bath at 100°C for a full reaction for 60 minutes, and place it in an oven to dry directly to obtain a precursor. The precursor was heat-treated at 400°C for 2 hours, heated to 1000°C for 20 hours, cooled and ground to obtain a nanocrystalline lithium-titanium composite oxide with a spinel structure, Li 4 Ti 5 o 12 Content 96%. The average grain size of the nanocrystalline lithium-titanium composite oxide is about 90nm, and the specific surface area is 30m 2 / g, under 0.1C charge and discharge conditions, its reversible lithium intercalation capacity is 165mAh / g, and the capacity retention rate under 100C charge and discharge conditions is 60%.

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Abstract

The invention discloses a making method of nanometer crystal Li-Ti composite oxide, which comprises the following steps: adopting titanium powder or titanium compound as raw material; blending the materials with 30% hydrogen peroxidate under low temperature; adding certain quantity of lithium salt solution and moulder; stirring evenly; reacting under water bath condition at 50-100 deg. c completely; drying the composite system directly to produce predecessor; proceeding heat disposal for the predecessor at 200-400 deg. c for 2-6h; heating to 600-1000 deg. c; sintering 8-36h; cooling; grinding; obtaining the nanometer crystal Li-Ti composite oxide with spinel structure and the content of Li4Ti5O12 over 90%; controlling the even grain size of the product between 15nm and 100nm and specific surface area between 10 and 100m2 / g due to different aperture shape of moulds, sintering time and temperatures; making the reversible specific capacity of the product over 160mAh / g under 0. 1C charging and discharging condition; keeping the capacity maintaining rate between 50% and 70% under discharging condition at 100deg. c as ideal negative electrode material of lithium ion dynamic battery and lithium ion super-capacitance.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation technology and green energy, and relates to a nanocrystalline lithium-titanium composite oxide negative electrode material applied to lithium-ion secondary batteries and lithium-ion supercapacitors. Background technique [0002] Lithium Titanium Oxide Li 4 Ti 5 o 12 It is a lithium-ion embedded electrode material with a spinel structure, which is characterized by a small change in the lattice constant of the material (volume change is less than 1%, also known as zero-strain material) with the insertion and extraction of lithium ions; The lithium intercalation potential of the material is relatively positive (1.55V, vs. Li + / Li), it is not easy to cause the precipitation of lithium dendrites during the charging and discharging process, and it will not form an SEI film with high impedance due to the reduction and decomposition of the electrolyte; Li 4 Ti 5 o 12 with Li 7 Ti 5 o 12 T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00C01G1/02C04B35/622C04B35/462H01M4/48B82B3/00
CPCY02E60/10
Inventor 吴锋苏岳锋陈实包丽颖徐斌穆道斌陈人杰王国庆
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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