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Method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation

A nano-lithium titanate and carbon coating technology, applied in the field of nano-lithium titanate, can solve the problems of affecting battery performance, easy enrichment of electrons, and poor conductivity, so as to improve mixing uniformity, alleviate particle agglomeration, and improve electrical conductivity sexual effect

Inactive Publication Date: 2012-12-12
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But spinel Li 4 Ti 5 o 12 There is a problem with the anode material used as lithium-ion battery - because Li 4 Ti 5 o 12 is an intrinsic conductivity of only 10 -9 S / cm insulating material, so the conductivity is extremely poor, resulting in easy enrichment of electrons under high-rate discharge conditions, resulting in electrode polarization and limiting the insertion and extraction of lithium ions, which ultimately affects the performance of the battery.

Method used

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  • Method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation
  • Method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation
  • Method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Example 1: Add 3.4mL of HNO to 170.16mL of absolute ethanol 3As a hydrolysis inhibitor of tetrabutyl titanate, solution A was obtained; according to the molar ratio Li:Ti=4.2:5, 8.508g tetra-n-butyl titanate (analytical pure) and 0.776g lithium carbonate ( Analytical pure, pre-ground into fine powder), magnetically stirred until completely dissolved and clear; according to the molar ratio of EDTA:CA=1:2, weigh 13.443g EDTA and 17.677gCA, drop 10mL distilled water for pre-mixing, then add 35.4mL ammonia water dissolved to obtain solution B. Mix solution A and solution B, adjust the pH of the mixed solution to 10 with ammonia water, and continue stirring until the mixed solution becomes clear as a sol. Continue heating and stirring at 100°C for 3 hours. After the sol becomes a transparent gel, put it in a blast oven at 240°C and dry it for 12 hours to obtain a black fluffy Li 4 Ti 5 o 12 Precursor. The precursor is ground and put into a muffle furnace, and calcined a...

Embodiment 2

[0031] Example 2: Mix 85.08mL of absolute ethanol with 8.51mL of deionized water according to the volume ratio of 1:0.1, add 8.51mL of hydrochloric acid as the hydrolysis inhibitor of the subsequent reactant, and obtain solution A; according to the molar ratio Li:Ti= 4.3:5, put 8.508g tetra-n-butyl titanate (analytical pure) and 1.419g lithium acetate (analytical pure) into solution A, stir magnetically until completely dissolved and become clear; according to the molar ratio, EDTA:CA=1: 1.5. Weigh 6.795g EDTA and 6.701g CA, drop 5mL of distilled water for pre-mixing, then add 15.21mL of ammonia water to dissolve, and obtain solution B. Mix solution A and solution B, adjust the pH of the mixed solution to 7 with ammonia water, and continue stirring until the mixed solution becomes clear as a sol. Continue heating and stirring at 80°C for 4 hours. After the sol becomes a transparent gel, put it in a blast oven at 240°C and dry it for 12 hours to obtain a black fluffy Li 4 Ti ...

Embodiment 3

[0032] Example 3: Mix 112.18mL of absolute ethanol with 22.44mL of deionized water according to the volume ratio of 1:0.2, add 22.44mL of acetic acid as the hydrolysis inhibitor of the subsequent reactant, and obtain solution A; according to the molar ratio Li:Ti= 4.0:5, put 7.105g tetraisopropyl titanate (analytical pure) and 1.38g lithium nitrate (analytical pure) into solution A, stir magnetically until completely dissolved and become clear; according to the molar ratio, EDTA:CA=1: 1. Weigh 13.151g of EDTA and 8.646g of CA, add 10mL of distilled water to pre-mix, then add 24.24mL of ammonia water to dissolve, and obtain solution B. Mix solution A and solution B, adjust the pH of the mixed solution to 8 with ammonia water, and continue stirring until the mixed solution becomes clear as a sol. Continue heating and stirring at 60°C for 5 hours. After the sol becomes a transparent gel, put it in a blast oven at 240°C and dry it for 12 hours to obtain a black fluffy Li 4 Ti 5 ...

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Abstract

The invention discloses a method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation. Pure Li4Ti5O12 is prepared by a sol-gel method and an EDTA-CA dual chelator joint complexation method; and a Li4Ti5O12 / C anode material is obtained by performing further carbon coating. The lithium titanate particles prepared by the method have a good dispersion effect; and a particle aggregation phenomenon is remarkably improved. The prepared Li4Ti5O12 / C has high charging and discharging specific capacity and stable cycle performance; at room temperature, when the ratio is 1C, the initial discharging capacity of the Li4Ti5O12 / C reaches 174.5 mAh / g which is close to the theoretical capacity; and when the ratio is 10C, the discharging capacity of the Li4Ti5O12 / C reaches over 140 mAh / g. Moreover, the Li4Ti5O12 / C has stable cycle performance, and has a wide application prospect in the field of civil portable electronic equipment and power equipment.

Description

technical field [0001] The invention relates to a method for preparing lithium titanate, a negative electrode material for lithium ion secondary batteries, in particular to a method for preparing carbon coating by sol-gel method using ethylenediaminetetraacetic acid-citric acid (EDTA-CA) combined complexation The method of nano lithium titanate. Background technique [0002] At present, lithium-ion batteries occupy the largest market share of rechargeable batteries, and are widely used in civilian portable electronic devices such as mobile phones, notebook computers, and MP3 players. In recent years, people have gradually applied them to power equipment. Hybrid vehicles have also entered the market. The negative electrode materials used in commercially available lithium-ion batteries are mostly carbon materials, but it has a fatal problem, that is, when the battery is charged quickly or overcharged, metal lithium may be precipitated on the surface of the electrode material,...

Claims

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Application Information

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IPC IPC(8): H01M4/485H01M4/62C01G23/00B82Y30/00
CPCY02E60/122Y02E60/10
Inventor 张遥遥张春明王丹吴晓燕余震汪元元何丹农
Owner SHANGHAI JIAO TONG UNIV
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