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Preparation method for Nb-doped Li4T5O12 nano material

A nanomaterial and equipment technology, applied in the field of non-hydrolyzable sol-gel method, can solve the problems of affecting battery performance, easy enrichment of electrons, poor conductivity, etc., achieve stable cycle performance, avoid the use of complexing agents and strong acid catalysts, The effect of improving performance

Inactive Publication Date: 2014-11-19
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Preparation method for Nb-doped Li4T5O12 nano material
  • Preparation method for Nb-doped Li4T5O12 nano material
  • Preparation method for Nb-doped Li4T5O12 nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Add 86mL of absolute ethanol into the reflux equipment, according to the molar ratio Li:Nb:Ti=4.0:0.01:4.99, add 5.692g tetraethyl titanate (analytical pure), 0.0135g chloride Niobium (analytical pure, anti-hydrolysis) and 0.8478g lithium chloride (analytical pure, pre-ground into fine powder), magnetically stirred until completely dissolved and in a clear state; then stirred for 20 minutes, and then the solution was first heated at 70°C, until reflux begins. Then adjust the temperature to 100°C, and reflux for 24 hours until the gel is formed, then stop the reflux, and take out the gel after cooling. The gel was dried at 200 °C to remove the solvent to obtain a black fluffy precursor of a black Nb-doped lithium titanate. The precursor was calcined in a muffle furnace at a high temperature of 650° C. for 5 hours to obtain white Nb-doped lithium titanate powder. figure 1 is the XRD pattern of the obtained sample. The position and relative intensity of each ...

Embodiment 2

[0028] Example 2: Add 107.5mL of absolute ethanol into the reflux equipment, according to the molar ratio Li:Nb:Ti=4.2:0.05:4.95, add 8.423g tetra-n-butyl titanate (analytical pure), 0.0675g Niobium chloride (analytical pure, anti-hydrolysis) and 0.8902g lithium chloride (analytical pure, pre-ground into fine powder), magnetically stirred until completely dissolved and in a clear state; then stirred for 40 minutes, and then the solution was first heated at 80°C Heat until reflux begins. Then adjust the temperature to 120°C, and reflux for 30 hours until the gel is formed, then stop the reflux, and take out the gel after cooling. The gel was dried at 250 °C to remove the solvent to obtain a black fluffy precursor of black Nb-doped lithium titanate. The precursor was calcined in a muffle furnace for 5 hours at 700° C. to obtain white Nb-doped lithium titanate powder. figure 2 The SEM image of the material shows that the dispersion of the material is very good and the structur...

Embodiment 3

[0029]Example 3: Add 129mL of absolute ethanol into the reflux device, according to the molar ratio Li:Nb:Ti=4.5:0.1:4.90, add 6.9634g tetraisopropyl titanate (analytical pure), 0.1351g Niobium chloride (analytical pure, anti-hydrolysis) and 0.9538g lithium chloride (analytical pure, pre-ground into fine powder), magnetically stirred until completely dissolved and in a clear state; then stirred for 30 minutes, and then the solution was first heated at 70°C Heat until reflux begins. Then adjust the temperature to 110°C, reflux for 36 hours, until the gel is formed, stop the reflux, and take out the gel after cooling. The gel was dried at 200 °C to remove the solvent to obtain a black fluffy precursor of a black Nb-doped lithium titanate. The precursor was calcined in a muffle furnace at a high temperature of 750° C. for 5 hours to obtain white Nb-doped lithium titanate powder. image 3 In order to use this material as the positive electrode and metal lithium as the negative e...

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Abstract

The invention discloses a preparation method for an Nb-doped Li4T5O12 nano material. The preparation method comprises the following steps of a, adding ethanol into backflow equipment; b, adding compounds of lithium chloride, niobium chloride and titanium in sequence into a solvent in the equipment, constructing the equipment, stirring until a solution is clarified, and then continuing to stir the solution; c, heating the solution in the step b firstly until backflow is started, then adjusting the temperature for backflow to 24-36 hours, ending the backflow after gel is formed, and taking out the gel after the gel is cooled; d, drying the gel under the temperature of 200-250 DEG C, and removing the solvent to obtain an Nb-doped lithium titanate precursor; and e, calcining the Nb-doped lithium titanate precursor obtained in the step d under the temperature of 650-750 DEG C to obtain the Nb-doped Li4T5O12 negative electrode material. The raw materials and the technology of the preparation method are simple; the particle size of the obtained product is small, and the dispersivity is high; the Nb-doped Li4T5O12 nano material is relatively high in specific charge and discharge capacity and relatively stable in cycle performance.

Description

technical field [0001] The invention relates to a lithium ion secondary electric negative electrode material Nb-doped Li 4 Ti 5 o 12 The preparation method of the electrode material, in particular, adopts the simple and effective non-hydrolytic sol-gel method which is less used at present. 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, and dendrites may form to cause a short circuit. This...

Claims

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Application Information

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IPC IPC(8): H01M4/485B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/485H01M10/0525Y02E60/10
Inventor 姚露露何丹农张春明郭松涛郭元宁子杨聂啸黄昭
Owner SHANGHAI JIAO TONG UNIV
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