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Preparation of lithium titanate material for lithium battery negative electrode by freeze-drying microemulsion method

A lithium titanate, microemulsion technology, applied in the direction of titanate, battery electrode, alkali metal titanate, etc., can solve the problems of loss of nanoparticle characteristics, high surface energy, instability, etc., and achieve excellent high-rate discharge Effects of Features

Inactive Publication Date: 2016-04-27
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the surface and interface effects of nanoparticles, the surface energy is high, the surface activity is very large, and it is extremely unstable. Performance is not ideal

Method used

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  • Preparation of lithium titanate material for lithium battery negative electrode by freeze-drying microemulsion method
  • Preparation of lithium titanate material for lithium battery negative electrode by freeze-drying microemulsion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 0.8685g of lithium acetate, add 10ml of distilled water to dissolve; then weigh 0.2375g of chitosan into 43.5ml of glacial acetic acid solution, and ultrasonically dissolve it into a uniform pale yellow liquid; add 0.87 g of chitosan to the chitosan solution g titanium dioxide powder, 0.0438g neodymium nitrate and 0.0152g scandium nitrate, ultrasonically, magnetically stir for 20min; add the dissolved lithium acetate solution to the chitosan solution, stir for 10min; add 0.4ml of epoxy chloride to the above solution Propane, continue magnetic stirring for 15h, transfer the solution to a petri dish, cover it with plastic wrap, freeze at -80°C, put the frozen sample into a freeze dryer, vacuumize, and dry for 24h to obtain a spongy white The sample was calcined at 800 °C for 10 h in a furnace to prepare the final product.

[0018] figure 1 is the XRD pattern of the obtained sample. It can be seen that the position and relative intensity of each diffraction peak in...

Embodiment 2

[0020] Weigh 0.868g of lithium acetate, add 10ml of distilled water to dissolve; then weigh 0.248g of chitosan into 50ml of glacial acetic acid solution, and ultrasonicate until it is completely dissolved into a uniform pale yellow liquid; add 0.68g to the chitosan solution Titanium dioxide powder, 0.0222g of samarium nitrate and 0.0433g of lanthanum nitrate, ultrasonically, magnetically stirred for 40min; add the dissolved lithium acetate solution to the chitosan solution, stir for 20min; add 0.5ml of epoxy chloride to the above solution Propane, continue magnetic stirring for 5h, transfer the solution to a petri dish, cover it with plastic wrap, freeze at -80°C, put the frozen sample into a freeze dryer, vacuumize, and dry for 10h to obtain a spongy white The sample was calcined at 600 °C for 15 h in a furnace to prepare the final product.

Embodiment 3

[0022] Weigh 0.9g of lithium acetate, add 10ml of distilled water to dissolve; then weigh 0.315g of chitosan into 80ml of glacial acetic acid solution, and ultrasonically dissolve it into a uniform pale yellow liquid; add 0.8g to the chitosan solution Titanium dioxide powder, 0.0438g neodymium nitrate and 0.0433g lanthanum nitrate, ultrasonically, magnetically stir for 50min; add the dissolved lithium acetate solution to the chitosan solution, stir for 40min; add 0.6ml of epichlorohydrin to the above solution , continue magnetic stirring for 15h, transfer the solution to a petri dish, cover it with plastic wrap, freeze at -80°C, put the frozen sample into a freeze dryer, vacuumize, and dry for 48h to obtain a sponge-like white sample , the samples were calcined at 900 °C for 8 h in a furnace to obtain the final product.

[0023] figure 2 In order to use the material as the positive electrode and the metal lithium sheet as the negative electrode to assemble a simulated batter...

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Abstract

The invention relates to a freeze-drying micro-emulsion method for preparing a lithium titanate material for a lithium-battery electrode. The method comprises: weighing lithium acetate, adding distilled water for dissolving; adding chitosan into a glacial acetic acid solution, adding titanium dioxide powder and a compound of a metal M and a metal N in to the chitosan solution, performing ultrasonic processing and magnetic stirring; adding the solution containing dissolved lithium acetate into the chitosan solution, and performing ultrasonic stirring; and adding chloropropylene oxide, and continuing to perform magnetic stirring; transferring the solution to a culture dish, refrigerating at -80 DEG C, putting the refrigerated sample into a freeze-drying machine, vacuumizing, drying for 10-48 h, putting the dried sample into a crucible, and sending to a tubular furnace and calcining at 600-900 DEG C for 8-15 h, so as to obtain the lithium titanate material applied to the lithium-battery electrode. Modified lithium titanate is prepared by employing the preparation method. The material has excellent high-rate discharging characteristic and applicable to power batteries.

Description

technical field [0001] The invention relates to a preparation method of battery electrode materials, in particular to a freeze-drying microemulsion method to prepare lithium titanate materials for lithium battery negative electrodes. Background technique [0002] As a new type of anode material, lithium titanate has the advantages of good cycle performance, high safety performance, and stable charge-discharge platform. It is one of the most excellent anode materials for lithium-ion batteries that has attracted much attention in recent years. However, since Li 4 Ti 5 O 12 The conductivity is relatively poor, and the capacity decays rapidly during high current charge and discharge, which limits its application. The electronic conductivity can be effectively improved by doping metal ions and carbon coating, or by preparing nanoparticles to reduce the diffusion path of lithium ions to improve the rate performance of lithium titanate materials. However, due to the surface and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485C01G23/00
CPCC01G23/005H01M4/485H01M10/0525Y02E60/10
Inventor 何丹农王丹张春明吴晓燕严鹏杨扬黄昭
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH