Preparation method of zirconium nitride coated lithium titanate composite material

A technology of zirconium nitride coating lithium titanate and composite materials, which is applied to electrochemical generators, electrical components, battery electrodes, etc., and can solve problems affecting battery life, electrolyte failure decomposition, and high resistivity of lithium titanate , to achieve good chemical stability, good coating effect, simple and controllable preparation process

Active Publication Date: 2016-03-30
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However Li 4 Ti 5 o l2 There are two deficiencies when it is directly applied to lithium batteries. One is the high resistivity of lithium titanate, and the other is that in the development of batteries, it is found that the lithium titanate power battery generally has the problem of flatulence, which seriously affects the performance of the battery.
Studies have shown that the crystallization water in the lithium titanate negative electrode material and the trace water in the electrolyte are difficult to remove. During the formation and cycle of the finished battery, these trace water will cause the electrolyte to decompose and generate gas, resulting in gas Swelling phenomenon, affecting battery life
At the same time, the study also found that the high-valent titanium in lithium titanate has strong catalytic activity, so it is easy to catalyze the decomposition of carbonate electrolyte to produce gas, which makes the battery cell flatulence

Method used

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  • Preparation method of zirconium nitride coated lithium titanate composite material
  • Preparation method of zirconium nitride coated lithium titanate composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Weigh lithium carbonate and titanium dioxide according to the molar ratio of lithium and titanium elements being 0.82, carry out ball milling dispersion treatment with alcohol for 6 hours, and then dry the obtained slurry in a vacuum oven at 100°C for 10 hours to obtain titanic acid Lithium precursor powder.

[0033] (2) According to the molar ratio of zirconium and titanium elements being 0.03, take aluminum powder and lithium titanate precursor powder in a high-energy ball mill tank, and then add ammonium chloride additive accounting for 5% of the total material mass percentage, and the ball-to-material ratio is 20:1, the filling ratio is 1 / 4, the ball milling tank is sealed after filling with argon, and the high-energy ball milling is performed for 4 hours.

[0034] (3) Transfer the above ball-milled uniform material to the material boat under the blowing of flowing argon gas 5L / min and send it into the tube-type nitriding atmosphere furnace that has been emptied...

Embodiment 2

[0039] (1) Take lithium carbonate and titanium dioxide according to the molar ratio of lithium and titanium elements being 0.82, carry out ball milling dispersion treatment with deionized water for 6 hours, then dry the slurry obtained in a vacuum oven at 100° C. for 10 hours to obtain Lithium titanate precursor powder.

[0040] (2) According to the molar ratio of zirconium and titanium elements being 0.03, take zirconium powder and lithium titanate precursor powder in a high-energy ball mill tank, and then add ammonium chloride additive accounting for 3% of the total material mass percentage, and the ball-to-material ratio is 20:1, the filling ratio is 1 / 4, the ball milling tank is sealed after filling with argon, and the high-energy ball milling is performed for 4 hours.

[0041] (3) Transfer the above ball-milled uniform material to the material boat under the blowing of flowing argon gas 5L / min and send it into the tube-type nitriding atmosphere furnace that has been empti...

Embodiment 3

[0044] (1) Weigh lithium nitrate and titanium dioxide according to the molar ratio of lithium and titanium elements being 0.84, carry out ball milling dispersion treatment with alcohol for 6 hours, and then dry the obtained slurry in a vacuum oven at 100°C for 10 hours to obtain titanic acid Lithium precursor powder.

[0045] (2) According to the molar ratio of zirconium and titanium elements being 0.05, take zirconium powder and lithium titanate precursor powder in a high-energy ball mill tank, and then add ammonium chloride additive accounting for 5% of the total material mass percentage, and the ball-to-material ratio is 20:1, the filling ratio is 1 / 4, the ball milling tank is sealed after filling with argon, and the high-energy ball milling is performed for 4 hours.

[0046] (3) Transfer the above ball-milled uniform material to the material boat under the blowing of flowing argon gas 5L / min and send it into the tube-type nitriding atmosphere furnace that has been emptied ...

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Abstract

The invention discloses a preparation method for a zirconium nitride-coated lithium titanate composite material, relating to the field of a negative electrode material of a lithium ion battery. The preparation method comprises the steps of preparing lithium titanate precursor powder, performing high-energy ball grinding on zirconium powder, a lithium titanate precursor and an additive under inert atmosphere, and finally performing high-temperature sintering under nitrogen mixing atmosphere to realize synthesis of lithium titanate and nitridation reaction of surface zirconium. According to the zirconium nitride-coated lithium titanate composite material prepared by the preparation method disclosed by the invention, the zirconium nitride coating layer is high in uniformity, good in coating effect and high in conductivity; the problem of low conductivity of lithium titanate is solved; meanwhile, the problem of swelling of a battery of the lithium titanate system is effectively solved; the circulation stability of a lithium titanate negative electrode material is improved, and the cycle life of the battery is greatly prolonged; furthermore, the preparation process of the preparation method is simple and controllable; the coating degree of the zirconium nitride can be controlled by controlling technical parameters for preparing the zirconium nitride-coated lithium titanate composite material.

Description

technical field [0001] The invention relates to the field of negative electrode materials for lithium ion batteries, in particular to a preparation method of a zirconium nitride-coated lithium titanate composite material. Background technique [0002] In recent years, due to rising oil prices and serious global warming, low-carbon life has attracted more and more attention. Hybrid electric vehicles and pure electric vehicles have begun to enter people's lives; lithium-ion batteries are such power tools best candidate. However, for this type of power vehicle, the key issue of lithium-ion batteries is safety performance. Since the existing lithium-ion batteries usually use carbon materials as negative electrodes, their lithium intercalation potential is very close to that of metal lithium. It is easy to grow dendrite lithium on the surface of the negative electrode, which brings safety hazards. Moreover, the carbon negative electrode is easy to form an SEI film during the fi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485H01M4/62
CPCH01M4/366H01M4/485H01M4/624H01M10/0525Y02E60/10
Inventor 郭钰静杨茂萍杨续来谢佳
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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