Preparation method for 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: 2014-08-13
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

Method used

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  • Preparation method for zirconium nitride-coated lithium titanate composite material
  • Preparation method for zirconium nitride-coated lithium titanate composite material

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1

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

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

[0034] (3) Transfer the above-mentioned uniformly ball-milled materials into the material boat under the blowing of 5L / min of flowing argon gas and send them into the tube-type nitriding atmosphere furnace that has been evacuated. Continu...

Example Embodiment

[0038] Example 2

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

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

[0041] (3) Transfer the above-mentioned uniformly ball-milled materials into the material boat under the blowing of 5L / min of flowing argon gas and send them into the tube-type nitriding atmosphere furnace that has been evacuated. Continue to p...

Example Embodiment

[0043] Example 3

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

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

[0046] (3) Transfer the above-mentioned uniformly ball-milled materials into the material boat under the blowing of 5L / min of flowing argon gas and send them into the tube-type nitriding atmosphere furnace that has been evacuated. Continue ...

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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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IPC IPC(8): H01M4/485H01M4/62
CPCY02E60/122H01M4/366H01M4/485H01M4/624H01M10/0525Y02E60/10
Inventor 郭钰静杨茂萍杨续来谢佳
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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