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Method for preparing lithium titanate by spray drying-solid phase method

A technology for preparing lithium titanate and solid-phase method, which is applied in the direction of titanate, alkali metal titanate, chemical instruments and methods, etc., can solve the problems of violent reaction process, volume expansion, safety accidents, etc., and achieve chemical uniformity Good, slow down the electrode polarization, improve the effect of discharge capacity

Pending Publication Date: 2019-08-06
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the anode materials of lithium-ion batteries on the market are basically graphite, but graphite has several problems: 1. The ion diffusion coefficient of graphite is low, which leads to unsatisfactory rate performance of graphite anode lithium-ion products
2. The graphite negative electrode will undergo a certain volume expansion during the process of deintercalating lithium. At the same time, the SEI film formed on the surface of the graphite negative electrode is a dynamic process of continuous consumption and repair during the charging and discharging process. Therefore, the battery using the graphite negative electrode The problem of cycle capacity fading remains to be overcome
3. The potential platform of graphite deintercalation lithium is about 0.1 ~ 0.15V, it is easy to form lithium precipitation at low temperature or high magnification, leading to safety accidents
The process of synthesizing nano-scale powder by sol-gel method is relatively complicated, while the solution combustion method uses glycine complexation. Although the performance of the synthesized nano-powder is better, the price of glycine complexing agent is relatively high, and the cost is greatly increased. In addition, the The reaction process is violent and difficult to control
The solid-state reaction method is one of the traditional methods for preparing spinel lithium titanate, which uses TiO 2 with LiOH·H 2 O or Li 3 CO 3 Lithium titanate is obtained by sintering at high temperature under nitrogen atmosphere after mixing, which has the advantages of simple process and low cost, but at the same time, there are problems that the powder raw materials need to be ground and mixed for a long time, the uniformity is limited, and the diffusion process is difficult to proceed smoothly. , at the same time, the preparation process of this method requires high-temperature sintering in a nitrogen atmosphere, and the sintering time is relatively long, which makes it difficult to realize in the actual production process

Method used

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  • Method for preparing lithium titanate by spray drying-solid phase method
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  • Method for preparing lithium titanate by spray drying-solid phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of lithium titanate material: Weigh tetrabutyl titanate according to the Li:Ti molar ratio of 0.816:1, add ammonia water, the pH of the ammonia water is 10, hydrolyze into titanyl hydroxide in an ice bath, add concentrated nitric acid A clear solution of titanyl nitrate was prepared by sonication. Weigh lithium nitrate according to the ratio of Li:Ti molar ratio of 0.816:1, add glycerol equivalent to 1.0wt% tetrabutyl titanate quality to form the first solution, add titanyl nitrate to the first solution , and stir evenly; then carry out spray drying, the spray drying system is set, the inlet temperature is set to 190°C, the feed rate is 650mL / h, and the atomizer pressure is 2Mpa to obtain the lithium titanate precursor powder. Spherical lithium titanate sample 1 was obtained by roasting at 800°C for 6 hours in an air atmosphere and cooling to room temperature.

[0036] pass figure 2 It can be seen from the XRD pattern that the present invention successful...

Embodiment 2

[0039] The preparation process of the lithium titanate material is the same as in Example 1, but the Li:Ti molar ratio is changed to 0.856:1, and the spherical lithium titanate sample 2 is obtained. pass figure 1 It can be seen from the scanning electron microscope photos that the lithium titanate material prepared by the present invention is micro-nano spherical lithium titanate particles, and the lithium titanate particles have a high degree of diffusion, good chemical uniformity, and uniform distribution at the atomic level. The lithium titanate negative electrode material for lithium ion battery prepared in this example was used as the working electrode, and the charge and discharge test was the same as in Example 1. The results showed that the discharge capacity could reach 159.3mAh / g at a current density of 0.1C, and the coulombic efficiency was 96.2%. , The capacity retention rate after 20 laps is 96.6%.

Embodiment 3

[0041] The preparation process of the lithium titanate material is the same as in Example 1, but the Li:Ti molar ratio is changed to 0.9:1, and the spherical lithium titanate sample 3 is obtained. The lithium-ion battery lithium titanate negative electrode material prepared in this example is used as the working electrode, and the charge and discharge test is the same as in Example 1. The results show that the discharge capacity can reach 166.9mAh / g at a current density of 0.1C, and the Coulombic efficiency is 93.8%. , The capacity retention rate after 20 laps is 95.8%.

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Abstract

The invention discloses a method for preparing lithium titanate by a spray drying-solid phase method, the method comprises the following steps: (1) weighing a titanium source, adding ammonia water, preparing metatitanic acid under a first reaction condition, adding concentrated nitric acid, and ultrasonically preparing a titanium oxynitrate clear solution; (2) weighing a lithium source, adding a dispersant and deionized water, and stirring to obtain a first solution; (3) mixing the titanium oxynitrate clear solution with the first solution, and then drying with a spray drier to obtain precursor powder; and (4) roasting and cooling the precursor powder to prepare the lithium titanate. According to the method, the lithium titanate is prepared by a method spray drying and solid phase combinedmethod, and the prepared lithium titanate is uniform and non-heterogenous micro-nano spherical lithium titanate particles, and the lithium titanate particles have high diffusion degree, good chemicaluniformity, atomic-level uniform distribution and high tap density. The lithium titanate can slow down the polarization of a electrode and increase the contact area between an electrode material andan electrolyte.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for preparing lithium titanate by a spray drying-solid phase method. [0002] technical background [0003] Lithium-ion batteries have the advantages of environmental protection, light weight, large capacity, and no memory effect, and have been widely used in various electronic products. At present, the anode materials of lithium-ion batteries on the market are mainly graphite. However, there are several problems with graphite: 1. The ion diffusion coefficient of graphite is low, which leads to unsatisfactory rate performance of graphite anode lithium-ion products. 2. The graphite negative electrode will undergo a certain volume expansion during the process of deintercalating lithium. At the same time, the SEI film formed on the surface of the graphite negative electrode is a dynamic process of continuous consumption and repair during the charging and discharging proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00H01M4/485H01M10/0525
CPCC01G23/005C01P2002/72C01P2004/03C01P2006/40H01M4/485H01M10/0525Y02E60/10
Inventor 韦克毅张玲张天栋杨建云汤丹瑜刘晓敏朱龙凌军
Owner CHINA TOBACCO YUNNAN IND
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