Preparation method of spinelle lithium titanate for lithium secondary battery negative electrode material

A lithium secondary battery and lithium halite titanate technology, which is applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of short reaction time, low heat treatment temperature, and low bulk density, and achieve the expansion of production scale and preparation Simple process and wide-ranging effects

Inactive Publication Date: 2007-02-28
BEIJING INSTITUTE OF TECHNOLOGYGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, most commercial lithium-ion battery anode materials use carbon materials, which have some disadvantages: the precipitation of lithium dendrites during the charging and discharging process; the first charge and discharge efficiency is low (about 85%); it reacts with the electrolyte; There is a noticeable voltage hysteresis
The traditional solid phase reaction method is simple in process, but the raw materials need to be grinded and mixed for a long time, and the degree of uniformity of mixing directly affects the performance of the product. The reaction diffusion speed is slow, the product particle distribution is uneven, and the bulk density is low. Higher heat treatment temperature and Long heat treatment time, high energy consumption
Compared with the solid-state reaction, the product prepared by the sol-gel method has high chemical purity, good uniformity, low heat treatment temperature, and short reaction time, but the cost increases due to the addition of organic compounds during the synthesis process.

Method used

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  • Preparation method of spinelle lithium titanate for lithium secondary battery negative electrode material
  • Preparation method of spinelle lithium titanate for lithium secondary battery negative electrode material
  • Preparation method of spinelle lithium titanate for lithium secondary battery negative electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] TiO 2 , LiOH·H 2 O and LiCl were mixed evenly at a molar ratio of 1.25:1:1.25, then transferred to a crucible, placed in a muffle furnace, and calcined at 1200 °C for 16 hours in an air atmosphere, and then naturally cooled to room temperature with the furnace, and the sample was taken out. Repeated washing with distilled water to remove excess Cl - and Li + , until the AgNO 3 The solution does not precipitate out. The washed samples were baked in a vacuum oven at 100° C. for 24 hours to obtain lithium titanate powder. The morphology of the product is octahedral structure observed by field emission scanning electron microscope (SEM), the particle size is 90-100 μm, and it is detected as pure phase spinel Li by X-ray powder diffraction (XRD). 4 Ti 5 o 12 .

[0020] The synthesized Li 4 Ti 5 o 12 , acetylene black and binder are mixed evenly in a mass ratio of 8:1:1, and coated on aluminum foil. After drying in a vacuum oven at 55°C for 24 hours, the pressed s...

Embodiment 2

[0022] TiO 2 , LiOH·H 2 O and LiCl were mixed uniformly at a molar ratio of 1.25:1:25, then transferred to a crucible, placed in a muffle furnace, and calcined at 500 °C for 6 hours in an air atmosphere, then cooled naturally to room temperature with the furnace, and the sample was taken out. Repeated washing with distilled water to remove excess Cl - and Li + , until the AgNO 3 The solution does not precipitate out. The washed sample was baked in a vacuum oven at 80° C. for 24 hours to obtain lithium titanate powder. The morphology of the product is octahedral structure observed by field emission scanning electron microscope, the particle size is 50-60nm, and it is detected as pure phase spinel Li by X-ray powder diffraction. 4 Ti 5 o 12 .

[0023] The preparation of the pole piece, the assembly of the experimental battery and the electrochemical performance test are the same as in Example 1. The current density is 0.07mA / cm 2 , the first charge-discharge efficiency...

Embodiment 3

[0025] TiO 2 , LiOH·H 2 O and binary low-temperature molten salt 0.59LiCl-0.41KCl were mixed evenly in a molar ratio of 1.25:1:10, then transferred to a crucible, placed in a muffle furnace, and calcined at 800°C for 8 hours in an air atmosphere, and then The furnace was naturally cooled to room temperature, and the samples were taken out. Repeated washing with distilled water to remove excess Cl - and Li + , until the AgNO 3 The solution does not precipitate out. The washed samples were baked in a vacuum oven at 100° C. for 24 hours to obtain lithium titanate powder. The morphology of the product was observed by a field emission scanning electron microscope as an octahedral structure with a particle size of 1-3 μm, as shown in Figure 1 . Detected as pure phase spinel Li by X-ray powder diffraction 4 Ti 5 o 12 , see Figure 2.

[0026] The preparation of the pole piece, the assembly of the experimental battery and the electrochemical performance test are the same as i...

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Abstract

The invention discloses a preparing method of spinel lithium titanate as Li-secondary battery cathode material, which adopts titanium dioxide and inorganic Li salt as raw material to low-temperature fusing salt as synthetic dielectrics to generate the product through solid-phase reaction.

Description

technical field [0001] The invention mainly relates to a preparation method of spinel lithium titanate, which is a negative electrode material for a lithium secondary battery, and belongs to the field of chemical power sources, in particular to the key material and technical field of lithium secondary batteries. Background technique [0002] At present, most commercial lithium-ion battery anode materials use carbon materials, which have some disadvantages: the precipitation of lithium dendrites during the charging and discharging process; the first charge and discharge efficiency is low (about 85%); it reacts with the electrolyte; There is a noticeable voltage hysteresis. Compared with carbon negative electrodes, alloy-based negative electrode materials generally have higher specific capacity, but poorer cycle performance. Spinel lithium titanate (Li 4 Ti 5 o 12 ) has obvious advantages: it is a zero-strain material, and the volume change of the material is small during ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00C01G23/00H01M4/58
CPCY02E60/12Y02E60/10
Inventor 白莹吴锋吴川包丽颖王国庆张旻昱王峰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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