Preparation method of lithium titanate

A technology of lithium titanate and lithium titanate, applied in electrolysis process, electrolysis components, etc., can solve problems such as low utilization rate of lithium titanate, solve product batch stability and consistency problems, and controllable particle size Effect

Active Publication Date: 2013-09-11
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Lithium titanate with too large particle size has low utilization rate and cannot be d...

Method used

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  • Preparation method of lithium titanate
  • Preparation method of lithium titanate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Commercially available 0.1~0.2 μm TiO 2 Powder and TiO 2 After mixing 10% glucose evenly, take 2g, press it into a test piece with a diameter of 20mm and a thickness of 3mm under 8MPa, and sinter at 600°C for 3 hours in an argon atmosphere to obtain a carbon source-coated TiO 2 Audition. After the test piece was tightly wrapped with molybdenum mesh, a thin molybdenum wire was wound on a long molybdenum wire as the cathode, a graphite rod was used as the anode, and a mixture of LiCl and NaCl with a melting molar ratio of 2:1 was used as the electrolyte. In the middle, the temperature is 500°C, the voltage is 3.2V, and the electrolysis is performed for 5 hours. After the electrolysis is completed, the cathode is raised from the molten salt liquid level and cooled to room temperature in the electrolytic cell, and the product is taken out, washed with distilled water, and vacuum dried at 60°C. , burned in the air at 750°C for 2 hours, and the resulting product was about 2...

Embodiment 2

[0029] Commercially available 0.1~0.2 μm TiO 2 Powder and TiO 2 After mixing 10% acetylene black evenly, take 5g, press under 5MPa to make two test pieces with a diameter of 20mm and a thickness of 5mm, and sinter at 600°C for 2 hours in an argon atmosphere. After the test piece is tightly wrapped with stainless steel mesh, stainless steel wire is wound on the long stainless steel wire as cathode, graphite rod is used as anode, and a mixture of LiCl and KCl with a melting molar ratio of 1:1 is used as electrolyte, in an argon atmosphere , the temperature is 600°C, the voltage is 2.8V, electrolysis for 4 hours, after the electrolysis is completed, the cathode is raised from the molten salt liquid level and cooled to room temperature in the electrolytic cell, the product is taken out, washed with distilled water, and vacuum dried at 60°C, Burned at 600°C in air for 3 hours to obtain 5.1g Li 4 Ti 5 o 12 .

Embodiment 3

[0031] Commercially available 0.1~0.2 μm TiO 2 with TiO 2 After mixing 30% activated carbon evenly, take 0.5 g, press it under 10 MPa to form a test piece with a diameter of 5 mm and a thickness of 1 mm, and sinter at 600 ° C for 3 hours in an argon atmosphere. Wind the test piece with molybdenum wire to make a cathode, use a graphite rod as an anode, and use a mixture of LiCl, KCl and NaCl with a melting molar ratio of 1:1:1 as an electrolyte. In an argon atmosphere, the temperature is 400 °C and the voltage is 3.2V, electrolysis for 5 hours, after the electrolysis is completed, lift the cathode out of the molten salt liquid level and cool it to room temperature in the electrolytic cell, take out the product, wash it with distilled water, dry it in vacuum at 60°C, and burn it in the air at 850°C for 1 hours, to get 0.4g Li 4 Ti 5 o 12 .

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Abstract

The invention discloses a preparation method of lithium titanate. The preparation method is characterized by comprising the following steps of: combining TiO2 powder which is wrapped by using a carbon source or is mixed by using a carbon material or a tabletting with a metal current collector so as to be used as a cathode; by taking graphite as an anode and taking a molten alkali halide as an electrolyte, electrolyzing for 1-5 hours in an argon atmosphere at an electrolysis temperature of 400-700 DEG C under an electrolysis voltage of 2.0-3.2V, cooling down to be the normal temperature and taking out, subsequently washing in distilled water or an organic solvent, and drying in vacuum so as to obtain LiTiO2 which is wrapped by using the carbon source or is mixed by using the carbon material; washing an electrolysis product, drying the electrolysis product in vacuum, and subsequently firing for 1-3 hours at 600-900 DEG C in air so as to obtain Li4Ti5O12. By utilizing the method, product grain size controllability is realized, and the problems of product batch stability and consistence caused by in-scale production are solved. The lithium titanate prepared by using the method can be used as an energy material to be directly applied to lithium ion secondary batteries and super-capacitors.

Description

technical field [0001] The invention belongs to a method for preparing inorganic materials, in particular to a method for preparing lithium titanate. Background technique [0002] Lithium titanate (Li 4 Ti 5 o 12 ) is a structurally stable "zero-strain" embedded material. Compared with traditional carbon anode materials, it has excellent cycle stability and has attracted the attention of many lithium-ion secondary battery researchers and enterprises at home and abroad. In addition, the chemical diffusion coefficient of lithium titanate is an order of magnitude larger than that of carbon electrode materials, so it can also be used as an electrode material for supercapacitors. [0003] At present, the methods for preparing lithium titanate mainly include high-temperature solid-phase method, sol-gel method, hydrothermal synthesis method, spray drying method and composite low-temperature molten salt method, etc. The above methods have their own advantages, but all require pr...

Claims

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Application Information

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IPC IPC(8): C25B1/14
Inventor 李伟肖方明王英唐仁衡肖志平
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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