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Preparation method of high-performance co-doped lithium titanate electrode material

An electrode material, heterolithium titanate technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of single ion doping, nanotechnology use restrictions, etc., and achieve the effect of high current charge and discharge performance

Inactive Publication Date: 2016-03-30
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, nanotechnology is mainly aimed at nanoparticles, while the industrial production of lithium titanate generally uses a high-temperature solid-phase method, and most of the products are submicron / micron particles, which limits the use of nanotechnology.
For metal ion doping and surface coating technology, the current research basically focuses on single ion doping or surface coating, and there is little research on simultaneously improving the internal conductivity and external conductivity of submicron / micron lithium titanate particles. There are reports

Method used

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  • Preparation method of high-performance co-doped lithium titanate electrode material
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  • Preparation method of high-performance co-doped lithium titanate electrode material

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Embodiment 1

[0030] A method for preparing a high-performance co-doped lithium titanate electrode material, specifically comprising the following steps:

[0031] 19.95g of titanium dioxide, 13.20g of lithium acetate, and 0.033g of niobium pentoxide were weighed in acetone, and then mixed in a ball mill at 300r / min to obtain a precursor slurry. The obtained precursor slurry was placed in a blast drying oven at 60° C. to dry to obtain a doped precursor. The obtained doped precursor was placed in a crucible and then placed in a muffle furnace for treatment at 700°C for 8 hours, and then cooled to room temperature to obtain niobium-doped lithium titanate. Then the obtained niobium-doped lithium titanate is placed in a tube furnace, under a nitrogen atmosphere, the temperature is raised to 600°C at 2°C / min and converted into methane, kept for 10min, and then cooled to room temperature under a nitrogen atmosphere. A carbon-coated niobium-doped lithium titanate electrode material is obtained. f...

Embodiment 2

[0033] A method for preparing a high-performance co-doped lithium titanate electrode material, specifically comprising the following steps:

[0034] Weigh 3.97g of titanium dioxide, 1.55g of lithium carbonate, and 0.055g of tantalum pentoxide in absolute ethanol, and mix in a ball mill at 400r / min to obtain a precursor slurry. The resulting precursor slurry was placed in a blast oven at 80°C to dry to obtain a doped precursor. The obtained doped precursor was placed in a crucible and placed in a muffle furnace for treatment at 850°C for 9 hours, and then cooled to room temperature to obtain internal tantalum-doped lithium titanate. The obtained tantalum-doped lithium titanate is then placed in a tube furnace, and under an argon atmosphere, the temperature is raised to 700°C at 5°C / min and converted into ammonia, kept for 30min, and then cooled to 700°C under an argon atmosphere At room temperature, a titanium nitride-coated tantalum-doped lithium titanate electrode material i...

Embodiment 3

[0036] A method for preparing a high-performance co-doped lithium titanate electrode material, specifically comprising the following steps:

[0037] 19.95 g of titanium dioxide, 9.02 g of lithium hydroxide monohydrate, and 0.036 g of molybdenum oxide were weighed in methanol at a molar ratio of 4.3:5, and mixed in a ball mill at 500 r / min to obtain a precursor slurry. The obtained precursor slurry was placed in a blast drying oven at 100° C. to dry to obtain a doped precursor. The obtained doped precursor was then placed in a crucible and placed in a muffle furnace for treatment at 900°C for 10 hours, and then cooled to room temperature to obtain molybdenum-doped lithium titanate. Then place the prepared molybdenum-doped lithium titanate in a tube furnace, heat up at 10°C / min to 900°C in a helium atmosphere, convert it into ethane, keep it warm for 60min, and then cool it down to room temperature in a helium atmosphere , to obtain a carbon-coated molybdenum-doped lithium tita...

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Abstract

The invention discloses a preparation method of a high-performance co-doped lithium titanate electrode material. The method comprises: adding titanium dioxide, a lithium source and a metal ion source into a solvent, carrying out high-energy ball milling and uniform mixing to obtain precursor grout, and then drying the precursor grout in an air dry oven at a temperature of 60 to 120 DEG C to obtain precursor powder; then calcining the precursor powder for 10 hours at a high temperature in a muffle furnace with a temperature of 700 to 1,000 DEG C to obtain metal ion doped lithium titanate; and finally, carrying out mixing and heat treatment on the doped lithium titanate and a nitrogen source or a carbon source to obtain the doped lithium titanate electrode material of which the outside is coated with a conductive layer and the inside is doped with metal ion bodies. The lithium titanate material synthesized by the method is prepared into a button cell by using metal lithium as a cathode, and capacitance of the button cell can reach 132.7mAh / g under a current density of 10C. The preparation method can be applicable to commercialized mass production, and the prepared lithium titanate product is stable in performance, and can be applied to the field of a high-power battery.

Description

Technical field [0001] The invention involves the field of secondary battery electrode materials technology, and it is specific to a preparation method of a high -performance co -doped lithium titanate electrode material. Background technique [0002] As a very promising lithium ion battery negative material, spinel lithium titanium titanium (li 4 TI 5 O 12 ) It is widely studied by people with a "zero -change" and excellent circular performance and a peaceful circulation performance.use.However, the lower electrical and ionic conductivity of lithium titanium titanium titanate makes its multiplier performance under large current density, and it is necessary to conduct modified research on it, thereby improving the electrochemical properties at its large current density.Structural nanoclacosis, metal ion doping, and surface covering are an effective way to improve lithium titanate conductivity.Among them, nanochemical technology is mainly aimed at nano particles, and the industria...

Claims

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Application Information

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IPC IPC(8): H01M4/485H01M4/62H01M4/131H01M4/1391H01M10/0525
CPCH01M4/131H01M4/1391H01M4/485H01M4/624H01M4/625H01M10/0525Y02E60/10
Inventor 王海辉郭敏王素清
Owner SOUTH CHINA UNIV OF TECH
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