Synthesis method of lithium ion battery cathode nano-powder by strengthening solid-phase reaction

A lithium-ion battery and nano-powder technology, which is applied to battery electrodes, secondary batteries, circuits, etc., can solve the problems of difficult to realize industrialized production, long nano-powder process cycle, low yield and production efficiency, etc. And the effect of uniform particle size, good electrochemical performance, and complete lattice

Active Publication Date: 2015-10-14
HUNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are also studies using nanoscale oxide powder (Co3O4) synthesized by the sol-gel method as a precursor, and solidifying it with lithium salt and LiOH at high temperature. Nanoscale LiCoO2 powder was synthesized by phase reaction, which has excellent electrochemical performance, but the liquid phase synthesis of nanometer Co3O4 powder The same process has the disadvantages of complicated process, low yield and high cost
[0005] Due to the long process cycle, low yield and low production efficiency of nano powder synthesis by liquid phase method, it is difficult to realize industrial production, and the production cost of the product is relatively high

Method used

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  • Synthesis method of lithium ion battery cathode nano-powder by strengthening solid-phase reaction
  • Synthesis method of lithium ion battery cathode nano-powder by strengthening solid-phase reaction
  • Synthesis method of lithium ion battery cathode nano-powder by strengthening solid-phase reaction

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Experimental program
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Effect test

Embodiment 1

[0031] Refer to attached picture 1. Preparation of LiCoO 2 Nanopowders, first commercially available (average particle size > 5 μm) CoCO 3 Powder and Li 2 CO 3The powders are measured separately according to the molar ratio of Li:Co ratio of 1:1, and the ingredients are mixed according to the ball-to-material ratio of 15:1, and put into the ball mill jar. After the powder mass percentage is 0.5% ball milling aid (the mixture of alcohol and low molecular weight polymer), the mixture is carried out high-energy ball milling treatment 10h in the planetary ball mill, and the rotating speed of ball mill is 300~400r / min, and the particle size is in the nanoscale After the ball milling product is dried in a drying oven, it is placed in a calciner for solid-phase thermal decomposition-diffusion reaction to obtain LiCoO 2 For nano powder, the reaction temperature is 600°C, and the reaction time is 3h; the low-temperature treated powder is calcined at 900°C for 1h, cooled with the fu...

Embodiment 2

[0034] Refer to attached picture 6. Preparation of LiNi 0.5 mn 1.5 o 4 Nano-powder, first commercially available (average particle size > 5μm) MnCO 3 、NiCO 3 Powder and Li 2 CO 3 The powders are respectively measured according to the molar ratio of Li:Ni:Mn ratio of 2:1:3, and the proportioning is carried out according to the ball-to-material ratio of 15:1, put into a ball mill jar, and the mixture is subjected to high-energy ball milling for 10 hours. The ball mill jar is agate. The ball is made of zirconia, and a ball milling aid with a powder mass percentage of 1% is added to the ball mill tank; after the ball mill product is dried in a drying oven, it is put into a calciner for solid-phase thermal decomposition-diffusion reaction synthesis, and the reaction The temperature is 700°C and the reaction time is 5h. The low-temperature treated powder was calcined at 900°C for 1 hour, cooled with the furnace, and pulverized to obtain the desired product.

Embodiment 3

[0036] Refer to attached picture 7a and 7b, Preparation of LiNi 1 / 3 mn 1 / 3 co 1 / 3 o 2 Nano-powder, first commercially available (average particle size > 5μm) MnCO 3 、NiCO 3 、CoCO 3 Powder and Li 2 CO 3 The powders are respectively measured according to the molar ratio of Li:Ni:Mn ratio of 3.1:1:1, and the ingredients are prepared according to the ball-to-material ratio of 15:1. Add a ball milling aid with a powder mass percentage of 1% in the ball milling tank, and perform high-energy ball milling on the mixture for 10 hours. After the ball milling product is dried in a drying oven, it is put into a calciner for solid-phase thermal decomposition-diffusion reaction synthesis, and the reaction The temperature is 700°C, and the reaction time is 7 hours. The low-temperature-treated powder is calcined at 950°C for 3 hours, cooled with the furnace, and pulverized to obtain the desired product.

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Abstract

A synthesis method of lithium ion battery cathode nano-powder by strengthening solid-phase reaction comprises the steps of: (1) nanocrystallization treatment on a raw material powder; (2) synthesis of a target product compound nano-powder; and (3) lattice complete treatment of synthesis product. The invention uses conventional carbonate meal as a raw material, employs strengthening solid phase thermal decomposition and diffusion reaction to directly and rapidly synthesize the nano-powder. The production process has the advantages of simpleness, short cycle, high efficiency, low energy consumption and no pollution, and is applicable to continuous production; the solid phase reaction process is complete; the powder has fine size, and uniform composition and particle size; and the synthetic product does not require subsequent pulverization treatment; and the powder has complete lattice and shows good electrochemical performance.

Description

technical field [0001] The invention belongs to the technical field of battery material preparation, and in particular relates to a method for directly and rapidly synthesizing nanometer and ultrafine powders for positive poles of lithium-ion batteries by using commercially available carbonate coarse powder through enhanced solid-phase thermal decomposition and diffusion reaction processes. Background technique [0002] At present, the commercially available lithium-ion battery cathode material LiCoO 2 、LiNi 0.5 mn 1.5 o 4 、LiNi 1 / 3 mn 1 / 3 co 1 / 3 o 2 They are all synthesized by high-temperature solid-state reaction method, and the raw materials used are Co, Ni, Mn oxides and Li 2 CO 3 , LiOH powder, the powder particle size is 5-10 μm, there are problems such as uneven mixing of raw material powder, resulting in poor uniformity of composition and particle size of the synthetic product, powder particle size of micron level and uneven distribution, unsatisfactory charg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1391H01M10/0525
CPCH01M4/1391H01M10/0525Y02E60/10
Inventor 严红革陈吉华阳轩野贺茂徐枫张正富黄彪
Owner HUNAN UNIV
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