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An in situ growth surface coordination polymerization for the preparation of hollow CO 3 o 4 nanosphere method

A technology of coordination polymerization and in-situ growth, applied in nanotechnology, electrochemical generators, structural parts, etc., can solve the problems of poor rate performance, low electron diffusion rate, accelerated capacity decay, etc., and achieve excellent electrochemical performance. Effect

Active Publication Date: 2021-12-07
JIANGXI UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such anode materials also have some disadvantages: 1) low electron diffusion rate and poor rate performance; 2) Li + The embedding / extraction leads to large volume changes, causing material structure collapse and pulverization, and accelerating capacity decay

Method used

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  • An in situ growth surface coordination polymerization for the preparation of hollow CO  <sub>3</sub> o  <sub>4</sub> nanosphere method
  • An in situ growth surface coordination polymerization for the preparation of hollow CO  <sub>3</sub> o  <sub>4</sub> nanosphere method
  • An in situ growth surface coordination polymerization for the preparation of hollow CO  <sub>3</sub> o  <sub>4</sub> nanosphere method

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Experimental program
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Effect test

Embodiment 1

[0027] Preparation of Hollow Co by Surface Coordination Polymerization by In Situ Growth 3 o 4 The method of nanosphere, concrete steps are as follows:

[0028] (1) Weigh 10mmol of cobalt nitrate hexahydrate, 20mmol of urea and 2mmol of sodium citrate and dissolve them in 50ml of pure water, then transfer the mixed solution to a 100ml high-pressure reactor, and react at a constant temperature of 95°C for 4h, and the reaction ends Afterwards, the product was collected, washed, and dried to obtain precursor A with a particle size of about 5 μm.

[0029] (2) Weigh 0.1g of precursor A and 5g of 2-methylimidazole and disperse them in 20ml of ethylene glycol, then add 40ml of pure water, stir and react at room temperature for 1 hour, collect the product after the reaction, wash, and dry to obtain the precursor Body B, the particle size is about 400nm.

[0030] (3) Precursor B was calcined in an air atmosphere, the heating rate was 1°C / min, the calcination temperature was 250°C, a...

Embodiment 2

[0037] Preparation of Hollow Co by Surface Coordination Polymerization by In Situ Growth 3 o 4 The method of nanosphere, concrete steps are as follows:

[0038] (1) Weigh 10mmol of cobalt chloride hexahydrate, 10mmol of urea and 1mmol of sodium citrate and dissolve them in 50ml of ultrapure water, then transfer the mixed solution to a 100ml autoclave, and react at a constant temperature of 100°C for 8h, After the reaction, the product was collected, washed, and dried to obtain precursor A with a particle size of about 30 μm.

[0039] (2) Weigh 0.1g of precursor A and 2g of 2-methylimidazole and disperse them in 20ml of glycerol, then add 20ml of pure water, stir and react at room temperature for 3h, collect the product after the reaction, wash and dry to obtain the precursor Body B, the particle size is about 270nm;

[0040] (3) will Co 3 o 4 The precursor is calcined, the heating rate is 2°C / min, the calcination temperature is 300°C, the calcination time is 2h, and the c...

Embodiment 3

[0043] Preparation of Hollow Co by Surface Coordination Polymerization by In Situ Growth 3 o 4 The method of nanosphere, concrete steps are as follows:

[0044] (1) Weigh 10mmol of cobalt sulfate heptahydrate, 40mmol of urea and 4mmol of sodium citrate and dissolve them in 50ml of ultra-pure water, then transfer the mixed solution to a 100ml autoclave, and react at a constant temperature of 110°C for 2h. After the end, the product was collected, washed, and dried to obtain precursor A with a particle size of about 20 μm.

[0045] (2) Weigh 0.1g of precursor A and 10g of 2-methylimidazole and disperse them in 20ml of ethyl acetate, then add 80ml of pure water, stir and react at room temperature for 0.5h, collect the product after the reaction, wash, and dry to obtain Precursor B, the particle size is about 80nm;

[0046] (3) will Co 3 o 4 The precursor is calcined, the heating rate is 5°C / min, the calcination temperature is 350°C, the calcination time is 1h, and the calcin...

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Abstract

The invention discloses an in-situ growth surface coordination polymerization reaction to prepare hollow Co 3 o 4 The method of nanospheres, comprising: dissolving inorganic cobalt salt, sodium citrate, and urea in pure water, heating and reacting, collecting the product after the reaction, washing, and drying to obtain precursor A; Imidazole is dispersed in the tackifier, and then pure water is added to stir the reaction. After the reaction, the product is collected, washed, and dried to obtain the precursor B; the precursor B is calcined in the air to obtain the hollow Co 3 o 4 nanospheres. In the present invention, the reaction speed and viscosity of the reaction system are controlled by adding a viscosifying agent, so that the polymerization reaction occurs on the surface of the microsphere precursor, and the transformation from the microsphere to the nanosphere is realized. The particle size can be adjusted by changing the ratio of the tackifier to water, and the thickness of the hollow spherical shell can be adjusted in the subsequent heat treatment step. The nano hollow material obtained by the invention shows excellent electrochemical performance when used as the negative electrode material of the lithium ion battery.

Description

technical field [0001] The invention belongs to the field of material synthesis and energy technology, in particular to an in-situ growth surface coordination polymerization reaction to prepare hollow Co 3 o 4 Nanosphere method. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, high working voltage, long cycle life, and no memory. They have been widely used in digital, energy storage, electric vehicles and other fields, and have become the most promising high-energy battery system. [0003] At present, commercial lithium-ion batteries mostly use graphite anode materials, but graphite materials have the disadvantage of low specific capacity. Its theoretical capacity is only 372mAh / g, which cannot meet the growing needs of people. Therefore, it is urgent to develop anode materials with higher specific capacity. to replace graphite. In all materials, Co 3 o 4 Due to its high theoretical specific capacity (890mAh / g), it has attr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/52H01M10/0525B82Y40/00
CPCB82Y40/00H01M4/523H01M10/0525Y02E60/10
Inventor 刘嘉铭卢彦华钟彩妮李金辉王瑞祥徐志峰
Owner JIANGXI UNIV OF SCI & TECH