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Porous silicon prepared by magnesiothermic reduction of ocean clay as lithium ion battery negative electrode material

A technology for lithium ion batteries and negative electrode materials, which is applied in battery electrodes, negative electrodes, secondary batteries, etc., can solve the problems of harsh reaction conditions, difficult opening of the structure, complicated aluminum removal process, etc., and achieves expansion of resources and good cycle performance. and the effect of magnification performance

Pending Publication Date: 2022-01-11
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its relatively good crystallization, the structure of terrestrial clay minerals is difficult to open, and the particles are large, which makes the removal process of aluminum more complex and the reaction conditions are harsher Wang, H.; Tang, W.; Ni, L.; Ma, W. ; Chen, G.; Zhang, N.; Liu, X.; Ma, R., Journal of Physics and Chemistry of Solids 2020,137

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Mix oceanic clay and 4mol / L sulfuric acid solution at a mass ratio of 1:3, react in a reactor at 120°C for 12h, and extract the prepared SiO by centrifugation 2 , washed with deionized water until pH = 7, and dried at 80°C.

[0024] (2) PC-SiO 2 , magnesium powder and sodium chloride were mixed in a glove box according to the mass ratio of 1:0.8:1, fully ground and transferred to a crucible, and reacted in a tube furnace at a low vacuum of 650°C for 5 hours.

[0025] (3) Treat the magnestic reduction product with 1mol / L HCl and 2% HF to remove unreacted Mg and SiO2 and the MgO generated by the reaction, and then the obtained porous Si was washed with a mixed solution of deionized water and ethanol, and dried in a vacuum oven at 60° C. for 12 hours to obtain PC-Si.

[0026] (4) Mix PC-Si and sucrose at a mass ratio of 1:0.8 in a glove box, grind them thoroughly and transfer them to a porcelain boat, react in a tube furnace at 800°C for 2 hours in an argon atmosphere...

Embodiment 2

[0030] (1) Mix oceanic clay and 4mol / L sulfuric acid solution at a mass ratio of 1:3, react in a reactor at 120°C for 12h, and extract the prepared SiO by centrifugation 2 , washed with deionized water until pH = 7, and dried at 80°C.

[0031] (2) PC-SiO 2 , magnesium powder and sodium chloride were mixed in a glove box according to the mass ratio of 1:0.8:1, fully ground and transferred to a crucible, and reacted in a tube furnace at a low vacuum of 650°C for 5 hours.

[0032] (3) Treat the magnestic reduction product with 1mol / L HCl and 2% HF to remove unreacted Mg and SiO 2 and the MgO generated by the reaction, and then the obtained porous Si was washed with a mixed solution of deionized water and ethanol, and dried in a vacuum oven at 60° C. for 12 hours to obtain PC-Si.

[0033] (4) Mix PC-Si and sucrose at a mass ratio of 1:1.6 in a glove box, grind them thoroughly and transfer them to a porcelain boat, react in a tube furnace at 800°C for 2 hours in an argon atmosphe...

Embodiment 3

[0037] (1) Mix oceanic clay and 4mol / L sulfuric acid solution at a mass ratio of 1:3, react in a reactor at 120°C for 12h, and extract the prepared SiO by centrifugation 2 , washed with deionized water until pH = 7, and dried at 80°C.

[0038] (2) PC-SiO 2 , magnesium powder and sodium chloride were mixed in a glove box according to the mass ratio of 1:0.8:1, fully ground and transferred to a crucible, and reacted in a tube furnace at a low vacuum of 650°C for 5 hours.

[0039] (3) Treat the magnestic reduction product with 1mol / L HCl and 2% HF to remove unreacted Mg and SiO 2 and the MgO generated by the reaction, and then the obtained porous Si was washed with a mixed solution of deionized water and ethanol, and dried in a vacuum oven at 60° C. for 12 hours to obtain PC-Si.

[0040] (4) Mix PC-Si and sucrose with a mass ratio of 1:2.4 in a glove box, grind them thoroughly and transfer them to a porcelain boat, and react in a tube furnace at 800°C for 2 hours in an argon at...

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Abstract

The invention relates to porous silicon prepared by magnesiothermic reduction of ocean clay as a lithium ion battery negative electrode material. Ocean clay widely existing in the ocean is utilized as a resource, and the porous carbon-silicon composite material capable of being applied to the LIB negative electrode can be obtained by a simple method. Tests show that the specific surface area of the porous silicon material can reach about 80m <2>. g <-1>. Porous silicon is carbonized, the porous carbon-silicon composite material which is applied to an LIB negative electrode and has high electrochemical performance is prepared, the initial specific capacity of the material can reach 1500 mAh.g <-1>-2300 mAh.g <-1>, and the initial coulombic efficiency is about 78%. The reversible specific capacity of 190 mAh.g <-1> to 550 mAh.g <-1> can still be provided after 120 times of circulation under the current density of 0.5 A.g<-1 >.

Description

technical field [0001] The invention relates to combining oceanic clay (PC) soil with a magnesia thermal reduction method to obtain a lithium ion battery negative electrode material with good electrochemical performance. Background technique [0002] Oceanic clay is widely distributed in the ocean. According to the research results of the relevant projects of the "Eleventh Five-Year Plan" plan of the China Oceanic Association, the amount of oceanic clay resources in the world's oceans is about 3.1×10 7 km 3 , it can be seen that its resource potential is huge. However, so far the research on it mainly focuses on its rich metal sulfide, manganese nodules, rare earth and other related researches, and there are still few studies on the comprehensive utilization of clay itself as a resource. [0003] Oceanic clay is mainly composed of clay minerals (mainly I / Smectite minerals) and contains about 5% organic matter. It has the characteristics of poor crystallization, high activ...

Claims

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Application Information

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IPC IPC(8): H01M4/38H01M4/583H01M10/0525
CPCH01M4/386H01M4/583H01M10/0525H01M2004/027Y02E60/10
Inventor 张培萍赵辰旭高钱孙雪张龙宇刘彤彤
Owner JILIN UNIV
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