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A kind of preparation method of high specific capacity porous silicon oxide compound

An oxygen compound, high specific capacity technology, used in silicon oxide, electrical components, battery electrodes, etc., can solve the problems of wasting silicon monoxide raw materials and hydrofluoric acid, lack of nano-silicon, low initial efficiency, etc., to reduce volume expansion. effect, uniform particle distribution, high specific capacity

Active Publication Date: 2016-03-30
山东玉皇盛世化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the cycle performance of the silicon-carbon composite material obtained by the high-temperature disproportionation of silicon monoxide and hydrofluoric acid corrosion in the above patents has been greatly improved, the overall specific capacity has been reduced due to the use of a large number of composite carbon materials, especially when a large amount of hydrogen fluorine is used. The acid corrodes all the silicon dioxide and silicon monoxide, which not only wastes the silicon monoxide raw material and hydrofluoric acid, but also makes the nano-silicon lack silicon oxide as a volume expansion buffer, resulting in lower specific capacity and lower first-time efficiency

Method used

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  • A kind of preparation method of high specific capacity porous silicon oxide compound
  • A kind of preparation method of high specific capacity porous silicon oxide compound
  • A kind of preparation method of high specific capacity porous silicon oxide compound

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Put 4.4g of silicon monoxide particles into the corundum ark, put the corundum ark into the tube furnace, turn on the mechanical pump, and after evacuating to 5Pa, turn on the molecular pump and evacuate to 10 -2 Pa. Raise the temperature at 10°C per minute to 1000°C, keep the temperature for 8 hours, and cool down to room temperature with the furnace. During this process, part of the silicon monoxide disproportionates to form silicon nanoparticles.

[0027] Place the prepared product in a plastic beaker, add 40ml of hydrofluoric acid aqueous solution with a mass fraction of 10%, stir for 10 minutes, and ultrasonically corrode for 2 hours. Corroded by hydrofluoric acid, as the corrosion time prolongs, more porous silicon-oxygen compounds float above the reaction solution. After the reaction is completed, filter, wash with deionized water three times, and dry in a vacuum oven at 120° C. for 2 hours to obtain a porous silicon oxide compound.

[0028] Mix the obtained po...

Embodiment 2

[0031] Put 4.4g of silicon monoxide particles into the corundum ark, put the corundum ark into the tube furnace, and pass nitrogen gas at a flow rate of 100 sccm (standard-state cubic centimeter per minute, standard-state cubic centimeter per minute) for 2 hours. Raise the temperature at 10°C per minute to 900°C, keep the temperature for 20 hours, and cool down to room temperature with the furnace. During this process, part of the silicon monoxide disproportionates to form silicon nanoparticles.

[0032] Place the prepared product in a plastic beaker, add 15ml of hydrofluoric acid aqueous solution with a mass fraction of 20%, stir for 10 minutes, and ultrasonically corrode for 15 minutes. Corroded by hydrofluoric acid, as the corrosion time prolongs, more porous silicon-oxygen compounds float above the reaction solution. After the reaction, filter, wash with deionized water three times, and dry in a vacuum oven at 80° C. for 20 hours to obtain a porous silicon oxide compound. ...

Embodiment 3

[0035] Put 4.4g of silicon monoxide particles into a corundum ark, put the corundum ark into a tube furnace, and feed a mixture of argon and hydrogen at a flow rate of 100 sccm, with a hydrogen ratio of 10%. After 2 hours, the temperature was raised to 1200°C at 10°C per minute, kept for 12 hours, and cooled to room temperature with the furnace. During this process, part of the silicon monoxide was disproportionated to form silicon nanoparticles.

[0036] Place the prepared product in a plastic beaker, add 10ml of hydrofluoric acid aqueous solution with a mass fraction of 40%, stir for 10 minutes, and ultrasonically corrode for 1 hour. Corroded by hydrofluoric acid, as the corrosion time prolongs, more porous silicon-oxygen compounds float above the reaction solution. After the reaction, filter, wash with deionized water three times, and dry in a vacuum oven at 80° C. for 8 hours to obtain a porous silicon oxide compound.

[0037] The production method of the button battery i...

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Abstract

The invention belongs to the field of lithium ion batteries and particularly relates to a high specific capacity porous silica compound preparation method. The preparation method is characterized by comprising the following steps: silicon monoxide is used as a raw material, processed for 8-20 hours at the temperature of 900-1200 DEG C under a protective atmosphere or a vacuum condition, and cooled to the room temperature along with a furnace; a product is placed into a plastic container, the hydrofluoric acid aqueous solution is added for corrosion treatment, and reaction is performed under the ultrasound condition; the reaction liquor is filtered and washed by deionized water, and the product is dried in vacuum to obtain the high specific capacity porous silica compound. According to the invention, the preparation method is simple; the porous silica compound can be obtained only through two steps namely high-temperature treatment and hydrofluoric acid corrosion; at high temperature, part of the silicon monoxide disproportionates to generate silicon nano-particles, and the silicon nano-particles can reduce the volume expansion effect; the deep-hole porous silica compound formed by hydrofluoric acid corrosion under the ultrasound condition enables an electrolyte to enter the interior of a particle conveniently.

Description

(1) Technical field [0001] The invention belongs to the field of lithium ion batteries, in particular to a preparation method of a porous silicon-oxygen compound with high specific capacity. (2) Background technology [0002] The rapid development of electric vehicles and smart phones has put forward higher requirements for lithium-ion batteries. The negative electrode of commercial lithium-ion batteries uses graphite, and its theoretical specific capacity is only 372mAh / g. Looking for safety, high specific capacity and fast charging and discharging The negative electrode material of the scientific research worker has always been the focus of attention and the focus of research. When lithium ions are intercalated into silicon, one silicon atom can combine up to 4.4 lithium atoms to form an alloy Li with a high lithium content. 4.4 Si, with a theoretical specific capacity of 4200mAh / g, is more than 10 times higher than the commercial lithium-ion battery anode material graphi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/113H01M4/36H01M4/48
CPCY02E60/10
Inventor 赵成龙王瑛宋春华陈欣
Owner 山东玉皇盛世化工股份有限公司
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