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Novel method for preparing nanometer silicon from silicon dioxide

A silicon dioxide and nano-silicon technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of high energy consumption in high-temperature reactions, difficult to control reactions, self-accelerating reactions, etc., and achieve high purity and easy scale-up , small size effect

Inactive Publication Date: 2016-10-26
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The high temperature reaction is not only energy-intensive, but also makes the reaction difficult to control
Magnesium thermal reduction is a strongly exothermic reaction, and high temperature will lead to a violent self-accelerating reaction, which is easy to get out of control when preparing in large quantities

Method used

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  • Novel method for preparing nanometer silicon from silicon dioxide
  • Novel method for preparing nanometer silicon from silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Amorphous SiO 2 Prepare nano-silicon by ball milling with a molar ratio of 1:2.1 to nano-magnesium powder (average particle size: 300nm)

[0027] (1) Take 10g of raw material of commercial amorphous SiO with a size of 50nm 2 And 8.4g of magnesium powder with an average particle size of 300nm, add 25 zirconia balls with a mass of 4g, and use a planetary ball mill to mill for 10min.

[0028] (2) Add hydrochloric acid to the mixture to remove MgO and generate MgCl 2 , 500rpm centrifugal separation of nano silicon, washed with deionized water to MgCl 2 After all of them were removed, they were washed with ethanol, heated and dried under vacuum at 150° C. for 1 h to obtain nano-silicon.

[0029] (3) The nano-silicon obtained in the previous step is etched with 20%wt HF solution, the surface oxide layer is removed, and the deionized water is washed to MgCl 2 After all of them were removed, they were washed with ethanol, and dried in a vacuum oven at 70° C. for 12 hours ov...

Embodiment 2

[0032] Preparation of nano-silicon by ball milling of mesoporous molecular sieve SBA-15 and nano-magnesium powder (average particle size 300nm) at a molar ratio of 1:2.5

[0033] (1) Take 5g of SBA-15 and 5g of nano-magnesium powder (average particle size: 300nm) as raw materials, add 10 zirconia balls with a mass of 4g, and use a planetary ball mill to mill for 30min.

[0034] (2) Add hydrochloric acid to the mixture to remove MgO and generate MgCl 2 , 10000rpm centrifugal separation of nano-silicon, washed with deionized water to MgCl 2 After all of them were removed, they were washed with ethanol, heated and dried at 50° C. under normal pressure for 36 hours to obtain nano-silicon.

[0035] (3) The nano-silicon obtained in the previous step is etched with 2%wt HF solution, the surface oxide layer is removed, and the deionized water is washed to MgCl 2 After all of them were removed, they were washed with ethanol, and dried in a vacuum oven at 70° C. for 12 hours overnight...

Embodiment 3

[0038] Diatomite and nano-magnesium powder (average particle size: 300nm) molar ratio of 1:3 ball milling to prepare nano-silicon

[0039] (1) Take 8g of diatomite and 12g of nano-magnesium powder (300nm) as raw materials, add 40 zirconia balls with a mass of 4g, and use a planetary ball mill to mill for 2 hours.

[0040] (2) Add hydrochloric acid to the mixture to remove MgO and generate MgCl 2 , 30000rpm centrifugal separation of nano-silicon, washed with deionized water to MgCl 2 After all of them were removed, they were washed with ethanol, heated and dried under vacuum at 100° C. for 12 hours to obtain nano-silicon.

[0041] The high-purity nano-silicon obtained after the above two steps has good crystallinity, a particle size of about 5 μm, and a pore size of about 100 nm. The specific surface area of ​​the sample obtained by nitrogen isothermal adsorption is 200m 2 / g.

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Abstract

The invention discloses a novel method for preparing nanometer silicon from silicon dioxide. The method is based on the principle that magnesiothermic reduction of SiO2 is achieved through spontaneous reaction based on heat release, reaction is triggered through low-rotating-speed ball milling at room temperature, spontaneous proceeding of reaction is maintained through heat release, and reaction can be finished basically within 10 min. Raw materials are easy to obtain, operation is quite easy, and the method has the advantages that operation is easy and fast, yield is high, cost is low, reaction product purity is high, and amplification is easy. Prepared nanometer silicon particles are small in size and uniform in distribution, are of a porous structure, can be applied to lithium ion battery cathode materials, sensors, optical devices and other fields, and have broad industrial application prospects.

Description

technical field [0001] The invention relates to the field of preparation of silicon nanometer particles, in particular to a method for preparing silicon nanometer particles by using a ball milling method to reduce silicon dioxide with magnesium at low temperature. Background technique [0002] Because of its unique electrical, optical, thermal, and chemical properties, nano-silicon has broad application prospects in lithium-ion batteries, sensors, displays, and drug delivery. The low-cost mass preparation of nano-silicon is an important link to realize its wide application. [0003] At present, the methods for preparing nano-silicon mainly include silane decomposition method (Mangolini, L.; Kortshagen, U., Plasma-Assisted Synthesis of Silicon Nanocrystal Inks. Advanced materials 2007, 19(18), 2513-2519; Fu, G.; Xu, Y.;Yu,W.;Zhan,X.;Wang,X.Growing nanocrystalline silicon powder comprises e.g.filling mixed gas to a reactionchamber through air inlet pipe,arranging radio freque...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/023B82Y30/00
CPCC01B33/023B82Y30/00C01P2004/64C01P2006/12C01P2006/16
Inventor 刘志亮常兴华郑捷李星国
Owner PEKING UNIV
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