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Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method

A nanotube and electrochemical technology, applied in chemical instruments and methods, inorganic chemistry, nanotechnology, etc., to achieve the effect of controllable shape, simple equipment, and uniform particle size

Active Publication Date: 2010-06-16
CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrochemical method of directly preparing nano-silicon and nano-silicon wires (tubes) from silicon compound SiX or a mixture containing silicon compound SiX has not been reported internationally.

Method used

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  • Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method
  • Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method
  • Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] 75 wt% of SiO with a purity of 99.95% and an average particle size of 0.2 μm 2 The powder is mixed with 25wt% binder (as SiO 2 The total weight of powder and binder is 100%), pressed by mechanical pressure at 5MPa to about 10mm in diameter and 1.1mm in thickness, and heated in air at 1100°C for about 5 hours to sinter the formed SiO 2 The small piece is combined with a conductive cathode current collector as the cathode, and the graphite rod is used as the anode to melt the CaCl 2 As an electrolyte, in an argon environment, the temperature is 800°C, the voltage is controlled by a voltage regulator to perform constant voltage electrolysis, and the cell voltage is 3.0V. After 2 hours of electrolysis respectively, the electrolyzed product was rinsed with 1% by volume dilute hydrochloric acid, water, and absolute ethanol, and vacuum-dried to obtain a product such as figure 1 As shown, it is a curved silicon nanowire with a diameter of about 50 nm and a length of 2-5 micro...

Embodiment 2

[0068] 75 wt% of SiO with a purity of 99.95% and an average particle size of 0.25 μm 2 The powder is mixed with 25wt% binder (as SiO 2 The total weight of the powder and the binder is 100%), pressed by mechanical pressure at 10MPa to a diameter of about 10mm, a thickness of 1.2mm, heated at 1200°C in air for about 4 hours, and the sintered SiO 2 The small piece is combined with a conductive cathode current collector as the cathode, and the graphite rod is used as the anode to melt the CaCl 2 As an electrolyte, in an argon environment, the temperature is 1000°C, and the voltage is controlled by a voltage regulator for constant voltage electrolysis, and the cell voltage is 2.0V. After 4 hours of electrolysis, the electrolyzed product was washed with 1% dilute hydrochloric acid, water and absolute ethanol successively by volume percentage, and vacuum-dried to obtain the product such as Figure 5 As shown, the product is mainly curved silicon nanowires / tubes with a diameter of 5...

Embodiment 3

[0070] 75wt% of nano-SiO with a purity of 99.95% 2 The powder is mixed with 25wt% binder (as SiO 2 The total weight of the powder and the binder is 100%), pressed by mechanical pressure at 15MPa to a diameter of about 10mm and a thickness of 1.5mm, heated in air at 100°C for about 1.5 hours and then heated to 1100°C for 3 hours, and the sintered molded SiO 2 The small piece is combined with the conductive cathode current collector as the cathode, the graphite rod as the anode, and the CaCl 2 +NaCl mixed salt is the electrolyte (wherein CaCl 2 Accounting for 51% of the total weight of the mixed salt, NaCl accounts for 49%), in an argon atmosphere, the temperature is 600 ° C, the voltage is controlled by a voltage regulator to carry out constant voltage electrolysis, and the cell voltage is 2.5V. After 5 hours of electrolysis, the electrolyzed product was rinsed with 1% dilute hydrochloric acid, water and absolute ethanol successively by volume percentage, and vacuum-dried to...

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Abstract

The invention provides an electrochemical method for directly preparing silicon nano power and nanowires (tubes) from a compound SiX or a mixture containing the compound SiX, which is characterized by comprising the following steps of: by using the compound SiX or the mixture containing the compound SiX as a cathode, setting an anode; placing the anode in electrolyte containing metallic compound fused salt; applying voltage between the cathode and the anode; controlling reaction conditions; and preparing the silicon nano power and the nanowires (tubes) on the cathode. The invention has the advantages of short production process without pollution, easy operation and material obtaining, inexpensive equipment and easy continuous production, also opens a new field for applying the electrochemical method to the preparation of one-dimensional nano materials and explores a new way for preparing the silicon nano power and the nanowires (tubes).

Description

technical field [0001] The invention relates to a method for preparing silicon nano powder and nano wire (tube) by electrochemical method. Background technique [0002] One-dimensional nano-silicon wire (tube) materials have attracted extensive attention of researchers due to their unique electrical and optical properties and high surface activity. At present, there are various methods for preparing silicon nanowires (tubes), including laser ablation [Morales A M, Lieber C M. Science, 1998, 279 (9): 208-211; Lee C S, Wang N, Tang Y H, et al. al.MRS.Bulletin., 1999:36~41], chemical vapor deposition (CVD) [Wang N L, Zhang Y J, Zhu J.Journal of Materials Science Letters, 2001, 20:89~91], plasma enhanced chemical vapor deposition Deposition (PECVD) [Zeng X B, Xu Y Y, Zhang S B, et al.Journal of Crystal Growth, 2003, 247(1): 13~16], thermal vapor deposition [Feng S Q, Yu D P, Zhang H Z, et al.Journal of Crystal Growth, 2000, 209: 513~517], solution method [Holmes J D, Johnston ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00C30B29/06C30B29/62C30B30/02C01B33/021
CPCC01B33/021Y10S977/899C30B9/14C25B1/006C30B29/06Y10S977/762C30B29/60Y10S977/814C25B1/33
Inventor 卢世刚杨娟玉张向军阚素荣
Owner CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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