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Method for preparing silicon nanotube

A technology of silicon nanotubes and nanospheres, which is applied in the field of preparation of silicon nanotubes, can solve the problems of limited application of silicon nanotubes, difficult to prepare in large quantities, and complicated preparation methods of tubular silicon nanowires, and achieves the effect of large specific surface area.

Active Publication Date: 2011-08-03
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation method of these tubular silicon nanowires is cumbersome, and it is not easy to be used in large-scale preparation, which limits the application of silicon nanotubes.

Method used

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  • Method for preparing silicon nanotube

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preparation example Construction

[0016] The method for preparing silicon nanotubes of the present invention uses Mg to SiO 2 The reduction effect of Fe, Ni, Cu, Zn, Nb, Al, Sn, C, etc. as a catalyst, the SiO 2 The nanospheres are reduced to silicon hollow nanotubes, thus obtaining silicon nanomaterials with a large specific surface area. The prepared silicon nanotubes are in the form of gray-black powder, and the inner diameters of the tubes are about 120-170nm. The silicon nanotubes are synthesized in two steps: (1) Hydrothermal synthesis of SiO using surfactants 2 Nanosphere precursor; (2) The solid-phase magnesium thermal method is used to synthesize silicon nanotubes under the action of Fe, Ni, Cu, Zn, Nb, Al, Sn, C and other catalysts.

[0017] The specific operations of the above steps are:

[0018] 1) Add 1 mmol of surfactant cetyltrimethylammonium bromide to the mixed solvent of 1,4-dioxane, ethanol and water, and the molar ratio of the solvent is composed of 1,4-dioxane: Ethanol: water = 2:8:10, stir unt...

Embodiment 1

[0021] The first step: mix 2mL 1,4-dioxane and 8mL ethanol, add 10mL H 2 O, add 1.0mmol cetyltrimethylammonium bromide to the above solution, stir to obtain a clear solution, weigh 8.0mmol urea, add to the above solution, and then stir to obtain a clear solution, slowly drop 2.0mmol orthosilicic acid Ethyl ester, stirred for 1h to obtain a colloidal solution, transferred to a hydrothermal reactor, reacted at 180℃ for 3h, cooled to room temperature, filtered and washed, dried at 60℃ to obtain white SiO 2 powder.

[0022] Step 2: Add 0.060g of the above SiO 2 The powder and 0.024g magnesium powder are mixed uniformly, put into a Nb tube, pass Ar protection, react in a tube furnace at 675°C for 10 hours, cool to room temperature, and still use Ar protection during cooling. The obtained product is protected by 2mol / Wash with L HCl and 0.3% HF, filter, and dry to obtain gray-black powder.

Embodiment 2

[0024] The first step: mix 2mL 1,4-dioxane and 8mL ethanol, add 10mL H 2 O, add 1.0mmol cetyltrimethylammonium bromide to the above solution, stir to obtain a clear solution, weigh 8.0mmol urea, add to the above solution, and then stir to obtain a clear solution, slowly drop 2.0mmol orthosilicic acid Ethyl ester, stirred for 1h to obtain a colloidal solution, transferred to a hydrothermal reactor, reacted at 180℃ for 3h, cooled to room temperature, filtered and washed, dried at 60℃ to obtain white SiO 2 powder.

[0025] Step 2: Add 0.060g of the above SiO 2 Mix the powder with 0.024g magnesium powder and 0.001g Nb powder evenly, put them in a quartz tube, pass in Ar protection, react in a tube furnace at 675°C for 10 hours, cool to room temperature, and still use Ar protection during cooling to obtain The product was washed with 2mol / L HCl and dilute HF, filtered, and dried to obtain gray-black powder.

[0026] figure 1 The scanning electron microscope test showed that the obtained...

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Abstract

The invention relates to a method for preparing a silicon nanotube. SiO2 nano balls are reduced into the silicon nanotube under the action of a catalyst by using the reducing action of Mg on SiO2. The prepared silicon nanotube is gray black powder and the inner diameter of the tube is in a range of 120 to 170nm. The silicon nanotube is synthesized by the following two steps of: (1) synthesizing a SiO2 nano ball precursor by using a surfactant through the hydrothermal synthesis method; and (2) synthesizing the silicon nanotube under the action of the catalyst, such as Fe or Ni or Cu or Zn or Nb or Al or Sn or C and the like by solid-phase magnesiothermy. The silicon nanotube prepared by the method has the common characteristics of a nanowire and a hollow nano material. A scanning electron microscope test shows that the obtained material is the hollow silicon nanotube and the inner diameter of the hollow tube is in the range of 120 to 170nm. A nitrogen adsorption test at the absolute temperature of 77K shows that the specific surface area (BET) of the material is 531m<2> / g.

Description

Technical field [0001] The invention relates to a method for preparing silicon nanotubes. Background technique [0002] Nanomaterials refer to various solid materials with a certain dimension in the range of 1-100nm. Due to the reduction of the scale and the change of the surface state, the nanomaterials lead to the generation of surface effects, small size effects, quantum effects and macroscopic quantum tunneling effects. Therefore, they will inevitably exhibit chemical activity, magnetism, light absorption, light reflection, and catalysis. Special nature. Silicon is a semiconductor material with excellent performance and a wide range of applications. The preparation of its nanomaterials, especially nanowires, has attracted great attention. Treuting and Arnold were the first to report on silicon nanowires. They successfully grew silicon needle-like crystals, which are now called nanowires. Later in the 1960s, Wagner and Ellis proposed the well-known vapor-liquid-solid (VLS) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/021B82Y40/00
Inventor 刘美玭杜红宾游效曾
Owner NANJING UNIV
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