Method for preparing silicon oxide nanotube and two-dimensional ordered assembly body thereof

A technology for nanotubes and silicon oxide, applied in the field of preparing silicon oxide nanotubes and their two-dimensional ordered assemblies, can solve the problems of complex preparation process, high cost, uneven size of silicon oxide nanotubes, etc. Effects of controllable reaction conditions

Inactive Publication Date: 2012-12-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Previously, most of the templates used in the preparation of silicon oxide nanotubes were hard templates such as carbon nanotubes and metal oxide nanorods. The preparation process was complicated and the cost was high; The few cases of silica nanotubes obtained by the soft template method based on surfactants are not uniform in size, and it is difficult to achieve precise control of their diameter and length (Satishkumar, B. C.; Govindaraj, A.; Vogl, E. M.; Basumallick , L.; Rao, C. N. R. J. Mater. Res.1997, 12, 604. Martin, C. R. Science 1994, 266 , 1961. Gao, C. B.; Lu, Z. D.; Yin, Y. D. Langmuir2011, 27, 12201. Harada, M.; Adachi, M. Adv. Mater. 2000, 12, 839.)

Method used

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  • Method for preparing silicon oxide nanotube and two-dimensional ordered assembly body thereof
  • Method for preparing silicon oxide nanotube and two-dimensional ordered assembly body thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: 30 mg PEO- b -PS was dissolved in 8 g tetrahydrofuran, and 1.5 g 2 M HCl aqueous solution was added to obtain a clear and transparent solution. Stir and volatilize overnight (12 h) at room temperature at about 5°C; add 0.30 g ethyl orthosilicate to the above solution , keep stirring (rotating at 100 rpm) to volatilize (if preparing a two-dimensional ordered assembly of silicon oxide nanotubes, add 20 mg 1,2 -bis(triethoxysilyl)ethylene), until a large amount of white precipitate appeared at the end; washed with water and collected by centrifugation, dried at 15°C; then dispersed in 2 M HCl aqueous solution, heated at 100°C for 24 h; collected water The hot product was dried at 15°C; the resulting white solid was calcined in a muffle furnace at 550°C for 5 h.

Embodiment 2

[0021] Example 2: 30 mg PEO- b -PS was dissolved in 10 g tetrahydrofuran, and 2 g 2 M HCl aqueous solution was added to obtain a clear and transparent solution, which was stirred and volatilized at room temperature at about 10 °C overnight (8 h); 0.30 g methyl orthosilicate was added to the above solution , keep stirring (200 rpm) to volatilize (if preparing a two-dimensional ordered assembly of silicon oxide nanotubes, add 50 mg of orthosilicate 4 h after adding 1,2 -bis(triethoxysilyl)ethane), until a large amount of white precipitate appeared at the end; washed with water and collected by centrifugation, dried at 25°C; redispersed in 2 M HCl aqueous solution, heated at 120°C for 20 h; collected The hydrothermal product was dried at 25 °C; the obtained white solid was calcined in a muffle furnace at 500 °C for 6 h.

Embodiment 3

[0022] Example 3: 30 mg PEO- b -PS was dissolved in 10 g tetrahydrofuran, and 1.5 g 2 M HCl aqueous solution was added to obtain a clear and transparent solution, which was stirred and volatilized overnight (10 h) at a room temperature of about 10 °C; 0.30 g tetraethyl orthosilicate was added to the above solution , keep stirring (rotating at 200 rpm) for volatilization (if preparing a two-dimensional ordered assembly of silica nanotubes, add 30 mg of diethyldiethoxysilane 3 h after adding methyl orthosilicate) , until a large amount of white precipitate appeared at the end; washed with water and collected by centrifugation, dried at 20 °C; then dispersed in 2 M HCl aqueous solution, heated at 80 °C for 30 h; collected hydrothermal products, dried at 20 °C; The white solid is dispersed in excess sodium hydroxide solution, heated to 80-100°C and refluxed to remove the template agent; the obtained solid is collected by centrifugation, washed with water and then dried.

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Abstract

The invention belongs to the technical field of an advanced nano-composite material, and particularly relates to a method for preparing a silicon oxide nanotube and a two-dimensional ordered assembly body of the silicon oxide nanotube. In the method, two segmented copolymers prepared in the laboratory are used as a template agent, a solvent volatizing inducing gathering self-assembly method is adopted, and a silicon oxide nanotube material with even bore diameter and length is mildly synthesizing under room temperature by taking tetraethoxysilane and the like as a silicon source, wherein the diameter is approximately to be 50nm, and the mean length is approximately to be 500nm. Under the condition that a small quantity of organosilane is added, the obtained silicon oxide nanotube can be assembled to form into a two-dimensional ordered nanopore material. The synthesized silicon oxide nanotube has even one-dimensional closed pore channel, biocompatibility, photoluminescence property, surface paintability and the like, so that the silicon oxide nanotube is wide in application prospects in the aspects such as the heterogeneous catalysis, drug load, limited range synthesis, nano-electronic appliance and environment monitoring sensor. The raw materials are easy to obtain, and the method is simple in technology, controllable in reaction conditions, free from high-temperature reaction, and suitable for expanded production.

Description

technical field [0001] The invention belongs to the technical field of advanced nanocomposite materials, and specifically relates to a method for preparing silicon oxide nanotubes and two-dimensional ordered assemblies thereof. Background technique [0002] As a typical one-dimensional nanomaterial, silicon oxide nanotubes have attracted extensive research interest from scientists all over the world in recent years. Due to the excellent physical and chemical properties of silica nanotube materials, such as biocompatibility, photoluminescence, and surface modification, they can be used in heterogeneous catalysis, drug loading, confinement synthesis, nanoelectronic devices, environmental Monitoring sensors and other fields have shown broad application prospects. [0003] Previously, most of the templates used in the preparation of silica nanotubes were hard templates such as carbon nanotubes and metal oxide nanorods. The preparation process was complicated and the cost was hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y40/00
Inventor 王春岳秦王明宏邓勇辉赵东元
Owner FUDAN UNIV
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