Porous silicon material and preparation method thereof

A technology of porous silicon and organosilicon, which is applied in the direction of halosilane and silicon halide compounds, can solve the problems of high production cost of porous silicon materials, polluting industrial production, and complicated processes, and achieves low production costs, uniform pore size, and high process efficiency. simple effect

Inactive Publication Date: 2014-01-15
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] One of the purposes of the present invention is to provide a preparation method of porous silicon material, adopt industrial silicon and methyl chloride (MeCl) catalytic reaction technology, by adjusting the reaction temperature, reaction time, silicon powder and solid copper-based catalyst particle size and its The mass ratio and different copper-based catalysts are used to control the pore size, porosity and silicon yield of silicon, so as to prepare porous silicon materials with uniform and adjustable pore size. At the same time, the reaction by-product chlorosilane can be recycled, solving the problem of porous silicon Problems such as high material production cost, complex process, serious pollution and difficulty in industrial production

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  • Porous silicon material and preparation method thereof
  • Porous silicon material and preparation method thereof
  • Porous silicon material and preparation method thereof

Examples

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Embodiment 1

[0041] Mix 10 g of commercially purchased silicon fume raw material (particle size range 10-100 μm) with commercially purchased Cu 2 10 grams of O powder (as a copper-based catalyst, particle size range 1-5 microns), 1 gram of zinc powder, mixed and ground evenly, then packed into a fixed-bed reactor, fed with methyl chloride gas (gas velocity is 30ml / min), adjusted The pressure is 0.3MPa. After preheating, the temperature is raised to 410°C. After 18 hours of reaction, it is cooled to room temperature. The gaseous product in the reaction process becomes a mixture of organosilicon monomers after condensation, and can be separated into chemicals by rectification later. Unreacted methyl chloride can be recycled. The solid residue after the reaction contains silicon and a solid copper-based catalyst. Air is introduced into a tube furnace (gas velocity: 100ml / min) and the temperature is raised to 500°C for 1 hour to remove carbon deposits, cooled to room temperature, and heated to...

Embodiment 2

[0049] Mix and grind 8 grams of commercially purchased silicon powder raw materials (with a particle size range of 5-50 microns), 5 grams of self-made Cu powder (as a copper-based catalyst, with a particle size range of 0.1-1 microns), and 0.2 grams of zinc powder. The fixed bed reactor is fed with methyl chloride gas (gas velocity is 30ml / min), and the pressure is adjusted to 1MPa. After preheating, the temperature is raised to 420°C. After 24 hours of reaction, it is cooled to room temperature, and the gaseous products in the reaction process are condensed Afterwards, it becomes a mixture of organosilicon monomers, which can be separated into chemicals by rectification in the later stage, and unreacted monochloromethane can be recycled. The solid residue after the reaction contains silicon and a solid copper-based catalyst. Air is introduced into the tube furnace (gas velocity is 200ml / min) and the temperature is raised to 600°C for 2 hours to remove carbon deposits, cooled t...

Embodiment 3

[0052] Combine 20 grams of commercially purchased silicon powder raw material (particle size range 1-20 microns) with commercially purchased Cu-CuCl powder 15 grams (as a copper-based catalyst, particle size range 0.1-10.0 microns), 2.0 grams of zinc powder, tin powder Mix and grind 0.05 grams evenly and put them into a fixed-bed reactor, feed in methyl chloride gas (gas velocity: 50ml / min), adjust the pressure to 0.6MPa, preheat, heat up to 480°C, react for 12 hours, and cool to room temperature , the gaseous product in the reaction process becomes a mixture of organosilicon monomers after condensation, which can be separated into chemicals by rectification in the later stage, and unreacted monochloromethane can be recycled. The solid residue after the reaction contains silicon and a solid copper-based catalyst. Air is introduced into a tube furnace (gas velocity: 100ml / min) and the temperature is raised to 500°C for 1 hour to remove carbon deposits, cooled to room temperature...

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Abstract

The invention relates to a porous silicon material and a preparation method thereof. The method for preparing the porous silicon material comprises the following steps: carrying out an in-situ catalytic reaction between a silicon material and chloromethane at the temperature of 401 to 800 DEG C in the presence of a solid copper-based catalyst, and preparing the porous silicon material through calcining, acid pickling, alkaline washing and other after-treatment impurity removal technologies, wherein the solid copper-based catalyst comprises one or a mixture of more than two in primary catalysts such as CuOx, CuCl and CuCl2, x is more than or equal to 0 and less than or equal to 1, as well as a small amount of secondary catalysts. Reaction condition parameters are regulated, so that the pore size, pore size distribution and porosity of the silicon material can be regulated. According to the method, a porous silicon material which is difficultly obtained in the patented technology at present is obtained, and important organic silicon monomer chemicals can be obtained. The porous silicon material prepared by the method is uniform in pore size, low in production cost, simple in process and suitable for industrial production and has wide application prospects.

Description

technical field [0001] The present invention relates to the field of porous silicon materials, in particular, the present invention relates to a method for preparing porous silicon materials by catalytic reaction of silicon and methyl chloride on solid copper-based catalysts and the prepared porous silicon materials. Background technique [0002] Porous silicon is a new functional porous material with a pore size ranging from nanometers to millimeters. Due to its unique dielectric properties, optical properties, microelectronic compatibility, large specific surface area and pore controllability, it is widely used in biological analysis, It has a wide range of applications in the fields of immune detection, insulating materials, sensitive components and sensors, lighting materials, optoelectronic devices, integrated circuits, solar cells and lithium-ion batteries. Porous silicon is a new type of semiconductor optoelectronic material with excellent photoluminescence and electr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/107
Inventor 苏发兵张在磊王艳红朱永霞翟世辉
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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