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Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon

A porous silicon, unreacted technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of high cost, serious pollution, difficult to treat fluorine-containing wastewater, etc., and achieves simple process, clean preparation, and easy scale. The effect of chemical production

Inactive Publication Date: 2012-11-28
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

[0004] Although wet chemical etching and electrochemical etching are the main methods for preparing porous silicon materials, there are some new patent applications for improvement and innovation every year, but it can be seen from the above patent applications that the preparation of porous silicon materials The process is relatively complicated, not suitable for large-scale production, requires highly toxic reagents such as hydrofluoric acid, and produces a large amount of difficult-to-treat fluorine-containing wastewater, resulting in high cost and serious pollution

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  • Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon
  • Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon
  • Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon

Examples

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Embodiment 1

[0036] Take 1g of commercial copper powder catalyst and 10g of silicon powder according to the required particle size and mix evenly, fill it in a fixed bed reactor, and pass in methylene chloride for reaction, wherein, the reaction temperature is 300°C, the pressure is 0.2MPa, and the space velocity of methylene chloride 100h -1 , after reacting for 10 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 50% of the silicon is unreacted and transformed, and the porosity of the porous silicon material is 53% (the calculation method is: porosity=1-bulk density / true density). The gaseous product in the reaction process is condensed into a mixture of organosilicon monomers, which can...

Embodiment 2

[0045] Take 1g of commercial copper powder catalyst and 10g of silicon powder according to the required particle size, mix evenly, fill it in a fixed bed, and pass in methylene chloride for reaction, wherein the reaction temperature is 300°C, the pressure is 0.3MPa, and the space velocity of methylene chloride is 100h -1 , after reacting for 5 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 60% of the silicon is unreacted and transformed, and the porosity of the porous silicon material is 41%. The pore distribution is measured according to the method of Example 1, and the pore diameter of the porous silicon material is 0.1 micron to 15 micron, mainly concentrated at about 3.3...

Embodiment 3

[0047] Take 1g of commercial copper powder catalyst and 10g of industrially pure raw silicon powder according to the required particle size, mix evenly, pack in a fixed bed, and feed in methylene chloride for reaction, wherein, the reaction temperature is 310°C, the pressure is 0.3MPa, and the air of methylene chloride is speed is 100h -1 , after reacting for 15 hours, cool to room temperature, take out the solid residue, place it in a high-temperature furnace for calcination in air, the calcination temperature is 600°C, and the calcination time is 1 hour. Remove non-silicon impurities, wash twice with distilled water, filter, and dry in a drying oven at 120° C. for 2 hours to obtain a porous silicon material. 10% of the silicon is unreacted and converted, and the porosity of the porous silicon material is 73%. The pore distribution is measured according to the method of Example 1, and the pore diameter of the porous silicon material is 0.01 micron to 8 micron, mainly concent...

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Abstract

The invention relates to the field of preparation of porous silicon materials, in particular to a method for preparing a porous silicon material by using a catalytic reaction of silicon and halogenated hydrocarbon. The method for preparing the porous silicon material, which is disclosed by the invention, comprises the following steps of: firstly, carrying out a heating reaction of silicon and gaseous halogenated hydrocarbon under the action of a solid catalyst and controlling the silicon to undergo an incomplete reaction; and secondly, separating the un-reacted silicon and removing impurities to obtain the porous silicon material. The aperture size, the distribution and the porosity factor of the silicon material can be controlled by adjusting reaction condition parameters. By using the method disclosed by the invention, the porous silicon material which is difficult to obtain by the present patent technology can be obtained, important organic silicon monomer chemical products can be also obtained, and the clean production of the porous silicon material can be realized; and the method is simple in process and has wide application prospect.

Description

technical field [0001] The invention relates to the field of preparation of porous silicon materials, in particular, the invention relates to a method for preparing porous silicon materials by utilizing the catalytic reaction of silicon and halogenated hydrocarbons. Background technique [0002] Porous silicon is a new type of sponge-like functional porous material with a pore size of nanometer to millimeter order. Its unique optical properties, dielectric properties, microelectronic compatibility, filterability, pore controllability and large specific surface area make it It has a wide range of applications in the fields of biological analysis, 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. It has excellent photoluminescence and electroluminescence properties at room tempera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/021
Inventor 苏发兵高俊杰翟世辉许光文
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI