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A Halogen-Free Silane Method for Preparation of Solar Grade Silicon

A solar-grade, halosilane-based technology, which is applied in the fields of inorganic chemistry, silicon compounds, chemical instruments and methods, etc., can solve the problem that the specific components of the catalyst and the reaction conditions are not clearly stated, the chemical reaction formula is not given, and the application cannot be filed. Obtain authorization and other issues to achieve social and economic benefits, improve safety, and eliminate pollution

Inactive Publication Date: 2018-03-06
李绍光 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has no clear description of the specific components and reaction conditions of the catalyst used, and even the chemical reaction formula of each step is not given, so its application has not been authorized.

Method used

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  • A Halogen-Free Silane Method for Preparation of Solar Grade Silicon
  • A Halogen-Free Silane Method for Preparation of Solar Grade Silicon
  • A Halogen-Free Silane Method for Preparation of Solar Grade Silicon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Step (1) The chemically pure industrial silicon with a purity ≥ 99.00% and a particle size of 40 μm and the nano-scale copper hydroxide with a purity of more than 99.5% are subjected to high-temperature drying at 150°C for 5 hours and microwave irradiation for 15 minutes to activate the pretreatment, Then put it into the dodecylbenzene solution at 20°C, and then pass through the solution successively with water content -4 Analyze pure methanol and potassium nitrate with a purity ≥ 99.5%, make it react as follows to generate 99% trimethoxysilane and 1% tetramethoxysilane, and use distillation to separate tetramethoxysilane to obtain trimethoxysilane Silane:

[0055]

[0056]

[0057] Step (2) uses sodium nitrate solution as a catalyst to make trimethoxysilane undergo the following disproportionation reaction at 20°C to generate monosilane:

[0058]

[0059] Step (3) Use molecular sieves to absorb monosilane, then cool monosilane to -120°C in a liquid nitrogen ta...

Embodiment 2

[0067] Step (1) The chemically pure industrial silicon with a purity ≥ 99.30% and a particle size of 300 μm and the nano-scale copper hydroxide with a purity of more than 99.5% are subjected to high-temperature drying at 250° C. for 0.5 hours and microwave irradiation. Activate the pretreatment for 5 minutes, then put it into the dodecylbenzene solution at 120°C, and then pass through the solution with a water content of -4 Analyze pure methanol and sodium nitrate with a purity ≥ 99.5%, make it react as follows to generate ≥ 99% trimethoxysilane and ≤ 1% tetramethoxysilane, and use distillation to separate tetramethoxysilane to obtain pure Trimethoxysilane:

[0068]

[0069]

[0070] Step (2) uses potassium nitrate solution as a catalyst, and at 150° C., trimethoxysilane undergoes the following disproportionation reaction to generate monosilane:

[0071]

[0072] Step (3) Use activated carbon as an adsorbent to absorb monosilane, and then cool monosilane to -130°C in ...

Embodiment 3

[0079] Step (1) The chemically pure industrial silicon with a purity ≥ 99.68% and a particle size of 150 μm and the nano-scale copper hydroxide with a purity of more than 99.5% are subjected to high-temperature drying at 150° C. for 2.5 hours and microwave irradiation. Activate the pretreatment for 5 minutes, then put it into the alkyl biphenyl type heat transfer oil at 250°C, and then pass through the solution with water content -4 Analyze pure methanol and potassium nitrate with a purity ≥ 99.5%, make it react as follows to generate 99% trimethoxysilane and 1% tetramethoxysilane, and use distillation to separate tetramethoxysilane to obtain trimethoxysilane Silane:

[0080]

[0081]

[0082] Step (2) uses calcium nitrate solution as a catalyst, and at 250° C., trimethoxysilane undergoes the following disproportionation reaction to generate monosilane:

[0083]

[0084] Step (3) Use molecular sieves to absorb monosilane, and then cool monosilane to -160°C in a liquid...

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Abstract

A halogen-free silane method for preparing solar-grade silicon, which uses industrial silicon powder and anhydrous methanol (or ethanol) as raw materials, is characterized in that it includes the following steps: (1) reacting silicon powder with anhydrous methanol or ethanol to prepare Take trimethyl(ethyl)oxysilane; (2) disproportionate trimethyl(ethyl)oxysilane to produce monosilane; (3) separate and purify monosilane by adsorption and cooling methods; (4) thermally decompose monosilane Preparation of solar grade polysilicon. The present invention completely abandons the metal hydride method, the trichlorosilane disproportionation reaction method and the silicon-magnesium alloy method, and is different from the existing silane method that requires the use of halogen element compounds, i.e. fluoride or chloride, to participate in the reaction. It can effectively avoid the corrosion of the equipment and the pollution of the environment by the halogen compound. The thermal decomposition of monosilane is compared with the hydrogen reduction of trichlorosilane, and the ratio of silicon obtained by the two is very different. Therefore, its economic index is far better than that of the Siemens method, and it has great social and economic benefits.

Description

technical field [0001] The invention belongs to the technical field of silicon purification, and specifically relates to a new process for preparing monosilane without participating in the reaction of halogen (fluorine or chlorine) compounds, and using monosilane to prepare solar-grade polysilicon. Background technique [0002] The traditional methods for preparing solar-grade high-purity polysilicon mainly include: trichlorosilane hydrogen reduction method (Siemens method) and silane method. Since the core technology of the Siemens method is monopolized by several large foreign companies, domestic polysilicon enterprises have low reaction yields, heavy environmental pollution, and high costs during the production process, making them unable to operate normally. The above problems have not been solved for a long time, so some manufacturers have turned to consider whether it is possible to use the silane method to produce solar-grade polysilicon? [0003] The existing silane...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/029
Inventor 李绍光顾玉山
Owner 李绍光