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Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia

A technology of alloying and compounding, applied in the direction of silicon hydride, etc., can solve the problems of difficult production of monosilane, limited practicality, high alloying temperature, etc., and achieve the effects of high yield, improved production efficiency, and low energy consumption

Active Publication Date: 2013-02-20
烟台万华电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the alloying temperature is high, the yield of disilane is limited to less than 25%, and it is difficult to greatly adjust the yield of monosilane, which limits their practicability as the main product for large-scale production

Method used

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  • Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia
  • Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia

Examples

Experimental program
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Effect test

Embodiment 1

[0030] A method for producing disilane by mechanically compounding hydrogenated metal-silicon after alloying and chemically reacting with ammonium chloride in a liquid ammonia medium, characterized in that the composition of the hydrogen-metal-silicon compound is Si 33.2%, Mg 66.5%, H 0.3%, the above percentages are molar percentages, and the reaction is carried out according to the following principles to improve reaction efficiency and disilane productive rate:

[0031] SiO 2 + 2MgH 2 =SiMg 2 + 2H 2 O

[0032] SiMg 2 H 0.01 + NH 4 Cl → MgCl 2 + H 2 + NH 3 + SiH 4 + Si 2 H 6

[0033]The alloying temperature is 500°C, monosilane is completely absorbed and transformed by the reflux silane absorption converter, the gas-liquid separation temperature is controlled at -40°C, and monosilane reacts with 2N KOH aqueous solution to produce hydrogen and potassium silicate, no by-products are produced, After disilane is sepa...

Embodiment 2

[0035] A method for producing disilane by mechanically compounding hydrogenated metal-silicon after alloying and chemically reacting with ammonium chloride in a liquid ammonia medium, characterized in that the composition of the hydrogen-metal-silicon compound is Si 32.1%, Mg 64.4%, V 3.2%, H 0.3%, the above percentages are mole percentages, and the reaction is carried out according to the following principles to improve efficiency and disilane yield:

[0036] SiO 2 + 2MgH 2 =SiMg 2 + 2H 2 O

[0037] SiMgV 0.1 H 0.01 + NH 4 Cl → MgCl 2 + VCl 2 + H 2 + SiH 4 + Si 2 H 6

[0038] The alloying temperature is 550°C, the reaction is safe and stable, monosilane is completely absorbed and transformed by the reflux silane absorption converter, no by-products are produced, and disilane is separated and purified to obtain high-purity products.

Embodiment 3

[0040] A method for producing disilane by mechanically compounding hydrogenated metal-silicon after alloying and chemically reacting with ammonium chloride in a liquid ammonia medium, characterized in that the composition of the hydrogen-metal-silicon compound is Si 31.1%, Mg 62.1%, Fe 3.1%, H 2.5%, Li 0.6%, Al 0.6%, the above percentages are mole percentages, and the reaction is carried out according to the following principles to improve reaction efficiency and disilane yield:

[0041] Mg + SiO 2 + LiAlH 4 →SiMg 2 + H 2 O

[0042] Li 0.02 SiMg 2 Fe 0.1 Al 0.02 H 0.08 + NH 4 Cl → MgCl 2 + FeCl 2 +H 2 + SiH 4 + Si 2 H 6

[0043] The alloying temperature is low, the reaction is safe and stable, monosilane is completely absorbed and transformed by the reflux silane absorption converter, monosilane is cracked at 600°C high temperature, no by-products are produced, and disilane is separated and purified t...

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Abstract

The invention provide a method and a device used for producing disilane through a chemical reaction of alloyed hydrogen-metal-silicon composition ammonium chloride in a liquid ammonia medium. According to the invention, hydrogen-metal-silicon composition and a corresponding alloying process are promoted; the composition is subjected to the chemical reaction with ammonium chloride in the liquid ammonia medium, such that monosilane and disilane are produced; monosilane is outputted under the control of a reflux monosilane absorption converter, and crude disilane is subjected to separation purification, such that high-yield disilane is prepared. The hydrogen-metal-silicon composition is composed of Si, H, and at least two components selected from: Mg, Ca, Sr, Ba, Li, Na, K, B, Al, Ti, Fe, and V. The composition is synthesized through a mechanical process, a thermo-mechanical process, or a mechanical chemical bonding process, and is subjected to heat treatment alloying, such that the composition can be utilized.

Description

technical field [0001] The invention belongs to the field of gas production, and relates to an alloying process of a hydrogen-metal-silicon compound and produces monosilane (SiH 4 ), disilane (Si 2 h 6 ), trisilane (Si 3 h 8 ) and other methods are especially suitable for the production of disilane. technical background [0002] Disilane is a promising silicon membrane precursor. Compared with monosilane, it has the advantages of fast deposition speed, low temperature requirement, and high film uniformity, and is one of the attractive special gases in the semiconductor industry. However, the existing preparation methods of disilane are mainly due to low yield, many by-products, high production cost due to expensive equipment, or unrealistic large-scale production due to the limitation of the amount of raw materials. Among them, the reaction product of magnesium silicide and ammonium chloride in liquid ammonia is mostly monosilane, and less than 2% of disilane can only ...

Claims

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Application Information

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IPC IPC(8): C01B33/04
Inventor 贺孝鸣
Owner 烟台万华电子材料有限公司
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