Preparation method of silane

Abstract

The invention provides a preparation method of silane. The method comprises steps of albite decomposition reaction, silicon fluoride purification and silane preparation, wherein the albite decomposition reaction comprises steps as follows: mixing albite, fluorite and sulfuric acid with concentration of 98% at a mass ratio of 1: (1.55-2.57): (3.28-4.62) and performing reaction at the temperature of 100-200 DEG C under the self-generated pressure to obtain solid residues and silicon fluoride contained gas; the silicon fluoride purification comprises steps as follows: performing dust removal on the silicon fluoride contained gas, liquefying the silicon fluoride contained gas after dust removal to obtain a silicon fluoride liquid, removing hydrogen fluoride in the silicon fluoride liquid to obtain a silicon fluoride liquid free of hydrogen fluoride, and gasifying the silicon fluoride liquid free of hydrogen fluoride to obtain pure silicon fluoride gas; and silane preparation comprises step as follows: introducing the pure silicon fluoride gas into a sodium aluminum hydride solution for reaction to obtain a silane product. According to the preparation method, gas products including silicon fluoride and sodium aluminum hydride which are generated after albite decomposition are mainly utilized and react to prepare silane, and one novel silane preparation method capable of realizing continuous production is provided.

Description

technical field

[0001] The invention relates to a method for preparing silane, in particular to a method for preparing silane by using albite. Background technique

[0002] At present, microelectronics technology is the main cornerstone of modern information technology and military technology, and one of the key factors to promote scientific and technological progress, industrial development, economic take-off and social advancement. Integrated circuit is the core of microelectronics technology, and its development level and industrial scale have become an important symbol to measure a country's economic strength. Electronic specialty gases (such as silane), especially high-purity electronic gases as a new category of electronic chemical materials, are important factors restricting the reliability and yield of integrated circuits. With the rapid development of electronic information technology, the integration level is getting higher and higher, and the purity requirements ...

Examples

Embodiment 1

[0018] A kind of preparation method of silane, comprises the following steps:

[0019] Decomposition of albite feldspar: first preheat albite and fluorite at 100°C for about 30 minutes, then add 98% sulfuric acid to react the three at 100°C and autogenous pressure for about 5 hours, and obtain calcium sulfate and sodium sulfate And the solid residue of aluminum sulfate and the gas product containing silicon fluoride, among them, the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:1.55:3.28, and the reaction principle is:

[0020] CaF 2 + H 2 SO 4 = 2HF + CaSO 4

[0021] 2NaAlSi 3 o 8 + 24HF + 4H 2 SO 4 = Na 2 SO 4 +Al 2 (SO 4 ) 3 + 6SiF 4 ↑ + 16H 2 o

[0022] Purifying silicon fluoride: using a dust removal filter to remove dust in the silicon fluoride gas; condensing the dedusted silicon fluoride gas with water to obtain the silicon fluoride liquid; removing impurity hydrogen fluoride in the silicon liquid to obtain the hydrogen fluoride-free...

Embodiment 2

[0025] The preparation method of the silane provided in this example and Example 1 is basically the same, the difference is: in the process of albite decomposition, the preheating temperature is 150°C, and the preheating time is 20 minutes; the reaction temperature is 150°C, the reaction time is 3.5 hours, and the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:2:4; in the process of preparing silane, the mass ratio of silicon fluoride to sodium aluminum hydride solute The ratio is 3:50, and the reaction temperature is 220°C.

Embodiment 3

[0027] The preparation method of the silane provided in this example and Example 1 is basically the same, the difference is: in the process of albite decomposition, the preheating temperature is 200 ° C, and the preheating time is 15 minutes; the reaction temperature is 200°C, the reaction time is 2 hours, and the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:2.5:4.6; in the process of preparing silane, the mass ratio of silicon fluoride to sodium aluminum hydride solute The ratio is 1:18, and the reaction temperature is 210°C.

technical field

[0001] The invention relates to a method for preparing silane, in particular to a method for preparing silane by using albite. Background technique

[0002] At present, microelectronics technology is the main cornerstone of modern information technology and military technology, and one of the key factors to promote scientific and technological progress, industrial development, economic take-off and social advancement. Integrated circuit is the core of microelectronics technology, and its development level and industrial scale have become an important symbol to measure a country's economic strength. Electronic specialty gases (such as silane), especially high-purity electronic gases as a new category of electronic chemical materials, are important factors restricting the reliability and yield of integrated circuits. With the rapid development of electronic information technology, the integration level is getting higher and higher, and the purity requirements ...

Examples

Embodiment 1

[0018] A kind of preparation method of silane, comprises the following steps:

[0019] Decomposition of albite feldspar: first preheat albite and fluorite at 100°C for about 30 minutes, then add 98% sulfuric acid to react the three at 100°C and autogenous pressure for about 5 hours, and obtain calcium sulfate and sodium sulfate And the solid residue of aluminum sulfate and the gas product containing silicon fluoride, among them, the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:1.55:3.28, and the reaction principle is:

[0020] CaF 2 + H 2 SO 4 = 2HF + CaSO 4

[0021] 2NaAlSi 3 o 8 + 24HF + 4H 2 SO 4 = Na 2 SO 4 +Al 2 (SO 4 ) 3 + 6SiF 4 ↑ + 16H 2 o

[0022] Purifying silicon fluoride: using a dust removal filter to remove dust in the silicon fluoride gas; condensing the dedusted silicon fluoride gas with water to obtain the silicon fluoride liquid; removing impurity hydrogen fluoride in the silicon liquid to obtain the hydrogen fluoride-free...

Embodiment 2

[0025] The preparation method of the silane provided in this example and Example 1 is basically the same, the difference is: in the process of albite decomposition, the preheating temperature is 150°C, and the preheating time is 20 minutes; the reaction temperature is 150°C, the reaction time is 3.5 hours, and the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:2:4; in the process of preparing silane, the mass ratio of silicon fluoride to sodium aluminum hydride solute The ratio is 3:50, and the reaction temperature is 220°C.

Embodiment 3

[0027] The preparation method of the silane provided in this example and Example 1 is basically the same, the difference is: in the process of albite decomposition, the preheating temperature is 200 ° C, and the preheating time is 15 minutes; the reaction temperature is 200°C, the reaction time is 2 hours, and the mass ratio of albite, fluorite, and 98% sulfuric acid is 1:2.5:4.6; in the process of preparing silane, the mass ratio of silicon fluoride to sodium aluminum hydride solute The ratio is 1:18, and the reaction temperature is 210°C.