Preparation method of silicane gas

A technology of gas and silane, which is applied in the field of electronic gas preparation, can solve the problems of difficult control of catalytic rate, low reaction activity, and easy hydrolysis of products, so as to inhibit the reaction of copper-catalyzed decomposition of alcohol dehydrogenation, increase reaction yield, and promote The effect of reaction rate

Active Publication Date: 2010-03-17
HARBIN INST OF TECH
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Problems solved by technology

[0006] The purpose of the present invention is to solve the difficulty of controlling the catalytic rate, the difficulty of catalyst feeding, and the difficulty of recovery in the existing process for preparing silane gas. In the preparation process of the raw material trialkoxysilane used for preparing sil...

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  • Preparation method of silicane gas
  • Preparation method of silicane gas

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specific Embodiment approach 1

[0026] Specific embodiment one: the preparation method of a kind of silane gas of this embodiment is realized through the following steps:

[0027] 1. Synthesis of trialkoxysilane: a. Put 100 mesh to 350 mesh metallurgical grade silicon powder in a mixed acid of hydrofluoric acid and nitric acid, and then etch for 0.5 to 2 minutes under the action of ultrasound, and then etch The silica powder is rinsed to neutrality and then dried, wherein the ratio of the amount of hydrofluoric acid to nitric acid is (1 / 10~10): 1;

[0028] b. Add the silicon powder etched in step a to the copper-based catalyst pre-precipitation solution, vacuumize, and then under the action of ultrasound, add the precipitation initiator to the mixed solution of the silicon powder and the copper-based catalyst pre-precipitation solution until no Copper-based catalyst precipitates are formed, then filtered, and then vacuum-dried to obtain a copper-based catalyst-coated silicon powder complex, and then pretreat...

specific Embodiment approach 2

[0037] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the particle size of the silicon powder in step 1 a is 200 mesh. Other steps and parameters are the same as those in Embodiment 1.

[0038] In this embodiment, silicon powder is a commercial product.

specific Embodiment approach 3

[0039] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the ultrasonic frequency of the ultrasonic action in Step 1 a is 40-80KHz. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

A preparation method of silicane gas relates to a preparation method of electronic gas. The preparation method solves the problems that in the existing technology for preparing silicane gas, catalyticrate is difficult to be controlled, catalytic agent feeding is difficult, recycling difficulty is big, copper silicon contacts have slow productivity and low reactive activity in the preparation process of trialkoxysilanesby, the catalytic agent easily loses effectiveness after meeting water, the products are easily hydrolyzed, and the utilization rate of alcohol is low. The preparation method ofsilicane gas comprises the following steps: 1. preparing trialkoxysilanesby by using silicon powder and alcohol; 2. preparing catalytic controlled release formulations; and 3. using trialkoxysilanesby obtained in the step one to prepare silicane gas by reaction under the action of the catalytic controlled release formulations. The selectivity of trialkoxysilanesby prepared by the method reaches 95% and transformation ratio thereof reaches 90%; in the preparation method, the resolution ratio of the trialkoxysilanesby is 99.8%, silicane productivity is 90-93% and the purity is 99%; and silicanecan be used for preparing noncrystalline silicon thin film solar batteries and used in LED, LCD industries.

Description

technical field [0001] The invention relates to a method for preparing electron gas. Background technique [0002] Silane (SiH 4 ) is an ultra-high-purity electronic gas obtained by purifying silicon metal through a series of physical and chemical reaction processes. It is an extremely important intermediate product in the silicon product industry chain. The main raw materials of devices such as thin film transistors and flat panel displays are the basic raw materials for the information industry and the new energy industry, and play a pivotal role in the industrial chain. [0003] At present, the most advanced silane preparation process in the world is the process of disproportionation of alkoxysilane to prepare silane. However, the catalysts used in the existing process of disproportionation of alkoxysilane to prepare silane are all solid powders, and there are difficulties in catalyst feeding and catalytic rate control. Problems such as difficulty in catalyst recovery, ...

Claims

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Application Information

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IPC IPC(8): C01B33/04B01J27/122B01J23/72B01J37/03B01J37/02B01J21/18
Inventor 杨春晖张磊杨恺胡成发李季葛士彬
Owner HARBIN INST OF TECH
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