Preparation device and preparation method of high-purity electronic-grade diiodosilane

Abstract

The invention provides a preparation device and a preparation method of high-purity electronic-grade diiodosilane, and relates to the technical field of diiodosilane purification. The preparation device comprises a first reactor, a second reactor and a vacuum rectification purifier. The first reactor is divided into a fluidized bed section, an oil phase section and a hydrogen iodide section; the lower ends of the oil phase section and the hydrogen iodide section are connected to the second reactor. The preparation method of the high-purity electronic-grade diiodosilane comprises the following steps: nitrogen replacement; initiating reaction by adopting phenylsilane, an oxygen-containing compound catalyst and an aromatic organic solvent to generate a phenylsilane layer, a monoiodobenzene silane layer and a hydrogen iodide layer; continuously introducing phenylsilane, adjusting the flow of the discharge port and the flow of the phenylsilane, and controlling the interface of the monoiodobenzene silane layer and the hydrogen iodide layer to be on the interface of the oil phase section and the hydrogen iodide section; and rectifying under reduced pressure. According to the preparation device and the preparation method, side reactions are reduced by isolating the contact between phenylsilane and HI, and the purity of the product and the conversion rate of raw materials are improved.

Description

technical field [0001] The invention relates to the technical field of diiodosilane purification, and in particular to a high-purity electronic-grade diiodosilane preparation device and a preparation method thereof. Background technique [0002] Diiodosilane, molecular formula SiH 2 I 2 , CAS No. 13760-02-6, referred to as DIS, is widely used in the catalytic reaction process of silylation and halosilylbenzene. [0003] With the development of semiconductor manufacturing process, diiodosilane is used as an important silicon source for chemical vapor deposition (CVD). Due to the appropriate bond angle between Si-I, the diiodosilane molecules can be arranged side by side on the surface of silicon / silicon dioxide regularly, and when ammonia gas is introduced, it can evenly react to the thickness of the molecular layer of silicon nitride, that is formed by atomic layer deposition (ALD). Moreover, under plasma enhancement, diiodosilane can generate more active silicon radical...

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Problems solved by technology

[0004] The synthesis and purification of diiodosilane only existed in the gram-level experimental stage in the past. Due to the problem of low reaction controllability, no reports of industrial-scale continuous production have been found.

Therefore, the by-product SiH in the crude product 3 There is a lot of I, and the conversion rate of raw materials is reduced

[0011] 2. HI is easy to volatilize, and after a large amount of HI is lost, it cannot effectively interact with Ph-SiH 2 Continue to react, so Ph-SiH in the raffinate 2 I waste a lot, and the conversion rate is further reduced

[0012] 3. The reaction time is very long, and the output scale is small, mainly gram-level production

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