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Preparation method and device of high-purity silicon tetrafluoride

A technology for preparing high-purity silicon tetrafluoride and equipment, applied in chemical instruments and methods, silicon halide compounds, halosilanes, etc., can solve problems such as high acidity, complex composition, and many impurities in silicon tetrafluoride, and achieve reduction Acidity, simple process, effect of improving purity

Active Publication Date: 2021-07-30
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is mostly a mixture of various substances, the composition is complex, and the silicon tetrafluoride produced has many impurities and high acidity, and the resulting product is difficult to handle and easy to hang on the wall, etc.

Method used

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  • Preparation method and device of high-purity silicon tetrafluoride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] A kind of preparation method of high-purity silicon tetrafluoride, described method adopts such as figure 1 The preparation device of a kind of high-purity silicon tetrafluoride shown is carried out, and step is as follows:

[0069] ①Place the elemental silicon particles 3 with a particle size of 0.1mm in layers on the layered plate 2 in the reaction tower 1, raise the temperature to a displacement treatment temperature of 80°C, open the vacuum valve 5 of the reaction tower, and connect the reaction tower through the vacuum pipeline 4. 1. Vacuumize the interior to -0.095MPa, close the vacuum valve 5 of the reaction tower, open the replacement gas feed valve 12, feed helium gas with a purity of 99.999% through the replacement gas pipeline 11 until the inside of the reaction tower 1 is at normal pressure, and complete one pass Replacement treatment, repeat the replacement treatment 3 times, until the moisture content detected in the helium after the treatment is 0.4ppm, i...

Embodiment 2

[0079] A kind of preparation method of high-purity silicon tetrafluoride, described method adopts such as figure 1 The preparation device of a kind of high-purity silicon tetrafluoride shown is carried out, and step is as follows:

[0080] ① Place the elemental silicon particles 3 with a particle size of 3mm in layers on the layered plate 2 in the reaction tower 1, raise the temperature to a displacement treatment temperature of 150°C, open the vacuum valve 5 of the reaction tower, and pass the vacuum line 4 to the reaction tower 1. Vacuumize the interior to -0.095MPa, close the vacuum valve 5 of the reaction tower, open the replacement gas feed valve 12, and feed helium gas with a purity of 99.999% through the replacement gas pipeline 11 until the inside of the reaction tower 1 is at normal pressure, and complete one round of replacement treatment, repeat the replacement treatment 8 times, until the moisture content detected in the helium after the treatment is 0.3ppm, indica...

Embodiment 3

[0090] A kind of preparation method of high-purity silicon tetrafluoride, described method adopts such as figure 1 The preparation device of a kind of high-purity silicon tetrafluoride shown is carried out, and step is as follows:

[0091] ① Place the elemental silicon particles 3 with a particle size of 1.5mm in layers on the layered plate 2 in the reaction tower 1, raise the temperature to a displacement treatment temperature of 120°C, open the vacuum valve 5 of the reaction tower, and connect the reaction tower through the vacuum pipeline 4. Vacuumize the inside of 1 to -0.095MPa, close the vacuum valve 5 of the reaction tower, open the replacement gas feed valve 12, and feed helium with a purity of 99.999% through the replacement gas pipeline 11 until the inside of the reaction tower 1 is at normal pressure, and complete one pass Replacement treatment, repeat the replacement treatment 5 times, until the moisture content detected in the helium after the treatment is 0.4ppm,...

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Abstract

The invention relates to a preparation method and device of high-purity silicon tetrafluoride, and belongs to the technical field of fluoride preparation. According to the method, crude SiF4 gas is prepared through reaction of HF and Si, the crude SiF4 gas is vacuumized at the temperature of-60 DEG C to-150 DEG C, light component impurities are removed, and the high-purity silicon tetrafluoride with the purity of 99.999% is obtained. The device mainly comprises a reaction tower, a layering plate, a vacuum pipeline, a discharging pipeline, a dust remover, a filter, a gas replacement pipeline, an HF pipeline, a gas distributor, an HF gas source, an emptying pipeline, a cooling kettle, a cooling column, a cooling pipeline, an analysis pipeline, an emptying pipeline and a thermometer. According to the method and the device, new impurities which are difficult to remove are not introduced, the flow rate of HF gas and the dosage of HF and Si are controlled, generation of fluosilicic acid is avoided, and the purity of the silicon tetrafluoride is improved; and the method and the device are simple in process, safe to operate and suitable for industrial production of the high-purity silicon tetrafluoride.

Description

technical field [0001] The invention relates to a method and a device for preparing high-purity silicon tetrafluoride, belonging to the technical field of fluoride preparation. Background technique [0002] Silicon fluoride is widely used in the electronics and semiconductor industries. It is an important raw material for the preparation of silane, crystalline silicon, and optical fibers. It can also be used to prepare cement and marble hardeners and photosensitizers. It has broad application prospects in the microelectronics industry. [0003] At present, various preparation methods of silicon tetrafluoride have been disclosed in existing documents or patents. CN109704345 of Zhejiang Zhongning Silicon Industry Co., Ltd. adopts a raw material storage tank, a compressor, a first heat exchanger, a second heat exchanger, a light removal tower, a weight removal tower and a finished product buffer tank for storing crude silicon tetrafluoride raw materials to prepare Silicon tetr...

Claims

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Application Information

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IPC IPC(8): C01B33/107
CPCC01B33/10705C01B33/10778
Inventor 王云飞柳彤林坤刘海芳张净普孙秋丽李海军蒋玉虎
Owner PERIC SPECIAL GASES CO LTD
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