Preparation method of electronic grade tetraethoxysilane

A tetraethyl orthosilicate, electronic-grade technology, applied in the direction of silicon organic compounds, can solve problems affecting the uniformity and flatness of the film layer, expensive gas chromatograph equipment, and reduce the insulation performance of the film layer, etc., to achieve low product cost , promote sustainable and stable development, and facilitate operation

Active Publication Date: 2014-05-07
贵州威顿晶磷电子材料股份有限公司
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  • Description
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Problems solved by technology

[0004] The content of industrial tetraethyl orthosilicate can reach 99% after general preparation, but it still contains up to 1% of impurities. Among them, metal ions are electrically active impurities, which will reduce the SiO deposited on semiconductor devices. 2 The insulation performance of the thin film layer will cause the micron-scale circuits to be connected to each other, resulting in the scrapping of the circuit board; the non-electrically active impurities such as water and organic matter will affect the uniformity

Method used

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  • Preparation method of electronic grade tetraethoxysilane

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Embodiment 1

[0027] A preparation method of electronic grade tetraethyl orthosilicate: (1) Take 12kg of industrially synthesized crude tetraethyl orthosilicate in a 20L polytetrafluoroethylene container, add 0.36kg of analytically pure ethylenediaminetetraacetic acid complex mixture, fully mixed and stirred for 30 minutes, and then filtered with a 0.1 micron microporous filter; (2) Pass the collected filtrate through a cation exchange column device to further remove metal impurities and collect the filtrate; (3) Collect the filtrate The filtrate was added to a plate-type quartz distillation tower for distillation, and after 7 hours of total reflux, the fraction was collected from the top of the tower at 163°C; (4) The collected fraction was distilled through a sub-boiling distiller, and the voltage of the heating device of the sub-boiling distiller was adjusted , maintain the liquid surface temperature at 95°C, collect the distilled product at 95°C, and take samples for testing; (5) The obt...

Embodiment 2

[0031] A preparation method of electronic grade tetraethyl orthosilicate: (1) Take 12 kg of industrially synthesized crude tetraethyl orthosilicate in a 20L polytetrafluoroethylene container, add 0.72 kg of analytically pure ethylenediaminetetraacetic acid complex mixture, fully mixed and stirred for 45 minutes, and then filtered with a 0.1 micron microporous filter; (2) Pass the collected filtrate through a cation exchange column device to further remove metal impurities and collect the filtrate; (3) Collect the filtrate The filtrate was added to a plate quartz distillation tower for distillation, and after 10 hours of total reflux, the fraction was collected from the top of the tower at 165°C; (4) Distill the collected fractions through a sub-boiling still, and adjust the voltage of the heating device of the sub-boiling still , maintain the liquid surface temperature at 98°C, collect the distilled product at 98°C, and take samples for testing; (5) The obtained product is fill...

Embodiment 3

[0035] A preparation method of electronic grade tetraethyl orthosilicate: (1) Take 12kg of industrially synthesized crude tetraethyl orthosilicate in a 20L polytetrafluoroethylene container, add 1.2kg of analytically pure ethylenediaminetetraacetic acid complex mixture, fully mixed and stirred for 60 minutes, and then filtered with a 0.1 micron microporous filter; (2) Pass the collected filtrate through a cation exchange column device to further remove metal impurities and collect the filtrate; (3) Collect the filtrate The filtrate was added to a plate quartz distillation tower for distillation, and after 15 hours of total reflux, the fraction was collected from the top of the tower at 163°C; (4) Distill the collected fractions through a sub-boiling still, and adjust the voltage of the heating device of the sub-boiling still , maintain the liquid surface temperature at 90°C, collect the distilled product at 90°C, and take samples for testing; (5) The obtained product is filled ...

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Abstract

The invention relates to a preparation method of electronic grade tetraethoxysilane and particularly relates to a preparation method of electronic grade tetraethoxysilane for chemical vapor deposition in semiconductor industry. The preparation method comprises the steps of firstly complexing most of metal impurities in raw materials by using a complexing agent, and then filtering by using a microporous filter of 0.1 micron; passing through a cation exchange tower, a quartz plate type distillation tower and a sub-boiling distiller, strictly controlling temperature, and removing trace metal impurities, ethanol, other organic impurities and water. The preparation method provided by the invention adopts conventional purification equipment and has the advantages of convenience in operation, effect of being conductive to industrial large-scale production and low product cost.

Description

technical field [0001] The invention relates to a preparation method of electronic grade tetraethyl orthosilicate, in particular to a preparation method of electronic grade tetraethyl orthosilicate used for chemical vapor deposition in the semiconductor industry. Background technique [0002] In the manufacture of semiconductor electronic components, the components must be encapsulated in glass, or glass is used as an interlayer insulating layer. Typically, the glass layer is SiO2 deposited on the wafer surface by chemical vapor deposition (CVD). 2 layer. [0003] At first, highly toxic and flammable silane was used as the source of vapor deposition. With the upgrading of electronic materials and technology, people pay more attention to its non-toxic, green and environment-friendly characteristics while pursuing high performance of the product. Compared with silane, the toxicity of tetraethyl orthosilicate is greatly reduced, and it is liquid at room temperature, so the op...

Claims

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Application Information

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IPC IPC(8): C07F7/04
Inventor 赵顺王天喜孙刚祝飘郭之军汪忠发蔡金刚陈进
Owner 贵州威顿晶磷电子材料股份有限公司
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