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Refining method of tetrakis(dimethylamido)titanium

A technology of dimethylamino and refining methods, which is applied in the field of purification of amino titanium, can solve the problem that the purity of titanium is difficult to exceed 99.99%.

Active Publication Date: 2018-05-22
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purity of tetrakis(dimethylamino)titanium used in existing patents and documented technologies is difficult to exceed 99.99% after rectification

Method used

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  • Refining method of tetrakis(dimethylamido)titanium

Examples

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Embodiment 1

[0019] A method for refining tetrakis(dimethylamino)titanium, comprising the following steps:

[0020] (1) In parts by weight, 100 parts of polysulfone hollow fiber ultrafiltration membranes are immersed in 1500 parts of deionized water and 8 parts of 2-hydroxyl-4-trifluoromethylaniline mixed solution, soaked for 17 hours, and taken out Dry it in the air, then immerse it in 1800 parts of n-hexane, 19 parts of trimesoyl chloride, soak it for 15 hours, take it out, dry it at 60°C, then immerse it in 1500 parts of n-hexane, 0.005 part of 2,4-decadienal, In a mixed solution of 0.004 parts of dicyclopentadiene titanium dichloride and 0.08 parts of 3,3-diallyltetrahydrofuran-2-ol, N 2 For protection, 60Co γ-ray irradiation dose is about 30kGy, and the irradiation time is 19 minutes. The grafted membrane is taken out, and the surface of the membrane is cleaned with 1500 parts of methanol and dried to obtain tetrakis(dimethylamino)titanium purification permeation membrane.

[0021] (...

Embodiment 2

[0023] A method for refining tetrakis(dimethylamino)titanium, comprising the following steps:

[0024] (1) In parts by weight, 100 parts of polysulfone hollow fiber ultrafiltration membranes are immersed in 1000 parts of deionized water and 3 parts of 2-hydroxyl-4-trifluoromethylaniline mixed solution, soaked for 10 hours, and taken out Dry it in the air, then immerse it in 1000 parts of n-hexane, 10 parts of trimesoyl chloride, soak for 10 hours, take it out, dry it at 50°C, then immerse it in 1000 parts of n-hexane, 0.001 part of 2,4-decadienal, In a mixed solution of 0.001 part of dicyclopentadiene titanium dichloride and 0.01 part of 3,3-diallyltetrahydrofuran-2-ol, N 2 For protection, 60Co γ-ray irradiation dose is about 10kGy, and the irradiation time is 30 minutes. The grafted membrane is taken out, and the surface of the membrane is cleaned with 1000 parts of methanol, and dried to obtain tetrakis(dimethylamino)titanium purification permeation membrane.

[0025] (2) I...

Embodiment 3

[0027] A method for refining tetrakis(dimethylamino)titanium, comprising the following steps:

[0028] (1) In parts by weight, 100 parts of polysulfone hollow fiber ultrafiltration membranes are immersed in 2000 parts of deionized water and 10 parts of 2-hydroxyl-4-trifluoromethylaniline mixed solution, soaked for 30 hours, and taken out Dry it in the air, then immerse it in 2000 parts of n-hexane, 30 parts of trimesoyl chloride, soak it for 30 hours, take it out, dry it at 80°C, then immerse it in 2000 parts of n-hexane, 0.01 part of 2,4-decadienal, In a mixed solution of 0.01 part of dicyclopentadiene titanium dichloride and 0.1 part of 3,3-diallyltetrahydrofuran-2-ol, N 2 For protection, 60Co γ-ray irradiation dose is about 50kGy, and the irradiation time is 10 minutes. The grafted membrane is taken out, and the surface of the membrane is cleaned with 2000 parts of methanol, and dried to obtain tetrakis(dimethylamino)titanium purification permeation membrane.

[0029] (2) ...

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Abstract

The invention relates to a refining method of tetrakis(dimethylamido)titanium. Industrial grade tetrakis(dimethylamido)titanium enters a membrane reactor provided with a tetrakis(dimethylamido)titanium purification pemeable membrane at the temperature of 10 to 30 DEG C and the flow velocity of 1 to 5 BV / h; the preliminarily refined tetrakis(dimethylamido)titanium is obtained; then, rectification is performed to obtain high-purity tetrakis(dimethylamido)titanium.

Description

technical field [0001] The invention relates to a method for purifying titanium amido, in particular to a method for refining tetrakis(dimethylamino)titanium. Background technique [0002] The continuous development of the semiconductor manufacturing industry makes it necessary to find high-k and metal gate material precursors suitable for ALD and CVD. For the 32nm technology node, issues such as material volatility, transport mode, and purity become critical. As the amount of information stored and retrieved has increased dramatically, so has the need for higher-K materials, which can be found in any available element from alumina to rare metals. Proper selection of high-K materials can meet production requirements such as dielectric constant, thermodynamic stability, gate electrode compatibility, and interface layer stability. [0003] Tetrakis(dimethylamino)titanium, molecular formula C 8 h 24 N 4 Ti, which is liquid at room temperature, is a compound that is very se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C211/65B01D67/00B01D71/68B01D61/14
CPCB01D61/145B01D67/0088B01D67/009B01D67/0095B01D71/68B01D2323/385B01D2323/46C07C209/84C07C211/65
Inventor 李军陈刚贺辉龙陈立峰花永紧张雪刚
Owner ZHEJIANG BRITECH CO LTD
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