Preparation method of tris(dimethylamino) cyclopentadienyl zirconium

A technology of cyclopentadienyl zirconium and dicyclopentadiene, applied in chemical instruments and methods, organic chemistry, metallocene, etc., can solve the problems of silicon-based gate insulator leakage, impurity diffusion, shrinkage, etc. The effect of reducing environmental pollution, simplifying reaction treatment and saving time and cost

Inactive Publication Date: 2017-09-22
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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Problems solved by technology

However, with the continuous improvement of integrated circuit integration and the continuous reduction of the feature size of MOS devices, the defects of traditional silicon dioxide or silicon nitride as gate insulators are gradually highlighted, especially when the thickness of the gate dielectric layer is less than 2nm , such a silicon-based gate insulator will suffer from leakage and impurity diffusion

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  • Preparation method of tris(dimethylamino) cyclopentadienyl zirconium

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Effect test

Embodiment 1

[0043] (1) Under an inert atmosphere, add 500mL of n-hexane and 500mL of n-butyl lithium in n-hexane solution (2.5mol / L) to a 2L reaction flask, keep the temperature of the system at about -15°C, and feed in dimethylformamide while stirring. Amine (67 g), vented completely, warmed to room temperature and kept stirring for 4 hours.

[0044] (2) The temperature of the reaction liquid kettle in step (1) is lowered to below -10°C, under the protection of an inert gas, zirconium tetrachloride (71g) is added to the above reaction system, after the addition is completed, slowly return to room temperature, It was then heated to reflux for 12 hours.

[0045](3) Lower the temperature of the reaction solution in step (2) to below -10°C, pass the prepared cyclopentadiene monomer (23g) and 28mL toluene solution through a constant pressure dropping funnel under the protection of a mixed inert gas Add dropwise to the reaction solution in step (2), and keep the kettle temperature below -10°C...

Embodiment 2

[0048] (1) Under an inert atmosphere, add 500mL of n-hexane and dimethylamine (67g) to a 2L reaction flask, keep the temperature of the system at about -15°C, and slowly add 500mL of n-butyl lithium dropwise to the reaction flask while stirring The n-hexane solution (2.5mol / L) was added dropwise, and after rising to room temperature, stirring was maintained for 4 hours.

[0049] (2) Lower the temperature of the reaction liquid kettle in step (1) to about -15°C, under the protection of an inert gas, slowly add the n-hexane solution containing zirconium tetrachloride (71g) into the reaction flask dropwise, and the dropwise addition is completed After that, it was slowly returned to room temperature, and then heated to reflux for 12 hours.

[0050] (3) Lower the temperature of the reaction solution in step (2) to below -10°C, pass the prepared cyclopentadiene monomer (23g) and 28mL toluene solution through a constant pressure dropping funnel under the protection of a mixed inert ...

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Abstract

The invention relates to a preparation method of tris(dimethylamino) cyclopentadienyl zirconium. The preparation method comprises the following steps: 1) lithium dimethylamide preparation: adding an n-hexane solution of n-butyllithium in a reactor, and under stirring starting and inert atmosphere protection, introducing dimethylamine gas to prepare lithium dimethylamide; 2) tetrakis(dimethylamino)zirconium preparation: under stirring starting and inert atmosphere protection, adding zirconium tetrachloride in a lithium dimethylamide solution; 3) cyclopentadienyl monomer preparation with dicyclopentadiene: adding dicyclopentadiene in the reactor, and distilling out a cyclopentadienyl monomer under the condition with the temperature higher than 160 DEG C; 4) dropwise adding the cyclopentadienyl monomer in the tetrakis(dimethylamino)zirconium, and carrying out reaction to produce tris(dimethylamino) cyclopentadienyl zirconium; and 5) distilling the tris(dimethylamino)cyclopentadienyl zirconium. According to the preparation method, the tris(dimethylamino)cyclopentadienyl zirconium is synthesized by a one-pot method, the reaction raw materials are simple and available, and reaction operation is simple; and cyclotentadienyl sodium does not need to be synthesized firstly, and separation of an intermediate is not needed.

Description

technical field [0001] The invention relates to a preparation method of tris(dimethylamino)cyclopentadienyl zirconium. Background technique [0002] At present, the rapid development of CMOS integrated circuits has greatly promoted the development of silicon-based microelectronics industry. Nearly 95% of semiconductor devices and 99% of integrated circuits (IC) are made of silicon materials. However, with the continuous improvement of integrated circuit integration and the continuous reduction of the feature size of MOS devices, the defects of traditional silicon dioxide or silicon nitride as gate insulators are gradually highlighted, especially when the thickness of the gate dielectric layer is less than 2nm , Such a silicon-based gate insulator will suffer from leakage and impurity diffusion. Therefore, it is necessary to seek a new gate dielectric layer to replace silicon dioxide. The most intuitive method is to increase the thickness of the gate dielectric layer, but i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00
CPCC07F17/00
Inventor 张晓斌刘志军范广鹏许从应林俊元顾大公邱良德常华
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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