Preparation method of tris(dimethylamino) cyclopentadienyl zirconium

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...

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