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Synthetic method of tetra(dimethylamino)zirconium

A technology of dimethylamine group and synthesis method, applied in the field of synthesis of metal organic complexes, can solve the problems of high boiling point, influence on reaction yield, difficult to remove and the like

Inactive Publication Date: 2014-07-09
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that it is easy to generate Li 2 (ether) 2 Zr(NMe 2 ) 6 Complexes, affect the reaction yield
Another method is to use toluene as a solvent, but the disadvantage of this method is that toluene is highly toxic and has a high boiling point, which is difficult to remove in post-processing

Method used

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  • Synthetic method of tetra(dimethylamino)zirconium

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Embodiment 1

[0017] Embodiment 1: the synthesis of four (dimethylamino) zirconium

[0018] (1) Under a nitrogen atmosphere, add 108g of dimethylamine and 300mL of n-hexane into a 2000mL three-necked bottle, stir mechanically, cool the system to -20~-60°C with a liquid nitrogen acetone bath, and then add 840mL (2.5mol / L) The n-butyllithium n-hexane solution was slowly added dropwise to the system, and the dropwise addition was completed within three hours, and the reaction was stirred for 10 hours after the dropwise addition was completed.

[0019] (2) Add 116.6 grams of zirconium tetrachloride to the above reaction system in batches, keep the temperature of the reaction system below 0°C, after the addition, naturally rise to room temperature, and stir for 24-30 hours under the protection of argon.

[0020] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under one atmospheric pressure, wait for the solvent n-hexane...

Embodiment 2

[0022] The synthesis method of tetrakis (dimethylamino) zirconium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 300 mL of n-hexane into a 2000 mL three-necked bottle, stir evenly, place the reaction bottle at -20 ° C, follow Dimethylamine: n-butyllithium is a molar ratio of 1.1:1, drips n-butyllithium solution in the reaction flask, stirs and reacts for 10 hours after the addition is completed; press zirconium tetrachloride: n-butyllithium is 1: In a molar ratio of 4.1, zirconium tetrachloride was added to the above reaction system, and the temperature of the reaction system was kept at -10°C. After adding zirconium tetrachloride, the reaction system was stirred and reacted for 24 hours under the protection of an inert gas; After the reaction is finished, remove the reaction solvent under one atmospheric pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction at 110-112°C / 4mmHg, whic...

Embodiment 3

[0024] The synthesis method of tetrakis (dimethylamino) zirconium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 300 mL of n-hexane into a 2000 mL three-necked bottle, stir evenly, and place the reaction bottle at -60 °C, According to the molar ratio of dimethylamine:n-butyllithium of 1.2:1, add n-butyllithium solution dropwise to the reaction bottle, stir and react for 10 hours after the addition is completed; zirconium tetrachloride: n-butyllithium is 1 : Molar ratio of 4.2, zirconium tetrachloride is added in the above-mentioned system, keep the temperature of reaction system at-20 degrees Celsius, after adding zirconium tetrachloride, allow the reaction system to stir and react for 30 hours under the condition of inert gas protection ; After the reaction, the solvent of the reaction is removed under an atmospheric pressure, which is a compound of zirconium tetradimethylamine. The yield was 80%. The product has passed the identification of NMR s...

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Abstract

The invention relates to a synthetic method of tetra(dimethylamino)zirconium, which comprises the following steps: 1)under argon atmosphere, adding dimethylamine and hexane in a three-necked bottle according to a proportion that 100-300 milliliters n-hexane is added in 100g dimethylamine, uniformly stirring, and placing the reaction bottle between the temperature of -20--60 DEG C, adding a n-butyllithium solution drop by drop in the reaction bottle, stirring after dropping, and reacting for 10 hours; 2)adding zirconium tetrachloride in the above reaction system, keeping the temperature of the reaction system between -20-0 DEG C, after adding zirconium tetrachloride, stirring the reaction system under the protection of inert gas to react for 24-30 hours; and 3)after the reaction is finished, removing a solvent of the reaction under one atmospheric pressure, after solvent n-hexane is completely removed, performing underpressure distillation, and collecting the fraction at 110-112 DEG C / 4mmHg which is the tetra(dimethylamino)zirconium compound. According to the invention, the reaction employs the raw material dimethylamino lithium and hafnium tetrachloride which are simple and easy to obtain, the operation is simple, and the cost is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing metal-organic complexes in the field of chemistry. Background technique [0002] With the further improvement of IC (integrated circuits) integration, the device size is continuously reduced. When the thickness of the gate dielectric is less than 2nm, the drive current of the MOSFET tends to reach saturation, and the transconductance also decreases with the thickness of the gate dielectric. . In addition, the ultra-thin gate oxide also has some inherent scattering mechanisms, such as scattering caused by the roughness of the polysilicon / oxide interface, remote impurity scattering, and interfacial plasmon scattering. Moreover, the ultra-thin gate oxide will cause direct tunneling of electrons due to the thinning of the interface barrier with silicon, so a new gate dielectric with a high dielectric constant is used to replace the traditional SiO 2 Gate dielectric has increasingly become one of the rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/65C07C211/04C07C209/00
Inventor 孔令宇虞磊潘毅陆志进安光辉孙海龙郑军
Owner NANJING UNIV
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