Tetrakis(ethylmethylamino)hafnium synthesis method

A synthetic method, ethylamino technology, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as increasing operation difficulty and cost, reducing reaction efficiency, and difficulty in filtration and separation , to achieve the effect of saving reaction cost, simple operation and cost reduction

Inactive Publication Date: 2014-02-26
NANJING UNIV
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  • Abstract
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Problems solved by technology

The basic principles of these two methods are the same, and their common disadvantage is that they all need to add another auxiliary solvent
Toluene is used in the first method, which makes the reaction more toxic, and the reaction needs to be carried out under heating conditions, which increases the operational difficulty and cost of the reaction
In the second method, tetrahydrofuran is used as an auxiliary solvent, which increases the toxicity of the reaction, and it also makes it more difficult to filter and separate lithium chloride salt. At the same time, because of the addition of tetrahydrofuran, there is a certain coordination effect, which makes distillation purification The process of the target product requires higher temperature and lower vacuum, which further increases the cost of the reaction and makes the yield low
At the same time, the reaction takes several days to complete, which greatly reduces the reaction efficiency.

Method used

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  • Tetrakis(ethylmethylamino)hafnium synthesis method

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Embodiment 1

[0024] Embodiment 1: the synthesis of hafnium tetramethylethylamino

[0025] (1) Under an inert atmosphere, add 130 g of methylethylamine and 600 mL of n-hexane into a 2000 mL three-necked flask, stir mechanically, and place the reaction flask at -10°C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 5 hours.

[0026] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding hafnium tetrachloride, let the reaction system react for 18 hours under the condition of mechanical stirring and inert gas protection.

[0027] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction at ...

Embodiment 2

[0028] Embodiment 2: the synthesis of hafnium tetramethylethylamino

[0029] (1) Under an inert atmosphere, add 236 g of methylethylamine and 500 mL of n-hexane into a 2000 mL three-necked bottle, stir mechanically, and place the reaction bottle at -50 °C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 12 hours.

[0030] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding the hafnium tetrachloride, let the reaction system react for 30 hours under the condition of mechanical stirring and inert gas protection.

[0031] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the frac...

Embodiment 3

[0032] Embodiment 3: the synthesis of tetramethylethylamino hafnium

[0033] (1) Under an inert atmosphere, add 177 g of methylethylamine and 700 mL of n-hexane into a 2000 mL three-necked bottle, stir mechanically, and place the reaction bottle at -80 °C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 10 hours.

[0034] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding hafnium tetrachloride, let the reaction system react for 20 hours under the condition of mechanical stirring and inert gas protection.

[0035](3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction ...

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Abstract

The invention relates to a tetrakis(ethylmethylamino)hafnium synthesis method, which comprises the following synthesis steps: (1) under an inert atmosphere, adding methylethylamine and an alkane solvent to a three-necked bottle, carrying out mechanical stirring, placing the reaction bottle into an environment with a temperature of -10 to -80 DEG C, adding a n-hexane solution of n-butyl lithium to the reaction bottle in a dropwise manner, and carrying out a stirring reaction after completing the addition; (2) adding hafnium tetrachloride to the reaction system, maintaining the temperature of the reaction system to not more than 60 DEG C, carrying out a stirring reaction on the reaction system under the protection of the inert gas after completing the addition; and (3) after completing the reaction, removing the reacting solvent under an atmospheric pressure, carrying out vacuum distillation after completely removing the solvent, and collecting the 110-115 DEG C / 4-5 mmHg fraction, wherein the fraction is the tetrakis(ethylmethylamino)hafnium compound. According to the present invention, the reaction adopts the simple and easily available materials such as methylethylamine, butyl lithium and hafnium tetrachloride as the raw materials, the operations are simple, and the cost is reduced.

Description

[0001] technical field [0002] The invention relates to a method for synthesizing a metal organic complex, specifically a method for synthesizing metal hafnium coordinated by an amine-based compound used for a high-k value precursor material. [0003] Background technique [0004] With the continuous development and progress of large-scale integrated circuits, the integration of integrated circuits has been continuously improved, which requires the size of the original device to be continuously reduced to meet its requirements. When the thickness of the gate dielectric is less than 2nm, the transconductance decreases as the thickness of the gate dielectric decreases, and the ultra-thin gate oxide will cause direct tunneling of electrons due to the thinning of the interface barrier with silicon. [0005] Currently, silicon dioxide is the commonly used dielectric despite its relatively low dielectric constant (k~4). Silicon dioxide also has a very good application on the ga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00
Inventor 梅海波韩建林潘毅王晓晨
Owner NANJING UNIV
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