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Synthetic method of tetra(dimethylamino)hafnium

A synthesis method, dimethylamine-based technology, applied in the field of synthesis of metal-organic complexes, can solve the problems of small lithium chloride salt particles, difficulty in separating lithium chloride salt, and difficulty in filtration, so as to simplify operations, reduce costs, Handle simple effects

Inactive Publication Date: 2012-04-18
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the generated lithium chloride salt particles are very small, and it is very difficult to filter, which brings great trouble to the operation.
Although there are relevant literature reports, it is not necessary to filter to remove lithium salts, but to leave the reaction mixture to stand, and after the precipitation settles down, directly take the supernatant liquid. Large amount of solvent and very time consuming
And in the known method, tetrahydrofuran is mostly used as an auxiliary solvent, which also makes it more difficult to separate the lithium chloride salt

Method used

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  • Synthetic method of tetra(dimethylamino)hafnium

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Embodiment 1

[0027] Embodiment 1: the synthesis of tetrakis (dimethylamino) hafnium

[0028] (1) Under an argon atmosphere, add 108 g of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked bottle, stir mechanically, and place the reaction bottle between -40 and -80 °C. Add 800 mL of 2.5 mol / L n-butyllithium solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 10 hours.

[0029] (2) Add 160 grams of hafnium tetrachloride in batches to the above reaction system, keeping the temperature of the reaction system not higher than 60°C. After adding the hafnium tetrachloride, let the reaction system react for 24-30 hours under the condition of mechanical stirring and inert gas protection.

[0030] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under an atmospheric pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure...

Embodiment 2

[0032] The synthesis method of tetrakis (dimethylamino) hafnium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked bottle and stir evenly, and place the reaction bottle at -40 °C , according to the molar ratio of dimethylamine:n-butyllithium of 1.1:1, the n-butyllithium solution added dropwise to the reaction flask, stirred and reacted for 10 hours after the dropwise addition; according to hafnium tetrachloride:n-butyllithium The molar ratio is 1:4.1, add hafnium tetrachloride to the above reaction system, keep the temperature of the reaction system at 20°C, after adding hafnium tetrachloride, let the reaction system stir and react under the protection of inert gas 24 hours; after the reaction, remove the reaction solvent under an atmospheric pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction at 80-85 °C / 2-5 mmHg, which is tetradimethyla...

Embodiment 3

[0034] The synthesis method of tetrakis (dimethylamino) hafnium, the steps are: under argon atmosphere, add 108 grams of dimethylamine and 200 mL of n-hexane into a 2000 mL three-necked bottle, stir evenly, and place the reaction bottle at -80 ℃, according to the molar ratio of dimethylamine:n-butyllithium of 1.2:1, add n-butyllithium solution dropwise to the reaction bottle, and stir for 10 hours after the addition; according to hafnium tetrachloride: n-butyl The molar ratio of lithium is 1:4.2, add hafnium tetrachloride to the above reaction system, keep the temperature of the reaction system at 60°C, after adding hafnium tetrachloride, let the reaction system stir under the protection of inert gas Reaction for 30 hours; after the reaction, remove the reaction solvent under an atmospheric pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, collect the fraction at 80-85°C / 2-5 mmHg, which is tetradimethylamino hafnium compound. Th...

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Abstract

The invention relates to a synthetic method of tetra(dimethylamino)hafnium, which comprises the following steps: in an argon atmosphere, adding dimethylamine and n-hexane into a three-necked bottle, evenly mixing, putting the reaction bottle at -40--80 DEG C, dropwisely adding an n-butyllithium solution into the reaction bottle, and mixing to react for 10 hours; adding hafnium tetrachloride into the reaction system, keeping the temperature of the reaction system at 20-60 DEG C, and after finishing adding the hafnium tetrachloride, mixing the reaction system under inert gas shielding to react for 24-30 hours; after the reaction finishes, removing the reaction solvent in one atmosphere; and after all the solvent n-hexane is removed, carrying out reduced pressure distillation to collect 80-85 DEG C / 2-5mmHg fraction which is the tetra(dimethylamino)hafnium compound. The dimethylamine, butyllithium and zirconium tetrachloride which are simple and accessible are used as the reaction raw materials; and thus, the invention is simple to operate and lowers the cost.

Description

[0001] technical field [0002] The invention relates to a method for synthesizing a metal-organic complex, in particular to a method for synthesizing metal hafnium coordinated by an amine compound. [0003] Background technique [0004] With the further improvement of IC (integrated circuits) integration, the size of the device continues to decrease. When the thickness of the gate dielectric is less than 2nm, the transconductance decreases with the thickness of the gate dielectric, and the ultra-thin gate oxide is due to and The thinning of the interface barrier of silicon will cause the phenomenon of direct tunneling of electrons, so a new gate dielectric with high dielectric constant is used to replace the traditional SiO 2 The gate dielectric has increasingly become one of the research hotspots at home and abroad, because the high-K gate dielectric can have a thicker physical thickness under the premise of ensuring a certain capacitance, so that the above-mentioned unfa...

Claims

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Application Information

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IPC IPC(8): C07F7/00
Inventor 潘毅孔令宇韩建林虞磊
Owner NANJING UNIV
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