Method for synthesizing hafnium tetra-tert-butoxide

A technology of hafnium tetra-tert-butoxide and a synthesis method is applied in the synthesis field of metal-organic complexes to achieve the effects of reducing toxicity, reducing costs and reducing losses

Inactive Publication Date: 2012-02-15
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Technical problem to be solved: the present invention mainly aims at the deficiency of the synthesis method of hafnium tetra-tert-butoxide in the prior art, and provides a novel synthesis method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1: Synthesis of tetra-tert-butoxy hafnium

[0027] (1) In a nitrogen atmosphere, add 49.2 g of potassium tert-butoxide and 200 mL of n-hexane into a 500 mL three-necked flask, and stir mechanically.

[0028] (2) Add 32 grams of hafnium tetrachloride in batches to the above reaction system, keeping the temperature of the reaction system not higher than 60°C. After the addition of hafnium tetrachloride, the temperature of the reaction system is maintained at 40-65°C, and the reaction is carried out for 6-10 hours under the protection of inert gas under mechanical stirring.

[0029] (3) Then remove the reaction solvent under normal pressure, and after the solvent n-hexane is completely removed, vacuum distillation, collect the 90-92 ℃ / 5 mmHg fraction, which is the tetra-tert-butoxy hafnium compound. The yield is 80-93%. The product has passed the identification of hydrogen nuclear magnetic spectrum. 1 H NMR (300 MHz, CDCl 3 ): 1.38 (s, 36H).

Embodiment 2

[0031] The synthesis method of tetra-tert-butoxy hafnium, the steps are:

[0032] (1) In a nitrogen atmosphere, add 49.2 g of potassium tert-butoxide and 200 mL of n-hexane into a 500 mL three-necked flask, and stir well;

[0033] (2) Add hafnium tetrachloride with a molar ratio of hafnium tetrachloride:potassium tert-butoxide of 1:4.4 to the above reaction system, keeping the temperature of the reaction system at 20°C; after adding hafnium tetrachloride, Keep the temperature of the reaction system at 40°C and stir and react for 10 hours under inert gas protection;

[0034] (3) Then remove the solvent of the reaction under one atmosphere pressure, and after the solvent n-hexane is completely removed, distill under reduced pressure to collect the 90-92 ℃ / 5 mmHg fraction, which is the tetra-tert-butoxy hafnium compound. The product has passed the identification of hydrogen nuclear magnetic spectrum. 1 H NMR (300 MHz, CDCl 3 ): 1.38 (s, 36H).

Embodiment 3

[0036] The synthesis method of tetra-tert-butoxy hafnium, the steps are:

[0037] (1) In a nitrogen atmosphere, add 49.2 g of potassium tert-butoxide and 200 mL of n-hexane into a 500 mL three-necked flask, and stir well;

[0038] (2) Add hafnium tetrachloride with a molar ratio of hafnium tetrachloride:potassium tert-butoxide of 1:4.8 into the above reaction system, keeping the temperature of the reaction system at 60°C; after adding hafnium tetrachloride, Keep the temperature of the reaction system at 65°C and stir and react for 6 hours under inert gas protection;

[0039] (3) Then remove the reaction solvent under one atmosphere pressure, and after the solvent n-hexane is completely removed, distill under reduced pressure to collect the 90-92℃ / 5 mmHg fraction, which is the tetra-tert-butoxy hafnium compound. The product has passed the identification of hydrogen nuclear magnetic spectrum. 1 H NMR (300 MHz, CDCl 3 ): 1.38 (s, 36H).

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PUM

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Abstract

The invention relates to a method for synthesizing hafnium tetra-tert-butoxide, which comprises the following steps of: adding potassium tert-butoxide and n-hexane into a three-necked bottle in nitrogen atmosphere, and uniformly stirring; adding hafnium tetrachloride into a reaction system in a molar ratio of the hafnium tetrachloride to the potassium tert-butoxide of 1:4.4-1:4.8, and keeping the temperature of the reaction system to be between 20 and 60 DEG C; keeping the temperature of the reaction system to be between 40 and 65 DEG C after the hafnium tetrachloride is completely added, and reacting for 6 to 10 hours with stirring under the protection of inert gas; removing a reacted solvent under one atmospheric pressure, distilling under reduced pressure after the solvent n-hexane is completely removed, and collecting 90 to 92 DEG C/5mmHg fractions, namely a hafnium tetra-tert-butoxide compound. Simple and readily available raw materials, namely the potassium tert-butoxide and the hafnium tetrachloride are reacted, the method is easy to operate, and cost is reduced.

Description

[0001] technical field [0002] The invention relates to a method for synthesizing metal-organic complexes in the field of chemistry, in particular to a method for synthesizing hafnium tetra-tert-butoxide. [0003] Background technique [0004] With the advancement of technology, the size of CMOS transistors is getting smaller and smaller, and the integration level is getting higher and higher. The current lithography scale has reached 45nm, and the equivalent oxide thickness of CMOS gate has dropped below 1nm, and the thickness of the gate oxide layer is close to the atomic distance. The reduction of equivalent oxide thickness will cause tunneling effect and large channel leakage current It will lead to high power consumption of the chip and corresponding heat dissipation problems, which will adversely affect the integration, reliability and life of the device. Therefore, it is urgent to develop a new high-k dielectric material to replace the traditional SiO 2 . [0005]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00
Inventor 韩建林潘毅孔令宇曹季
Owner NANJING UNIV
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