Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of pentakis(dimethylamino) tantalum

A technology of dimethylamino and dimethylamine, which is applied in the field of preparation of penta(dimethylamino)tantalum, can solve the problems of high risk of organolithium and unfavorable process industrialization, etc., and achieve good operability, improve activity and The effect of service life and high productivity

Active Publication Date: 2020-01-17
ZHEJIANG BRITECH CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation of penta(dimethylamino)tantalum in the above inventions and the prior art requires the use of organolithium reagents, which are very dangerous, and the use of such substances is not conducive to the industrialization of the process

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of pentakis(dimethylamino) tantalum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of preparation method of penta(dimethylamino)tantalum, its specific scheme is as follows:

[0020] In a dry nitrogen atmosphere, dissolve 9.3kg of butylmagnesium chloride in 100kg of tetrahydrofuran solution, add 0.05kg of cocatalyst, stir and mix evenly, then control the reaction temperature to minus 10°C, and pass dimethylamine gas into the solution to consume 7.8 kg of dimethylamine, complete the reaction to obtain bis(dimethylamino)magnesium; then add 10.5kg of tantalum pentachloride into the reaction kettle, control the temperature at 5°C, and continue the reaction for 10h. After the reaction is completed, filter and remove the After the solvent is distilled off, the crude product of penta(dimethylamino)tantalum can be obtained, and the product of penta(dimethylamino)tantalum can be obtained after purification.

[0021] Its preparation method of described promoter is as follows:

[0022] Take 400Kg of 0.3mol / L potassium iodide solution, add 1Kg of sodium me...

Embodiment 2

[0029] A kind of preparation method of penta(dimethylamino)tantalum, its specific scheme is as follows:

[0030] In a dry nitrogen atmosphere, dissolve 11.8kg of butylmagnesium chloride in 130kg of tetrahydrofuran solution, add 0.25kg of cocatalyst, stir and mix evenly, then control the reaction temperature to minus 20°C, and pass dimethylamine gas into the solution to consume 10.8 kg of dimethylamine, complete the reaction, and obtain bis(dimethylamino)magnesium; then add 14.5kg of tantalum pentachloride into the reaction kettle, control the temperature at 20°C, and continue the reaction for 15 hours. After the reaction is completed, filter and remove the After the solvent is distilled off, the crude product of penta(dimethylamino)tantalum can be obtained, and the product of penta(dimethylamino)tantalum can be obtained after purification.

[0031] Its preparation method of described promoter is as follows:

[0032] Take 300Kg of 0.1mol / L potassium iodide solution, add 0.3Kg ...

Embodiment 3

[0039] A kind of preparation method of penta(dimethylamino)tantalum, its specific scheme is as follows:

[0040]In a dry nitrogen atmosphere, dissolve 14.1kg of butylmagnesium chloride in 150kg of tetrahydrofuran solution, add 0.5kg of cocatalyst, stir and mix evenly, then control the reaction temperature to minus 30°C, and pass dimethylamine gas into the solution to consume 12.8 kg of dimethylamine, complete the reaction to obtain bis(dimethylamino)magnesium; then add 17.5kg of tantalum pentachloride into the reaction kettle, control the temperature at 30°C, and continue the reaction for 20h. After the reaction is completed, filter and remove the After the solvent is distilled off, the crude product of penta(dimethylamino)tantalum can be obtained, and the product of penta(dimethylamino)tantalum can be obtained after purification.

[0041] Described cocatalyst is a kind of nanoscale cuprous iodide particle, and its preparation method is as follows:

[0042] Take 500Kg of 0.5m...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
The average particle sizeaaaaaaaaaa
The average particle sizeaaaaaaaaaa
The average particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention relates to the field of fine chemical engineering, in particular to a preparation method of pentakis(dimethylamino) tantalum. The method comprises the following steps: dissolving butyl magnesium chloride in a tetrahydrofuran solution, adding a cocatalyst, introducing dimethylamine gas to obtain bis (dimethylamino) magnesium, and reacting with tantalum pentachloride to obtain the product. According to the preparation method of pentakis(dimethylamino) tantalum, a Grignard reagent is adopted to participate in nucleophilic reaction, and a dangerous organic lithium reagent is prevented from being used, so that the experimental process is safer, the operability is better, and the industrialization of the process is facilitated; according to the process, nanoscale cuprous iodide particles are adopted as a cocatalyst, so that the reaction is facilitated, the generation of byproducts is reduced, and the yield is relatively high.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a preparation method of pent(dimethylamino)tantalum. Background technique [0002] Penta(dimethylamino)tantalum (PDMAT) is a product that was created in the laboratory a long time ago. In the 2010s, it became a popular precursor for making tan films for barrier / liner applications in integrated circuit fabrication. The process was developed by Applied Materials (AMAT) and is used in Endura metallization process tools. In the copper damascene process, some tan films are used as barrier / liner layers. In some specific applications, PDMAT is used as an electrode in the hkmg process. Almost all IC manufacturing processes (memory and logic chipmakers) use this TaN process to some extent. [0003] 201310235743.2 relates to a system and method for in-situ deposition of barrier and seed layers. The in-situ deposition system proposed by the present invention includes a deposition ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C209/00C07C211/04C07F9/00B01J31/30
CPCC07C209/00C07F9/005B01J31/30B01J35/398B01J35/23C07C211/04
Inventor 陈刚李军毛索源张广第杨建成徐琴琪黄磊徐聪
Owner ZHEJIANG BRITECH CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com