Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of tris [N, N-bis (trimethylsilyl) amino] yttrium

A trimethylsilyl and amine-based technology is applied in the field of preparation of tris[N,N-bis(trimethylsilyl)amino]yttrium, which can solve the problem that the metal purity of the product cannot reach the ALD process technology and is unfavorable to the industry. Chemical production, removal of by-products, etc., to achieve the effects of cheap reactants, low cost, and fewer side reactions

Inactive Publication Date: 2021-10-26
苏州源展材料科技有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of reaction introduces metal impurities into the reactants, and lithium chloride, a by-product, is produced during the reaction process. It is difficult to completely remove the by-product by general recrystallization methods, resulting in the metal purity of the product not meeting the requirements of the ALD process technology.
The product prepared by the above method needs to be sublimated to further improve the purity, thus resulting in a serious drop in yield and increased cost, which is not conducive to industrial production

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 tris [N, N-bis (trimethylsilyl) amino] yttrium
  • Preparation method of tris [N, N-bis (trimethylsilyl) amino] yttrium
  • Preparation method of tris [N, N-bis (trimethylsilyl) amino] yttrium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a nitrogen atmosphere glove box, add 10.6 g of yttrium trichloride into a 100 mL schleck bottle, stir at 0.13 mbar and 90 °C for 5 hours; inject 40 mL of methyl tert-butyl ether and 8.5 mL of Add triethylamine in turn to the schleck bottle, and stir to obtain a suspension; slowly add 12.1 mL of hexamethyldisilazane dropwise into the suspension, and stir at room temperature for 12 h; after the reaction is complete, add The reaction solution was passed through diatomaceous earth, and washed four to five times with an appropriate amount of n-pentane to obtain a light yellow filtrate; the filtrate was concentrated until a large amount of white precipitate was precipitated, filtered in a glove box, and a small amount of n-pentane refrigerated at -30 °C Wash once or twice; collect the filter residue, add 25 mL of n-hexane to dissolve the filter residue, put the solution at -40 ℃ for 6 h, precipitate solid, filter, repeat this step to dissolve first, then quickly cool down a...

Embodiment 2

[0048] In a nitrogen atmosphere glove box, add 31.2 g of yttrium trichloride into a 250 mL schleck bottle, stir for 5 hours at 0.13 mbar, 90 °C; inject 150 mL of methyl tert-butyl ether and 25.5 mL of Add triethylamine in turn to the schleck bottle, and stir to obtain a suspension; slowly add 36.5 mL of hexamethyldisilazane dropwise into the suspension, and stir at room temperature for 12 h; after the reaction is complete, add The reaction solution was passed through diatomaceous earth, and washed four to five times with an appropriate amount of n-pentane to obtain a light yellow filtrate; the filtrate was concentrated until a large amount of white precipitate was precipitated, filtered in a glove box, and a small amount of n-pentane refrigerated at -30 °C Wash once or twice; collect the filter residue, add 60 mL of n-hexane to dissolve the filter residue, put the solution at -40 ℃ for 6 h, precipitate solid, filter, repeat this step to dissolve first, then quickly cool down an...

Embodiment 3

[0053] In a nitrogen atmosphere glove box, add 10.6 g of yttrium trichloride into a 100 mL schleck bottle, stir at 0.13 mbar and 90 °C for 5 hours; inject 40 mL of methyl tert-butyl ether and 6.5 mL of The tert-butylamine was added to the schleck bottle in turn, and stirred to obtain a suspension; 12.1 mL of hexamethyldisilazane was slowly added dropwise to the suspension, and the reaction was stirred at room temperature for 12 h; after the reaction was complete, the reaction solution was Pass through diatomaceous earth, and wash with an appropriate amount of n-pentane four to five times to obtain a light yellow filtrate; concentrate the filtrate until a large amount of white precipitate precipitates, filter in a glove box, and wash with a small amount of n-pentane refrigerated at -30 °C for one to two times; collect the filter residue, add 20 mL of n-hexane to dissolve the filter residue, put the solution at -40 ℃ for 6 h, precipitate solid, filter, repeat this step, first dis...

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

No PUM Login to View More

Abstract

The invention discloses a preparation method of tris [N, N-bis (trimethylsilyl) amino] yttrium, the preparation method comprises the following steps: (1) mixing anhydrous yttrium trichloride, an organic solvent and organic amine in a protective atmosphere to obtain a suspension; (2) dropwise adding hexamethyldisilazane into the suspension, and reacting under the condition of stirring or heating reflux; and (3) after the reaction is finished, collecting a reaction product to obtain the tri [N, N-bis (trimethylsilyl) amino] yttrium. According to the preparation method, yttrium trichloride and hexamethyldisilazane are promoted to react through a coupling reaction to generate a target product, introduction of metal impurities in reactants is avoided, the subsequent purification difficulty is reduced, the metal purity of the product can reach 5N, the reactants are low in price, the production cost is greatly reduced, and the preparation method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of tris[N,N-bis(trimethylsilyl)amino]yttrium. Background technique [0002] Yttrium oxide film has high thermal stability, plasma resistance and good light projection, and has high dielectric constant, good stability to reducing medium, so it is used in heat-resistant protective film, plasma-resistant film, optical It has a wide range of applications in the manufacture of thin films and microelectronic integrated circuits. At present, the methods for preparing yttrium oxide thin films mainly include the following: sputtering method, ion plating method, coating pyrolysis method, sol-gel method, chemical vapor deposition method and atomic layer deposition method (ALD), among which chemical vapor deposition method And atomic layer deposition method can prepare high-quality yttrium oxide thin film. The preparation of yttrium oxide thin films by ALD re...

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): C07F7/10C23C16/40C23C16/455
CPCC07F7/10C23C16/45525C23C16/405
Inventor 江德圣
Owner 苏州源展材料科技有限公司