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Preparation method of oxygen free trialkyl gallium

An oxygen-free trialkylgallium and trialkylgallium technology, which can be used in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. Problems such as low yield, to achieve the effect of easy operation

Inactive Publication Date: 2003-04-16
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method needs to prepare the Grignard reagent and gallium trichloride first, and then allow the two to react. In fact, three-step reactions are required, which obviously has the disadvantage of troublesome operation. In addition, the yield of the reaction is not high. Considering the preparation yield of gallium trichloride, the yield of preparation is also relatively low, as obtained (i-pr) 3 Ga·(NEt 3 ) 0.6 The yield is 27%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: In a reaction flask, add triethylamine (excess) and a mixture of magnesium and gallium, use Schlenk oxygen-free and anhydrous technology to remove the air in the system and fill with nitrogen, under heating (about 40-80 ° C) and stirring , slowly add methyl iodide, after adding, continue to stir and react for 4 hours, evaporate the excess triethylamine under reduced pressure, and obtain the complex of trimethylgallium and triethylamine by vacuum distillation, and the yield is 40% in terms of gallium.

Embodiment 2

[0013] Embodiment 2: in the reaction flask, add N,N-diethylaniline, magnesium gallium mixture, adopt Schlenk oxygen-free anhydrous technology to remove the air in the system and fill with nitrogen, add toluene as solvent, heat (about 40- 80 ° C), stirring, slowly add iodomethane, after adding, continue to stir and react for 6 hours, filter, under normal pressure or reduced pressure, the filtrate is evaporated to remove the solvent and other volatile impurities, and the trimethyl gallium is removed under vacuum. The complex with N,N-diethylaniline was decomplexed to obtain trimethylgallium in a yield of 36% based on gallium.

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PUM

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Abstract

A process for preparing trialkyl gallium without oxygen includes such steps as loading the organic alamine and Ga-Mg mixture in a reactor containing inertial gas, heating, adding halogenoane while stirring up to full reaction, pressure-reduction and removing excessive organic alamine, solvent and volatile substance, normal pressure and pressure-reduction distilling to obtain the mixture of trialkyl gallium and amine, and separating. Its advantages are simple operation and high output rate (more than 30%).

Description

1. Technical field [0001] The invention relates to a preparation method of trialkylgallium used in the field of optoelectronic technology, in particular to a preparation method of oxygen-free trialkylgallium. 2. Background technology [0002] High-purity trialkylgallium is one of the important supporting materials for the epitaxial growth of compound semiconductors by advanced metal organic chemical vapor deposition (MOCVD) technology. It is widely used in the growth of compound semiconductor materials such as GaAs, GaN, AlGaAs, and GaInN. It has important application value in the development and production of optoelectronic devices such as tubes, semiconductor lasers, various band detectors, and solar cells. [0003] The quality and purity of high-purity trialkylgallium are the most important quality indicators of high-purity trialkylgallium sources. The quality and purity of high-purity trialkylgallium directly affect the performance of the compound semiconductor grown. Wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
Inventor 潘毅朱春生徐昕陈化冰虞磊李翔孔令宇孙祥祯
Owner NANJING UNIV
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