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Preparation method of high-purity triethyl gallium

A triethylgallium, high-purity technology, applied in the field of preparation of high-purity triethylgallium, can solve the problems of high viscosity, high risk, difficult operation, etc., and achieve the effect of improving purification effect and simple operation.

Active Publication Date: 2015-07-15
苏州普耀光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the complexing agents are macromolecular high-boiling point liquids with high viscosity. Small-molecular low-boiling point impurities are easily wrapped in macromolecular high-boiling point complexing agents and are not easy to be eliminated. The purity generally only reaches 95.0-99.0 %
On the other hand, in order to ensure the purity of triethylgallium, the existing technology will choose to give up part of triethylgallium and let it be taken out with low boiling point impurities. However, due to the characteristics of triethylgallium itself, this part of the work The risk is greater, it is not easy to operate, and it is more difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Disperse 100g of silica gel powder with a particle size of 400 mesh in an aqueous hydrochloric acid solution with a concentration of 0.1mol / L, stir at 60-70°C for 10-20h, cool to 40°C, add 5g of γ-aminopropyltriethoxysilane and continue stirring 10~20h, then add 10g of tri-n-octylamine, stir for 4~8h, filter to get grafted silica. Put the obtained grafted silica into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, then add n-hexane to wash, and the first chromatographic column can be obtained after washing. Put 100 g of silica gel powder with a particle diameter of 400 mesh into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and the second chromatographic column can be obtained.

Embodiment 2

[0026] in CH 3 CH 2 MgX and GaX 3 (X is I or Br) as a raw material, with diethyl ether as a solvent, after the synthesis reaction, triethylgallium with a purity of 99.0% is obtained through crude extraction. The crude triethylgallium product was subjected to a purification operation including the following steps.

[0027] Step 2.1: Pour the triethylgallium into the second chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out.

[0028] Step 2.2: Pour all the solution collected in step 2.1 into the first chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out; then pour all the collected solution into the first chromatographic column , repeat the aforementioned operation of step 2 3 times;

[0029] Step 2.3: Heat and decompose the first chromatographic column after step 2.2. The heating temperature is 100°C, and...

Embodiment 3

[0032] CH 3 CH 2 X (X is I or Br), gallium and magnesium are used as raw materials, ether is used as a solvent, and triethylgallium with a purity of 99.0% is obtained through crude extraction after the synthesis reaction. The crude triethylgallium product was subjected to a purification operation including the following steps.

[0033] Step 2.1: Pour the triethylgallium into the second chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out.

[0034] Step 2.2: Pour all the solution collected in step 2.1 into the first chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out; then pour all the collected solution into the first chromatographic column , repeat the aforementioned operation of step 2 3 times;

[0035] Step 2.3: Heat and decompose the first chromatographic column after step 2.2. The heating temperature ...

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Abstract

The invention relates to a preparation method of high-purity triethyl gallium, belonging to the technical field of preparation of compounds of Group 3 metals in the periodic table. The preparation method comprises the following steps: (1) preparing a triethyl gallium crude product by using aether as a solvent; and (2) purifying the triethyl gallium crude product obtained in the step (1), wherein a first chromatographic column is utilized to purify the triethyl gallium crude product and adopts grafted silicon dioxide as a stationary phase, and the grafted silicon dioxide is silicon dioxide with tri-n-octyl amine grafted on the surface. The preparation method adopts the two steps of synthesis and separation to obtain the triethyl gallium of which the purity can reach 6N. The purification method combines the solid-liquid separation means to load the specific complexant onto the silicon dioxide; and thus, the method is simple to operate and further enhances the purification effect.

Description

technical field [0001] The invention belongs to the technical field of preparation of group III metal compounds of the periodic table of elements, and more specifically, the invention relates to a preparation method of high-purity triethylgallium. Background technique [0002] High-purity triethylgallium is widely used in the growth of indium gallium phosphide, indium gallium arsenic nitrogen, indium gallium arsenic and other compound semiconductor thin film materials. It is an optoelectronic material grown in metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE) The most important and the most used raw material at present. In order to meet the high-purity and high-precision quality requirements of optoelectronic materials (triethylgallium with insufficient purity will have a great impact on the performance of the chip and will also greatly damage the MOCVD equipment), high-purity triethylgallium is required The purity reaches 99.9999%, otherwise f...

Claims

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Application Information

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IPC IPC(8): C07F5/00
CPCC07F5/00
Inventor 顾宏伟茅嘉原李敏王士峰洪海燕
Owner 苏州普耀光电材料有限公司
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