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Preparation method of trimethyl bismuth

A technology of trimethyl bismuth and methyl halide magnesium is applied in the direction of bismuth organic compounds, etc., to achieve the effects of simple preparation process, easy industrial production and high purity

Pending Publication Date: 2021-12-17
广东先导微电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are very few methods for preparing trimethylbismuth, so it is urgent to develop a method for preparing trimethylbismuth with high purity.

Method used

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Examples

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Effect test

preparation example Construction

[0020] The present application discloses a method for preparing trimethylbismuth, which comprises the following steps: step 1, using metal magnesium, methyl halide, and ether as reaction raw materials to synthesize methylmagnesium halide, and storing it in an inert atmosphere for future use; step 2 , to synthesize trimethylbismuth: dissolve and dilute bismuth trihalide with a high boiling point solvent, then add the methylmagnesium halide dropwise in step 1 while stirring; step 3, carry out vacuum distillation with the trimethylbismuth synthesized in step 2, and discard After the first 5% to 10% fraction, collect the crude product of trimethylbismuth; step 4, rectify the crude product of trimethylbismuth collected in step 3, collect the former fraction, and the former fraction is the crude product of trimethylbismuth 25% to 35% of the volume, the middle fraction is collected, the volume of the middle fraction is 50% to 65% of the volume of the crude product of trimethylbismuth,...

Embodiment 1

[0039] Step 1, a. The reagents used are firstly dewatered so that the water content is below 100ppm; b. Washing the metal magnesium chips with dilute nitric acid to remove the oxide film on the surface, washing with absolute ethanol, air-drying under a nitrogen atmosphere, and storing for future use C. add 43.8g metal magnesium and 500mL ether solvent that removes oxide film in the there-necked flask that constant pressure dropping funnel, condensation pipe, thermometer jacket (thermometer) are housed, add 142g methyl iodide in constant pressure dropping funnel 200m of a mixed solution of diethyl ether, turn on the heating and set the temperature to 40°C, start stirring, start to add the mixed solution of methyl iodide and diethyl ether dropwise, after the reaction is triggered, turn off the heating, slowly add the mixed solution of methyl iodide and diethyl ether dropwise, after the dropwise addition, To obtain methylmagnesium iodide, after the reaction is complete, diethylene...

Embodiment 2

[0045] Step 1, a. The reagents used are firstly dewatered so that the water content is below 100ppm; b. Washing the metal magnesium chips with dilute nitric acid to remove the oxide film on the surface, washing with absolute ethanol, air-drying under a nitrogen atmosphere, and storing for future use c. add 24g magnesium metal, 1.2g aluminum trichloride and 250mL diethylene glycol dimethyl ether to remove oxide film in the there-necked flask that constant pressure dropping funnel, condensing pipe, thermometer sleeve pipe (thermometer) are housed, Add a mixed solution of 78g methyl iodide and 110m diethylene glycol dimethyl ether into the constant pressure dropping funnel, turn on the heating and set the temperature to 45°C, start stirring, and start to add the mixed solution of methyl iodide and diethylene glycol dimethyl ether dropwise After the reaction is initiated, the heating can be turned off, and the mixed solution of diethylene glycol dimethyl ether is slowly added dropw...

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Abstract

The invention discloses a preparation method of trimethyl bismuth, which comprises the following steps: 1, synthesizing methyl magnesium halide by taking metal magnesium, halogenated methane and ether as reaction raw materials, and storing the methyl magnesium halide in an inert atmosphere for later use; 2, synthesizing trimethyl bismuth: dissolving and diluting bismuth trihalide with a high-boiling-point solvent, and then dropwise adding the methyl magnesium halide in the step 1 while stirring; 3, carrying out reduced pressure distillation on the trimethyl bismuth synthesized in the step 2, and collecting a crude product of the trimethyl bismuth after the front 5%-10% of fractions are abandoned; and 4, rectifying the trimethyl bismuth crude product collected in the 3, collecting a front fraction which accounts for 25-35% of the volume of the trimethyl bismuth crude product, and collecting a middle fraction which accounts for 50-65% of the volume of the trimethyl bismuth crude product and is high-purity trimethyl bismuth. The preparation method of trimethyl bismuth disclosed by the invention is simple in process and easy to realize industrial production, and the prepared trimethyl bismuth is high in purity.

Description

technical field [0001] The invention relates to the field of preparation of MO sources (high-purity metal organic compounds), in particular to a preparation method of trimethylbismuth. Background technique [0002] Semiconductor manufacturing technology is the cornerstone of the development of the semiconductor industry, which directly determines the quality and performance of semiconductor products. Among them, deposition technology is one of the more commonly used methods in semiconductor manufacturing technology. Deposition technology mainly consists of metal organic compound chemical vapor deposition (MOCVD), physical vapor deposition (PVD), liquid phase growth (LPE), molecular beam orientation growth (MBE), chemical beam orientation growth (CBE), etc. . Among them, the MOCVD method is versatile. Selecting the appropriate MO source compound can decompose the organometallic precursor compound to layer the metal layer at higher temperature, atmospheric pressure or reduce...

Claims

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Application Information

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IPC IPC(8): C07F9/94
CPCC07F9/94
Inventor 曾翼俊黄邹松徐成
Owner 广东先导微电子科技有限公司
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