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Synthesis and purification method of electronic grade arsines

A purification method and electronic-grade technology, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve the problems of low adsorption efficiency, difficulty in obtaining heavy metals, high system cost, etc., and achieve high adsorption rate

Active Publication Date: 2014-07-30
HEFEI ZHENGFAN ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are also published arsine purification methods in China, which mainly use gallium-indium alloy liquid deep adsorption dehydration and oxygen to obtain electronic grade arsine. This adsorption method is not renewable, and heavy metals are difficult to obtain, resulting in high cost of the entire system. Promotion Will be limited, on the other hand, these heavy metal alloys are inherently toxic, and the adsorption efficiency of deep adsorption is low

Method used

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  • Synthesis and purification method of electronic grade arsines

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Embodiment

[0032] As shown in Figure 1, it is a flowchart of the synthesis and purification method of a kind of electronic grade arsine provided by the present invention, and the specific steps are as follows:

[0033] Step S1: Weigh 3.46g of zinc arsenide powder 2 into the reactor 1, seal it and evacuate it, slowly add 9.2ml of dilute sulfuric acid with a mass concentration of 30% from the feed port 3 until no bubbles are generated in the solution, Whole reaction is carried out under vacuum state;

[0034] Step S2: the crude arsine gas generated in step S1 passes through the condenser 4, and the condensation temperature is -30°C, so that the liquid droplets in the gas are separated;

[0035] Step S3: the crude arsine gas produced in step S2 passes through an adsorption trap 5 equipped with desiccant and carbon dioxide adsorbent to remove most of the water and carbon dioxide, and the desiccant and carbon dioxide adsorbent can be recycled;

[0036] Step S4: Pass the crude arsine obtained...

Embodiment 2

[0043] As shown in Figure 1, it is a flowchart of the synthesis and purification method of a kind of electronic grade arsine provided by the present invention, and the specific steps are as follows:

[0044] Step S1: Weigh 6.23g of zinc arsenide powder 2 into the reactor 1, seal it and evacuate it, and slowly add 6.4ml of dilute sulfuric acid with a mass concentration of 50% from the feed port 3 until no bubbles are generated in the solution. Whole reaction is carried out under vacuum state;

[0045] Step S2: the crude arsine gas generated in step S1 passes through the condenser 4, and the condensation temperature is 0°C, so that the liquid droplets in the gas are separated;

[0046] Step S3: the crude arsine gas produced in step S2 passes through an adsorption trap 5 equipped with desiccant and carbon dioxide adsorbent to remove most of the water and carbon dioxide, and the desiccant and carbon dioxide adsorbent can be recycled;

[0047] Step S4: Pass the crude arsine obtain...

Embodiment 3

[0054] As shown in Figure 1, it is a flowchart of the synthesis and purification method of a kind of electronic grade arsine provided by the present invention, and the specific steps are as follows:

[0055] Step S1: Weigh 4.15g of zinc arsenide powder 2 into the reactor 1, seal it and evacuate it, and slowly add 17.2ml of dilute sulfuric acid with a mass concentration of 10% from the feed port 3 until no bubbles are generated in the solution, Whole reaction is carried out under vacuum state;

[0056] Step S2: the crude arsine gas generated in step S1 passes through the condenser 4, and the condensation temperature is -40°C, so that the liquid droplets in the gas are separated;

[0057] Step S3: the crude arsine gas produced in step S2 passes through an adsorption trap 5 equipped with desiccant and carbon dioxide adsorbent to remove most of the water and carbon dioxide, and the desiccant and carbon dioxide adsorbent can be recycled;

[0058] Step S4: Pass the crude arsine obt...

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Abstract

The invention discloses a synthesis and purification method of electronic grade arsines, wherein zinc arsenide powder is reacted with dilute sulfuric acid to generate coarse arsine gas; the coarse arsine gas passes through a condenser to separate liquid drops in the gas, then passes through an adsorption trap to remove water and carbon dioxides and then is placed into a first liquid nitrogen cold trap to freeze arsines; then arsines are heated and evaporated; chemical adsorption columns are put into arsines to remove impurities containing sulfides, then molecular sieve adsorption columns are put into arsines to remove the impurities containing the water, oxygen and carbon dioxides; at the last, arsine gas is put into a second liquid nitrogen cold trap to freeze arsines and obtain high-purity arsine products. The arsine products prepared by using the synthesis and purification method have the advantages that the purity is 6 N, and the impurity content in the products is less than 0.1 ppm.

Description

technical field [0001] The invention relates to a method for synthesizing and purifying electronic grade arsine. Background technique [0002] Arsane (AsH 3 ) is a very important electron gas, as an n-type dopant, it plays a key role in epitaxy and ion implantation processes. At the same time, arsine is also an important raw material for the synthesis of compound semiconductors gallium arsenide (GaAs) and gallium arsenide phosphide (GaAsP). Compound semiconductors are widely used in the manufacture of light-emitting diodes (LEDs) and high-efficiency solar cells. [0003] Arsane (AsH 3 ) synthesis cannot be achieved by simple elemental reactions and is usually prepared using the hydrolysis of metal arsenides. The yield depends on the nature of the metal elements in the arsenide and which decomposer is used. Usually the yield is between 14%-86%. [0004] The purity of arsane currently used in the electronics industry is around 6N (99.9999%), and it is mainly produced and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G28/00
Inventor 李东升周力汤剑波
Owner HEFEI ZHENGFAN ELECTRONICS MATERIAL
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