Analysis method and apparatus of ultra pure arsine

Abstract

The invention relates to an analysis method and an apparatus of ultra pure arsine. The analysis method comprises following steps: firstly, sampling, wherein negative pressure sample injection and static analysis are adopted, the pressure of a quantitative tube is reduced to 1X10<-4> to 1X10<-7>Pa using a molecular pump assembly, oxygen nitrogen base pressure and nitrogen base pressure are reduced to less than 10ppb accompanied with helium sweeping and negative pressure replacement, and then the quantitative tube is filled with ultra pure arsine until gage pressure reaches zero for sample injection analysis; separating of trace impurities, wherein obtained sampled samples to be tested are delivered into a separation system, which is treated via antiseptic treatment and anti-adsorption treatment, by a carrier gas with a flowing speed of 20 to 50mL / min for trace impurity separation; and at last, detecting, wherein the samples to be tested, which are treated via trace impurity separation, are delivered into a detector so as to obtain analysis results. According to the analysis method and the apparatus, the trace impurities in ultra pure arsine can be separated, and a direct current discharge helium ionization detector (DID) is used for analyzing impurity gases; the analysis method and the apparatus are safe and stable; equilibrium analysis values can be obtained in a short time; quantification is accurate; detection limit is low; and analysis period is short.

Description

technical field [0001] The invention relates to an analysis method of ultra-pure arsine and a device thereof. Background technique [0002] Arsane is used in "N" type doping of epitaxial silicon in the semiconductor industry, "N" type diffusion in silicon, ion implantation, growth of gallium arsenide (GaAs), gallium arsenide phosphide (GaAsP) and group III / V elements formed compound semiconductors. In addition, arsine is also used as standard gas, calibration gas and standard mixed gas. Therefore, it is of great significance to actively carry out the research and development of ultra-pure arsine gas to promote the development of the electronic industry and other related technologies. At the same time, the development of ultra-pure arsine detection technology also brings higher requirements. [0003] The DC discharge helium ionization detector (DID) is a non-selective and highly versatile detector. It has a very sensitive response to any gas except the carrier gas He, and ...

AI Technical Summary

Problems solved by technology

The disadvantages of the above method are: 1) Dual detectors and dual gas paths, which easily lead to unfavorable factors such as complex analysis scheme, large dead volume, and long analysis cycle, and are no longer suitable for trace analysis of high-purity electronic gases and the development trend of modern chromatography

2) Hydrogen flame ionization detector (FID) is analyzing CO, CO 2 It needs to be converted to methane before detection, because there are problems with conversion rate and conversion mechanism, which will bring secondary errors

3) The complex gas path cannot realize the full analysis of one injection, prolong the analysis cycle and reduce the analysis efficiency

4) Positive pressure or normal pressure sampling and dynamic analysis are used in the analysis. The disadvantage is that it must be accompanied by positive pressure replacement and purging to achieve accurate quantification, and the resulting problems are leakage and tail gas treatment. From the perspective of safety point of view is unreasonable

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