GB/T 37211.3-2022Method for chemical analysis of metal germanium—Part 3: Determination of trace impurity elements content—Glow discharge mass spectrometry (English PDF)

Foreword

This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1: Structure and Drafting Rules for Standardization Documents" drafting.

This document is part 3 of GB/T 37211 "Methods for Chemical Analysis of Germanium Metals". GB/T 37211 has issued the following parts.

--- Part 1: Determination of arsenic content Arsenic spot method;

--- Part 2: Determination of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, zinc content by inductively coupled plasma mass spectrometry;

--- Part 3: Determination of trace impurity elements Glow discharge mass spectrometry.

Introduction

Metal germanium has a wide range of uses, and is an important part of traditional materials and even contemporary high-tech new materials. Infrared germanium single crystal, germanium-containing light Fibers, semiconductor germanium sheets and other materials are widely used in communication technology, electronic computers, aerospace development, photosensitive materials, optoelectronic materials, energy materials and other fields area. Germanium has the chemical properties of lithophilic, sulfophilic, ferrophilic, and organophilic, and it is difficult to form independent minerals. It is generally distributed in other elements in a dispersed state.

In the minerals, it becomes the associated component of various metal deposits. GB/T 37211 "Chemical Analysis Methods for Germanium Metal" is a chemical analysis method for germanium metal The series of standards are of great significance for improving the technical capability and process control level of germanium metal production and meeting the needs of domestic and foreign markets.

GB/T 37211 consists of 3 parts.

--- Part 1: Determination of arsenic content Arsenic spot method. The purpose is to establish the determination method of arsenic content in metal germanium.

--- Part 2: Determination of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, zinc content Inductively coupled plasma mass spectrometry. The purpose is To establish the determination method of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, zinc content in metal germanium.

--- Part 3: Determination of trace impurity elements Glow discharge mass spectrometry. The purpose is to establish the trace impurity elements in metal germanium test methods.

With the development of society and technological progress, the high-end applications of germanium are constantly expanding. Determination of impurity elements in metal germanium by glow discharge mass spectrometer The content of germanium has become the daily requirement of the application side. The formulation of this document is very important for the study of the physical and chemical properties of germanium and the control of product quality. To a certain extent, it can strengthen the foundation of product quality, provide technical support for quality upgrading, and have great social benefits.

1 Scope

This document specifies the method for the determination of trace impurity elements in metallic germanium by glow discharge mass spectrometry.

This document is applicable to the determination of trace impurity elements in germanium metal, and the determination range is 0.001mg/kg~2mg/kg.

2 Normative references

The contents of the following documents constitute the essential provisions of this document through normative references in the text. Among them, dated references For documents, only the version corresponding to the date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 14264 Terminology of semiconductor materials

3 Terms and Definitions

The terms and definitions defined in GB/T 14264 apply to this document.

4 Principles of the method

The sample is used as the cathode for glow discharge, and in the argon atmosphere, the surface atoms are sputtered away from the sample and enter the glow discharge plasma.

In the plasma, it is ionized and then introduced into the mass spectrometer. At the isotopic mass of each element with a preset number of scan points and integration time The corresponding peaks were integrated, and the resulting area was the peak intensity. When there is a standard sample, firstly carry out an independent test on the standard sample under the same measurement conditions.

Determine the relative sensitivity factor, and then use the relative sensitivity factor to calculate the mass fraction of each element; when there is no standard sample, the computer The mass fraction of each element is automatically calculated according to the "typical relative sensitivity factor" in the instrument software.

5 Interfering factors

It is necessary to calibrate the working efficiency of the instrument detector before sample testing, otherwise it will cause test errors.

6 Reagents or materials

Unless otherwise specified, only pure water with a resistivity of not less than 18.2 Mohm·cm is used in the analysis, and the reagents used in the test are MOS level.

6.1 Absolute ethanol.

6.2 Mixed acid: the volume ratio of nitric acid (71% by mass fraction) and hydrofluoric acid (49% by mass fraction) is 9:1.

6.3 Blank sample: a high-purity germanium sample with impurity element content lower than that of the tested sample.