GB/T 40566-2021Granular polysilicon produced by fluidized bed method—Determination of hydrogen—Pulse heating inert gas fusion infrared absorption method (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 of Standardization Documents" Drafting.

1 Scope

This document describes a method for measuring the hydrogen content in granular silicon by pulse heating inert gas fusion infrared absorption method.

This document is applicable to the determination of hydrogen content in granular silicon by the fluidized bed method, and other silicon materials are used as reference.

Note: The measurement range of hydrogen content in this document depends on the range of the hydrogen analyzer used, and the maximum measurement range is 0.00008mg~2.5mg of hydrogen. By quality The measurement range of the hydrogen analyzer indicated by the number (%) varies with the amount of the sample weighed. For example, the mass fraction of the maximum measurement range of 1g sample is 0.000008%~0.25%; The mass fraction of the maximum measuring range of 0.15g sample is 0.00006%~1.66%.

2 Normative references

The content of the following documents constitutes an indispensable clause of this document through normative references in the text. Among them, dated quotations 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 6379.2 Accuracy of measurement methods and results (accuracy and precision) Part 2: Determine the repeatability of standard measurement methods Basic methods of sex and reproducibility

GB/T 8170 Numerical rounding rules and the expression and determination of limit values

GB/T 14264 Terminology of Semiconductor Materials

3 Terms and definitions

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

4 Principle

The sample is placed in a degassed graphite sleeve crucible, heated and melted under an inert atmosphere, and the hydrogen in the sample is released in the form of hydrogen molecules (H2) Put and enter the carrier gas stream, the hydrogen molecules will be converted into water (H2O) after passing through the hot copper oxide with the carrier gas stream, which is detected in a special infrared cell. root According to the change of infrared absorption intensity signal, the hydrogen content is calculated.

5 Disturbing factors

5.1 The main factors that have a greater impact on the test results are the uniformity of the sample, the cleanliness of the sample surface, the purity of the inert gas, the graphite crucible and the The purity of the auxiliary material (high-purity nickel capsule), the accuracy and uncertainty of the calibration sample value, the accuracy of the electronic balance, the operating parameters of the instrument Optimize selection, etc.

5.2 Inert gas (helium or argon) is used as the carrier gas in the test instrument, and its impurities may affect the accuracy of the test results.

Use high-purity inert gas to improve the accuracy of test results.

5.3 The impurity elements of graphite crucible and auxiliary materials may absorb part of the released hydrogen, and the hydrogen content of graphite crucible and auxiliary materials is also […]