Method for determining iron content in silicon nitride material

A silicon nitride and iron content technology, applied in the field of determination and material analysis, can solve the problems of lack of standard samples and unsatisfactory detection limit, and achieve low detection limit, high sensitivity and good reproducibility

Inactive Publication Date: 2014-05-21
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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Problems solved by technology

According to the characteristics of silicon nitride, DC arc atomic emission spectrometry can be used for analysis, but this method has problems such as no standard sample and too high detection limit to meet the needs of determination.

Method used

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  • Method for determining iron content in silicon nitride material
  • Method for determining iron content in silicon nitride material
  • Method for determining iron content in silicon nitride material

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Embodiment Construction

[0035] The present invention will be further described below in conjunction with specific embodiments.

[0036] The invention uses microwave digestion to process samples, and uses an inductively coupled plasma mass spectrometer to measure Fe content in silicon nitride, and the test experiment of the invention is carried out in a high-purity laboratory. Specific steps are as follows:

[0037] 1. Sample pretreatment

[0038] Weigh 0.10g of silicon nitride, accurate to 0.0001g, into a polytetrafluoroethylene digestion tank, add 2mL of concentrated nitric acid and 1mL of hydrofluoric acid, use microwave digestion for sample pretreatment, and do a blank test with the sample. The temperature control procedure for microwave digestion is as follows:

[0039] In the first step, it takes 10 minutes to raise the temperature to 120°C and keep it for 5-10 minutes;

[0040] In the second step, it takes 5 minutes to raise the temperature to 180°C and keep it for 10min~15min.

[0041] Ste...

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Abstract

The invention relates to a method for determining iron content in a silicon nitride material, wherein microwave digestion is adopted to carry out a sample pretreatment, and an inductively coupled plasma mass spectrometer is adopted to determine iron impurity content in silicon nitride. The method specifically comprises: weighing a silicon nitride sample, adding HNO3 and HF, adopting microwave digestion to treat the silicon nitride sample to obtain a sample solution, adding a Sc internal standard solution, diluting to obtain a solution requiring detection, adopting a random sample to carry out a blank test, adopting single crystal silicon to carry out backing, adding the equivalent Sc internal standard solution to each standard solution to prepare a series of standard solutions of iron, selecting working conditions of an inductively coupled plasma mass spectrometer, analyzing the series of the standard solutions according to the concentration range from the low concentration to the high concentration to obtain an iron working curve, analyzing the blank solution and the silicon nitride solution requiring detection, substituting into the working curve to calculate to obtain the Fe concentration value in the blank solution and the Fe concentration value in the solution requiring detection, and calculating to obtain the mass percentage of the iron in the sample requiring detection. The method has characteristics of high accuracy and good reproducibility.

Description

technical field [0001] The invention relates to a method for measuring iron content in silicon nitride materials, in particular to a method for measuring iron percentage content in silicon nitride by using microwave digestion to treat samples and an inductively coupled plasma mass spectrometer, and belongs to the technical field of material analysis and measurement. Background technique [0002] Silicon nitride is a superhard substance, insoluble, inherently lubricious, and resistant to wear. Impurity elements in silicon nitride have a great influence on its performance. According to the characteristics of silicon nitride, direct current arc atomic emission spectrometry can be used for analysis, but this method has problems such as no standard sample and too high detection limit to meet the needs of determination. Contents of the invention [0003] The purpose of the present invention is to provide a method for measuring the iron content in silicon nitride materials, main...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64G01N1/44
Inventor 墨淑敏张志刚
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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