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Method for preparing glow discharge mass spectrometer analysis test sample

A technique for glow discharge mass spectrometry and sample analysis, which is used in the preparation of samples for testing, material analysis by electromagnetic means, and material analysis. Accuracy and other issues, to achieve the effect of clean surface, fast analysis speed and high density

Inactive Publication Date: 2015-03-25
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The density of the GDMS sample prepared by this method is low, which affects the stability of the sample analysis results
At the same time, calcining ruthenium powder in a reducing atmosphere may reduce some elements originally present in the powder during the calcination process, thus affecting the accuracy of the analysis results

Method used

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  • Method for preparing glow discharge mass spectrometer analysis test sample
  • Method for preparing glow discharge mass spectrometer analysis test sample
  • Method for preparing glow discharge mass spectrometer analysis test sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Put the ruthenium powder to be analyzed into a graphite mold coated with alumina. The inner diameter of the graphite mold is 30 mm. The ruthenium powder is pressurized and sintered at a temperature of 1300° C. by vacuum hot pressing, and the applied The pressure is 40MPa. After the sintering is completed, the density of the obtained ruthenium block is measured by the Archimedes method, which can reach 99% of the theoretical density of ruthenium. A polycrystalline cubic boron nitride turning tool was used to turn the ruthenium block into a ruthenium sample with a diameter of 28 mm. The ruthenium samples were ultrasonically cleaned with acetone, ethanol and ultrapure water, and dried. Put the sample into the ElementGD block sample stage, and carry out pre-sputtering for a certain period of time, with easily polluted Na, Fe, Ca as the target, start to collect data when the concentration is basically stable, record the time of pre-sputtering, and collect part of ...

Embodiment 2

[0031] Put the ruthenium powder to be analyzed into a graphite mold coated with zirconia. The inner diameter of the graphite mold is 30mm. The ruthenium powder is pressure-sintered at a temperature of 1000°C by spark plasma sintering. The applied pressure is 20MPa. After the sintering is completed, the density of the obtained ruthenium block is measured by the Archimedes method, which can reach 95% of the theoretical density of ruthenium. The ruthenium block was turned into a ruthenium sample with a diameter of 28 mm using a cemented carbide turning tool. The ruthenium samples were ultrasonically cleaned with acetone, ethanol and ultrapure water, and dried. Put the sample into the Element GD block sample stage and perform pre-sputtering for a certain period of time. Taking easily polluted Na, Fe, Ca as the target, start collecting data when its concentration is basically stable, record the time of pre-sputtering, and collect five sets of data of some typical elements at the ...

Embodiment 3

[0033] Put the ruthenium powder to be analyzed into a graphite mold coated with boron nitride. The inner diameter of the graphite mold is 30 mm. The ruthenium powder is pressure sintered at a temperature of 1200 by direct current heating and sintering, and the applied pressure is 30 MPa. . After the sintering is completed, the density of the obtained ruthenium block is measured by the Archimedes method, which can reach 97% of the theoretical density of ruthenium. A diamond turning tool was used to turn the ruthenium block into a ruthenium sample with a diameter of 28 mm. The ruthenium samples were ultrasonically cleaned with acetone, ethanol and ultrapure water, and dried. Put the sample into the Element GD block sample stage and perform pre-sputtering for a certain period of time. Taking easily polluted Na, Fe, Ca as the target, start collecting data when its concentration is basically stable, record the time of pre-sputtering, and collect five sets of data of some typical ...

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Abstract

The invention discloses a method for preparing a glow discharge mass spectrometer analysis test sample. The method comprises the following steps: a) putting refractory metal powder to be analyzed into a graphite mold which is internally coated with a demolding agent; b) forming the powder by using a pressure sintering method; c) milling a formed blank. By using the method disclosed by the invention, the test sample is relatively high in compactness and is clean in surface while the content of impurities in the sample is kept unchanged as much as possible, so that the accuracy and the precision of the glow discharge mass spectrum analysis result are ensured, and meanwhile the test sample prepared by using the method has the advantages of high analysis speed and high efficiency.

Description

technical field [0001] The invention relates to a method for preparing a sample analyzed by a glow discharge mass spectrometer (GDMS). Background technique [0002] In the purity analysis of many high-purity elements or alloys, a glow discharge mass spectrometer (GDMS) is required. Glow discharge mass spectrometer is an instrument that can directly analyze impurities in solid-state conductive samples. The principle is that the glow discharge ion source uses inert gas (usually argon) to produce ions at a voltage of thousands of volts to hit the surface of the sample. Sputtering occurs, and the sample atoms produced by sputtering diffuse into the plasma for further ionization, and then are collected and detected by a mass spectrometer. At present, the glow discharge mass spectrometer that is mainly produced and sold in the world is the Element GD glow discharge mass spectrometer produced by Thermo Electron Company of the United States. This kind of equipment can detect and qu...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N27/68
Inventor 王传军李艳琼谭志龙张俊敏闻明毕珺沈月管伟明
Owner KUNMING INST OF PRECIOUS METALS
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