Pre-test treatment method of high-purity indium sample for glow discharge mass spectrometric detection

A technology of glow discharge mass spectrometry and processing method, applied in the field of high-purity metal composition analysis, can solve problems such as result deviation and impurity dissolution, and achieve the effects of improving accuracy, no impurity introduction, and relaxing the requirements of shape and size

Active Publication Date: 2019-12-06
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the soft material of high-purity indium, ordinary grinding or sandpaper treatment will embed silicon, sodium, aluminum and other impurities on the sandpaper into high-purity indium. Using cutting tools such as grinding wheels and saw blades will introduce iron and calcium into the original. The method of pickling after cutting can reduce some impurities introduced during the cutting process, but if the cleaning time is too long, the impurities in the original sample will also be dissolved, causing deviations in the results

Method used

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  • Pre-test treatment method of high-purity indium sample for glow discharge mass spectrometric detection
  • Pre-test treatment method of high-purity indium sample for glow discharge mass spectrometric detection
  • Pre-test treatment method of high-purity indium sample for glow discharge mass spectrometric detection

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: as figure 1 As shown, the pre-measurement method for the high-purity indium sample used for glow discharge mass spectrometry detection, the specific steps are as follows:

[0030] (1) Put 12g of high-purity indium sample 2 whose size is smaller than the sputtering hole 1 and does not meet the test requirements, and place it in a hydrochloric acid solution with a concentration of 6mol / L for ultrasonic corrosion for 15s (attached figure 1 as shown in 3);

[0031] (2) Place the ultrasonically etched sample in step (1) in deionized water for 360s ultrasonic cleaning (attached figure 1 4 in), and the samples after ultrasonic cleaning were blown dry with high-purity nitrogen (attached figure 1 shown in 5);

[0032] (3) Place the dried sample in step (2) between two clean and dust-free acrylic plates, and place the bottom acrylic plate on a horizontal plane;

[0033] (4) Use a clean hammer to hammer the upper acrylic plate from top to bottom above the acrylic...

Embodiment 2

[0035] Embodiment 2: The pre-measurement method of the high-purity indium sample used for glow discharge mass spectrometry detection, the specific steps are as follows:

[0036] (1) Put 7g of the high-purity indium sample 2 to be tested, which is smaller than the sputtering hole 1 and does not meet the test requirements, in a hydrochloric acid solution with a concentration of 3mol / L and ultrasonically corrode it for 85s;

[0037] (2) Place the sample after ultrasonic etching in step (1) into deionized water for ultrasonic cleaning for 170s, and dry the sample after ultrasonic cleaning with high-purity argon;

[0038] (3) Place the dried sample in step (2) between two clean and dust-free polytetrafluoroethylene plates, and place the bottom polytetrafluoroethylene plate on a horizontal plane;

[0039] (4) Use a clean hammer to hammer the upper PTFE plate from top to bottom above the upper PTFE plate of the sample. After the sample is squeezed, a plane will be formed at the botto...

Embodiment 3

[0041] Example 3: (1) Put 5 g of the high-purity indium sample 2 to be tested, which is smaller than the sputtering hole 1 and does not meet the test requirements, in a hydrochloric acid solution with a concentration of 1 mol / L for ultrasonic corrosion for 180 s;

[0042] (2) Place the sample after ultrasonic etching in step (1) into deionized water for ultrasonic cleaning for 30s, and dry the sample after ultrasonic cleaning with high-purity argon and nitrogen;

[0043] (3) Place the dried sample in step (2) between two clean and dust-free non-metal hard plates, the upper non-metal hard plate is an acrylic plate, and the bottom non-metal hard plate is a tempered glass plate , and place the tempered glass plate at the bottom on a horizontal plane;

[0044] (4) Use a clean small hammer to hammer the upper acrylic plate from top to bottom above the upper acrylic plate of the sample. After the sample is squeezed, a plane will be formed at the bottom of the sample. Continue hammerin...

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Abstract

The invention discloses a pre-test treatment method of a high-purity indium sample for glow discharge mass spectrometric detection. According to the method, firstly, the to-be-tested high-purity indium sample is subjected to ultrasonic corrosion, then the corroded sample is subjected to ultrasonic cleaning and blow-drying sequentially, and the blow-dried sample is placed between two non-metallic hard plates; an external force is applied to the upper non-metallic hard plate, so that a plane is generated at the bottom of the sample after the sample is extruded; the external force continues to beapplied to the upper hard plate till the plane at the bottom of the sample is gradually enlarged to a size required by a glow discharge mass spectrometric test, and then application of the external force is stopped; and the flaky sample between the two non-metallic hard plate is taken out, cleaned and blow-dried, and then a to-be-tested sample sheet meeting the test demand is obtained. Compared with a traditional pre-test treatment method, the method is simple, easy to implement, free of impurity introduction and pollution to the sample and low in cost; and through the method, the time of theglow discharge mass spectrometric detection is shortened, the detection speed is increased, and the practical value is high.

Description

technical field [0001] The invention belongs to the field of high-purity metal component analysis, and in particular relates to a pre-testing method for high-purity indium samples used for glow discharge mass spectrometry detection. Background technique [0002] Indium with a purity above 5N is called high-purity indium, which is widely used in the production of semiconductor materials, semiconductor compounds and CuInxGa(1-x)Se because of its excellent physical and chemical properties and mechanical properties 2 Thin film solar cells and other fields. With the rapid development of the semiconductor industry, the requirements for the purity of high-purity indium are getting higher and higher, so it is of great significance to be able to accurately determine the content of impurity elements in it. [0003] Glow discharge mass spectrometry is widely used in the compositional analysis of high-purity metals due to its low detection limit, fast analysis speed, small memory effec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/32G01N1/34G01N1/28G01N27/68
CPCG01N1/286G01N1/32G01N1/34G01N27/68
Inventor 杨斌赵晋阳徐宝强刘大春杨红卫陈秀敏郁青春王飞戴永年杨佳吴鉴李一夫蒋文龙田阳熊恒曲涛
Owner KUNMING UNIV OF SCI & TECH
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