New method for analyzing non-conductor material by utilizing glow discharge mass spectrum

A glow discharge mass spectrometry, non-conductor technology, applied in the analysis of materials, material analysis by electromagnetic means, instruments, etc., can solve the problems of unsatisfactory signal-to-noise ratio, poor discharge stability, narrow application range, etc., and achieve good discharge stability and analysis repeatability, easy operation, and ideal signal-to-noise ratio

Active Publication Date: 2011-09-07
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of brand-new method of applying glow discharge mass spectrometry to analyze non-conductor materials, to solve the problems in the prior art of "complicated pretreatment, easy to cause pollution, poor discharge stability, signal-to-noise ratio (S / N ) are unsatisfactory, highly targeted, and narrow in scope of application” and other defects

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  • New method for analyzing non-conductor material by utilizing glow discharge mass spectrum
  • New method for analyzing non-conductor material by utilizing glow discharge mass spectrum
  • New method for analyzing non-conductor material by utilizing glow discharge mass spectrum

Examples

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Embodiment 1

[0037] Under normal pressure, the lead tungstate (PWO) to be analyzed is processed into a small strip sample with a size of 18mm×2mm×2mm; 3 ) and ultrapure water, ultrasonically cleaned in a mixed solution of ultrapure water, then ultrasonically twice in ultrapure water, finally washed with ethanol, and dried; put metal indium into a quartz crucible and heat it to melt, and then keep it warm at 150°C to 155°C ℃; Use polytetrafluoroethylene tweezers or metal nickel tweezers to pick up the sample and put it into a quartz crucible filled with molten indium. After the molten indium forms a continuous smooth metal indium film on the outer layer of the sample (the film thickness is 10 μm, the film area is 2 / 3 of the surface area of ​​the sample), take out the sample, and cool it down; 3 ) and ultrapure water for ultrasonic cleaning, then ultrasonically twice in ultrapure water, finally washed with ethanol, and dried; the sample was put into the dc-GD-MS needle sample cell for analys...

Embodiment 2

[0045] Under normal pressure, the zirconia (ZrO 2 ) processed into small strip samples with a size of 18mm×2mm×2mm; 3 ) and ultrapure water, ultrasonically cleaned in a mixed solution of ultrapure water, then ultrasonically twice in ultrapure water, finally washed with ethanol, and dried; put metal indium into a quartz crucible and heat it to melt, and then keep it warm at 150°C to 155°C ℃; Use polytetrafluoroethylene tweezers or metal nickel tweezers to pick up the sample and put it into a quartz crucible filled with molten indium. After the molten indium forms a continuous smooth metal indium film on the outer layer of the sample (the film thickness is 10 μm, the area is 2 / 3 of the surface area of ​​the sample), take out the sample, and cool it down; 3 ) and ultrapure water, ultrasonically cleaned in ultrapure water twice, and finally washed with ethanol and dried; the sample was put into the dc-GD-MS needle sample cell for analysis, and the discharge voltage was 1.0kV, th...

Embodiment 3

[0053] Under normal pressure, the lanthanum titanate (La 2 Ti 2 o 7 ) processed into small strip samples with a size of 18mm×2mm×2mm; 3 ) and ultrapure water, ultrasonically cleaned in a mixed solution of ultrapure water, then ultrasonically twice in ultrapure water, finally washed with ethanol, and dried; put metal indium into a quartz crucible and heat it to melt, and then keep it warm at 150°C to 155°C ℃; Use polytetrafluoroethylene tweezers or metal nickel tweezers to pick up the sample and put it into a quartz crucible filled with molten indium. After the molten indium forms a continuous smooth metal indium film on the outer layer of the sample (the film thickness is 10 μm, the film area is 2 / 3 of the surface area of ​​the sample), take out the sample, and cool it down; 3 ) and ultrapure water for ultrasonic cleaning, then ultrasonically twice in ultrapure water, finally washed with ethanol, and dried; the sample was put into the dc-GD-MS needle sample cell for analysi...

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Abstract

The invention discloses a method for analyzing a non-conductor material by utilizing a glow discharge mass spectrum, comprising the following concrete steps of: (a), processing the non-conductor material to be analyzed into a strip sample; (b), cleaning and stoving the strip sample; (c), placing metal indium into a silica crucible and heating to a molten state; (d), cladding the surface of the strip sample with a layer of metal indium membrane; (e), cleaning and stoving the strip sample again; and (f), carrying out direct current glow discharge mass spectrum analysis. By utilizing the analysis method provided by the invention, sample grinding and polishing are not needed, the pretreatment is simple and the pollution is avoided; the operation is simple and convenient, the usage amount of the metal indium is greatly decreased and the analysis cost is reduced; the discharge of the sample is similar to that of a conductor sample and is easily stabilized, the stability of a signal is good, the SNR(Signal to Noise Ratio) is ideal, the analysis time is shortened and the analysis efficiency is increased; the method is suitable for the analysis of massive or crystalline materials, the universality is strong and the application range is wide; and the sample has very good discharge stability and analysis repeatability.

Description

technical field [0001] The invention relates to a method for analyzing non-conductor materials by glow discharge mass spectrometry, in particular to a new method for analyzing non-conductor materials by direct current glow discharge mass spectrometry (dc-GD-MS). Background technique [0002] Glow discharge mass spectrometry (GD-MS) is a direct analysis method for solid materials. It is by far the only elemental analysis method with the widest range of analytical elements and sufficient sensitivity. It has been widely used in solid materials (especially Trace element analysis of high-purity metal materials). [0003] When direct current glow discharge mass spectrometry (dc-GD-MS) analyzes a sample, it is required that the sample itself acts as the cathode of the GD source and must have certain conductivity. The vast majority of inorganic non-metallic materials are poor conductors. Experiments have shown that typical high-purity silicon (resistivity about 1.3×10 5 Ωcm), the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68
Inventor 钱荣
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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