Direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3

A technology of DC glow discharge and impurity elements, which is applied in the direction of measuring devices, material analysis through electromagnetic means, instruments, etc., to achieve the effect of simplifying the steps of sample pretreatment

Inactive Publication Date: 2015-01-21
GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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Problems solved by technology

The dc-GDMS method is used to determine α-Al 2 o 3 The content of impurity elements in the powder has not been reported in China

Method used

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  • Direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3
  • Direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3
  • Direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3

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Embodiment

[0025] α-Al 2 o 3 The powder and copper powder (the content of each element to be tested is not higher than 0.1 μg / g) are mixed evenly at a ratio of 1:2, and the appropriate powder is selected by using a DY-60 electric powder tablet press (Tianjin Keqi High-tech Co., Ltd.). Pressure The mixed powder is pressed into tablets, the mold is selected as Φ=20mm, and six tablet samples are prepared in parallel. use N 2 Blow off the powder on the surface of the tableted sample and put it into the sample cell. Element GD glow discharge mass spectrometer (Thermo Fisher, USA) was used to adjust parameters such as discharge current and discharge gas flow rate, as shown in Table 1, and pre-sputter for 15 minutes to remove contamination on the surface of the tablet. Then measure with the measurement parameters in Table 1, collect the signals of the elements to be measured and the matrix elements Al, O and Cu, the instrument automatically gives the content of the elements to be measured in...

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Abstract

A direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3 comprises the following steps: (1) evenly mixing Al2O3 powder and copper powder according to the proportion, then tabletting the mixed powder, blowing away the powder on the surface of the sample with N2, and filling the sample into a sample pool; (2) setting the flow of discharge gas at 500 mL / min, discharge current of 30 mA and ion source cooling temperature at 5-25 DEG C, and pre-sputtering for 15 min; (3) acquiring the signal intensity of the element to be measured under the experimental conditions set in step (2), defining the total sum of signal intensity generated by Al, O and Cu as 100%, and calculating the element content to be measured in the mixed powder according to the ratio of the signal intensity of the element to be measured to the total signal intensity of the three elements Al, O and Cu; and deducting the content of the element to be measured in the copper powder to obtain the content of the element to be measured in Al2O3. The invention realizes the determination of the content of impurity elements in non-conductive alpha-Al2O3 powder by the direct current glow discharge mass-spectrometry method, and the determination results are basically consistent with those of the DC arc emission spectroscopy method.

Description

technical field [0001] The invention relates to a method for measuring high-purity α-Al by DC glow discharge mass spectrometry 2 o 3 The method of impurity elements. Background technique [0002] High-purity alumina is an important material for making transparent ceramic materials and single crystal materials, and its purity directly affects the microstructure and performance of the product. α-Al 2 o 3 (α-Al 2 o 3 ) belongs to one of the insoluble inorganic materials, and is insoluble in acid and alkali under normal temperature and pressure. The insolubility of such samples brings difficulties to detection. The conventional sample dissolution method adopts the sodium carbonate / borax alkali fusion method, but this method is easy to introduce a large amount of reagent blanks and salts, which is not conducive to instrument determination; microwave digestion technology is a new type of sample dissolution technology, which requires a small amount of reagents. However, ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68
Inventor 胡芳菲王长华李继东
Owner GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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