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Method for determining trace impurity elements in high purity alumina polycrystalline material

A high-purity alumina and determination method technology, which is applied in the field of determination of trace impurity elements in high-purity alumina polycrystalline materials, can solve problems such as glow discharge interference, difficult to grasp the mixing ratio, and influence on measurement results, and achieve Simplified sample pretreatment steps, easy to stabilize signal stability, simple sample preparation process

Inactive Publication Date: 2019-01-18
XINJIANG JOINWORLD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this sample preparation method has great disadvantages and limitations: ①It is only suitable for the determination of α-type high-purity alumina powder samples, not for the determination of bulk high-purity alumina polycrystalline materials; ②Select high-purity copper powder As the second cathode material, it is impossible to detect the key impurity element copper as a quality control in high-purity alumina products, and the main impurity elements Fe, Si, Na and other elements in high-purity copper powder are also in high-purity alumina products. The main concern is impurity elements, which are likely to have a greater impact on the accuracy of the test results; ③ mixing is difficult to grasp, it is easy to introduce impurities during the sample mixing process, and the moisture and air adsorbed on the surface of the powder sample may cause the sample to be released during the discharge process. Collapse, which will cause great interference to the glow discharge and affect the measurement results
In this method, the surface of a non-conductive sample is coated with a layer of metal indium for GD-MS measurement. Due to the low melting point of high-purity indium, it needs to be carried out at a lower ion source analysis temperature. The sample preparation and testing methods described above are only suitable for VG9000 Type GD-MS (discontinued in 2005, the ion source is cooled by liquid nitrogen), is not suitable for the determination of the Element type GD-MS (ion source is cooled by water) widely used in the world, and has great limitations; The sample preparation process is relatively complicated, and impurities are easily introduced during the melting process using a quartz crucible, which affects the accuracy of the test results

Method used

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  • Method for determining trace impurity elements in high purity alumina polycrystalline material
  • Method for determining trace impurity elements in high purity alumina polycrystalline material
  • Method for determining trace impurity elements in high purity alumina polycrystalline material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Break the sample AP1# of massive high-purity alumina polycrystalline material to be tested, and process it into a particle sample with a diameter of 2-4mm; avoid pollution caused by the operation process during sample processing.

[0042] (2) First corrode the high-purity tantalum sheet with a mixed solution of nitric acid and hydrofluoric acid with a volume ratio of 3:1, then wash it with pure water, wash it with absolute ethanol, and dry it;

[0043] Take a 2.5mm high-purity alumina polycrystalline particle and place it on two cleaned high-purity tantalum sheets (thickness 0.5mm, purity ≥ 99.999%, and Na, Mg, Si, Ca, Ti, V, Cr, Mn , Fe, Ni, Cu, Zn, Ga single impurity element content should not be greater than 0.05μg / g; length × width = 25mm × 25mm); under the pressure of about 2KN, use SYP-30TS manual tablet press (Shanghai Xinnuo instrument) to inlay polycrystalline particles onto the surface of high-purity tantalum sheets.

[0044] Introduce a high-purity tanta...

Embodiment 2

[0056] The specific operation steps are as follows:

[0057] (1) Break AP2# of the massive high-purity alumina polycrystalline material sample to be tested, and process it into a particle sample with a diameter of 2-4mm; during the sample processing process, avoid pollution caused by the operation process.

[0058] (2) First corrode the high-purity tantalum sheet with a mixed solution of nitric acid and hydrofluoric acid with a volume ratio of 3:1, then wash it with pure water, wash it with absolute ethanol, and dry it;

[0059] Take a 3.5mm high-purity alumina polycrystalline particle on two cleaned high-purity tantalum sheets (thickness 8mm, purity ≥ 99.999%, and Na, Mg, Si, Ca, Ti, V, Cr, Mn, Fe , Ni, Cu, Zn, Ga single impurity element content should not be greater than 0.05μg / g, length × width = 25mm × 25mm); under the pressure of about 2KN, use SYP-30TS manual tablet press (Shanghai Xinnuo Instrument) , so that polycrystalline particles are embedded on the surface of hig...

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Abstract

The invention relates to a method for determining trace impurity elements in the high purity alumina polycrystalline material. The invention provides a method for determining trace impurity elements in the high purity alumina polycrystalline material, comprising the following steps of: (1) breaking the block high purity alumina polycrystalline material sample into polycrystalline particles; (2) placing the polycrystalline particles between two high purity enamel sheets, pressing, and mosaicing on the surface of the high purity enamel sheets; (3) putting the high purity enamel sheets into a GD-MS sample holder, and the side with the high purity alumina polycrystalline material is the detection surface; (4) evacuating an ion source, and adjusting a discharge voltage and a discharge currentin a pulse mode; (5) performing a pulsed glow discharge mass spectrometer analysis under the conditions set in step (4), collecting the signal intensity of the element to be tested, and calculating the mass fraction of the impurity to be tested. The determining method avoids the influence of irregularity or surface roughness of the alumina polycrystalline sample on the discharge and the detectionresult, and can be directly used for the determination of impurities of the high purity alumina polycrystalline material.

Description

technical field [0001] The invention specifically relates to a method for determining trace impurity elements in high-purity alumina polycrystalline material. Background technique [0002] With the rapid development of the LED industry, the industry's demand for high-quality sapphire substrates is increasing. As a high-purity alumina polycrystalline material with high temperature resistance and corrosion resistance, sapphire has excellent optical properties, mechanical properties and chemical stability, high strength, high hardness, and erosion resistance. Work is an extremely important basic material for modern industry and optoelectronics industry. However, the purity of high-purity alumina directly affects the microstructure and performance of its products, so the detection and control of impurity elements in high-purity alumina is very important. [0003] Since high-purity alumina is an insoluble compound with a high melting point and a high boiling point, it has poor ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68H01J49/00
CPCG01N27/68H01J49/0031
Inventor 肖丽梅马冰白永冰王秀娟张丽娟
Owner XINJIANG JOINWORLD CO LTD
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