Preparation method of ultra-high purity aluminum sample for GDMS detection and impurity analysis method of ultra-high purity aluminum sample

A pure aluminum and sample technology, applied in the field of high-purity metal composition analysis, can solve the problems of long stable time of element detection values, unstable detection results, accumulation of surface impurities, etc. The effect of simple sample preparation method

Inactive Publication Date: 2018-03-27
KONFOONG MATERIALS INTERNATIONAL CO LTD
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Problems solved by technology

For samples with low purity, the existing methods can meet the detection requirements, but for ultra-high-purity aluminum samples used for sputtering targets, the existing methods have their limitations: mainly due to the presence of Na and Si in the sample preparation process. Easy to introduce (Na is mainly introduced from the surrounding environment, such as sweat stains on hands, and Si is mainly introduced due to the high content of Si in the air), the amount of introduction is easily higher than the content of the element in the sam

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  • Preparation method of ultra-high purity aluminum sample for GDMS detection and impurity analysis method of ultra-high purity aluminum sample
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  • Preparation method of ultra-high purity aluminum sample for GDMS detection and impurity analysis method of ultra-high purity aluminum sample

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preparation example Construction

[0033] According to a first aspect of the present invention, a method for preparing an ultra-high-purity aluminum sample for GDMS detection is provided, comprising the following steps:

[0034] Ultrasonic pickling is carried out on the ultra-high-purity aluminum sample to be tested with pickling solution. The pickling solution is mainly composed of nitric acid, hydrofluoric acid and water. The volume ratio of nitric acid, hydrofluoric acid and water is 1:(2~5) : (5~8).

[0035] GDMS is the abbreviation of glow discharge mass spectrometry (glow discharge mass spectrometry), which is an analytical method that uses a glow discharge source as an ion source to connect with a mass spectrometer for mass spectrometry.

[0036] figure 1 A schematic diagram of the assay setup for GDMS samples, such as figure 1 As shown, GDMS is mainly composed of an ion source, a mass analyzer and a detection system. During detection, the measured sheet sample 1 with a flat surface is used as the cath...

Embodiment 1

[0079] A preparation method for an ultra-high-purity aluminum sample detected by GDMS, comprising the following steps:

[0080] (a) Surface treatment of the ultra-high-purity aluminum sample to be tested is carried out by turning or mechanical grinding to make the testing surface smooth;

[0081](b) Ultrasonic pickling is carried out on the surface-treated ultra-high-purity aluminum sample with pickling solution. The ultrasonic pickling time is 6 minutes, the ultrasonic pickling temperature is 20°C, and the ultrasonic power is 150W. Fluoric acid and water are mixed, and the volume ratio of nitric acid, hydrofluoric acid and water is 1:2:8;

[0082] (c) The ultra-high-purity aluminum samples after ultrasonic pickling were first washed with distilled water for 3 times and then with ethanol for 3 times, and then put into a drying oven and dried at 25°C for 30 minutes for later use.

Embodiment 2

[0084] A preparation method for an ultra-high-purity aluminum sample detected by GDMS, comprising the following steps:

[0085] (a) Surface treatment of the ultra-high-purity aluminum sample to be tested is carried out by turning or mechanical grinding to make the testing surface smooth;

[0086] (b) Ultrasonic pickling is carried out on the surface-treated ultra-high-purity aluminum sample with pickling solution. The ultrasonic pickling time is 3 minutes, the ultrasonic pickling temperature is 30°C, and the ultrasonic power is 150W. Fluoric acid and water are mixed, and the volume ratio of nitric acid, hydrofluoric acid and water is 1:3:8;

[0087] (c) The ultra-high-purity aluminum sample after ultrasonic pickling was washed 5 times with distilled water and then 5 times with ethanol, and then put into a drying oven and dried at 15°C for 45 minutes for later use.

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Abstract

The invention discloses a preparation method of an ultra-high purity aluminum sample for GDMS detection and an impurity analysis method of the ultra-high purity aluminum sample, relating to the technical field of analysis of high-purity metal components. The preparation method comprises the step of carrying out ultrasonic acid pickling on a to-be-tested ultra-high purity aluminum sample, wherein acid pickling liquid is mainly prepared by mixing nitric acid, hydrofluoric acid and water in a volume ratio of 1 to (2-5) to (5-8). According to the preparation method, the problems that existing methods are not suitable for ultra-high purity aluminum samples, Na and Si are easily introduced in a sample preparation process, and then the detection is slightly high or the stabilization time of an element detection value is long are alleviated. By utilizing a sample preparation method disclosed by the invention, the problem that Na and Si in the ultra-high purity aluminum sample are easily introduced can be effectively alleviated, meanwhile, impurities can be effectively removed, the formation of an oxidation layer on the surface is effectively inhibited, the GDMS detection time is effectively shortened, and the accuracy, stability and repeatability of detection are guaranteed.

Description

technical field [0001] The invention relates to the technical field of high-purity metal component analysis, in particular to a method for preparing an ultra-high-purity aluminum sample used for GDMS detection and an impurity analysis method for an ultra-high-purity aluminum sample. Background technique [0002] Ultra-high-purity aluminum refers to aluminum with a purity of 99.999% (5N) and above. Ultra-high-purity aluminum is mainly used to make sputtering targets, and then used for semiconductor coating. Due to the advantages of low resistivity, easy deposition, easy etching, and mature technology, the aluminum-coated thin film has become a popular choice for integrated circuits, discrete devices, and liquid crystals. Display key materials in other fields. The purity and impurity content of ultra-high-purity aluminum directly affect the performance of aluminum thin films, thereby affecting the performance of related semiconductor components. [0003] GDMS (Glow Discharge...

Claims

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Application Information

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IPC IPC(8): G01N1/34G01N1/32G01N1/28
CPCG01N1/28G01N1/32G01N1/34
Inventor 姚力军潘杰王学泽陈胜洁
Owner KONFOONG MATERIALS INTERNATIONAL CO LTD
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