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Method of manufacturing analysis specimen

A sample and powder technology, which is applied in the field of production of analytical samples, can solve the problems of contamination of analytical samples, difficulty in grinding, and difficulty in removing the surface of samples, and achieve the effect of inhibiting oxidation

Inactive Publication Date: 2007-10-03
JX NIPPON MINING & METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The metal mold when molding the powder sample is made of tool steel and superhard alloy with iron as the main component. However, because ruthenium is very hard, when the powder is molded, the metal mold and the ruthenium powder are rubbed, and the wear powder of the metal mold Problems leading to contamination of analytical samples
[0009] Because the contamination caused by abrasive powder remains on the surface, it can be removed by mechanical grinding. However, because the powder compact and sintered body are porous, the abrasive powder remains in the sample, and there is a problem due to the hardness of ruthenium. Problems that are difficult to grind due to its brittleness
In addition, the wear powder of the metal mold is mainly composed of iron, but iron and ruthenium are both Group 8 elements in the periodic table of elements, and have high mutual affinity. If sintered, the iron on the surface is easy to diffuse and penetrate into the interior of the sample. , so it is also difficult to remove the surface of the sample by discharge with a glow discharge mass spectrometer
Therefore, it is difficult to determine whether it is the cause of surface contamination by contamination from the metal mold

Method used

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  • Method of manufacturing analysis specimen

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Embodiment 1

[0030] Examples of the present invention are described below. Example 1 will be described with the flowchart shown in FIG. 1 .

[0031] Ruthenium powder is produced by the following method.

[0032] Sodium bromate is added to an aqueous solution of platinum group metals using copper electrolytic precipitates as a raw material to distill ruthenium into volatile ruthenium tetroxide and recover as ruthenium chloride in a 6 mol / L hydrochloric acid solution.

[0033] Add ammonium chloride to 7 liters of the hydrochloric acid solution containing the ruthenium chloride, heat at 90°C for 2 hours and let it cool to room temperature, filter the crystallized ammonium hexachlororuthenium (hexachlororuthenium) with filter paper, put high-purity alumina The obtained container was kept at 600° C. for 2 hours in a nitrogen atmosphere with a tubular furnace, and the first-stage calcination was performed to obtain sponge-like (sponge) crude ruthenium. It is crushed with a mortar to obtain rut...

Embodiment 2

[0039] In Example 2, ruthenium powder was molded with a mold made of yttrium-stabilized zirconia, and a sample was produced in the same manner as in Example 1, except that pure hydrogen was used in the atmosphere during sintering. There was no discoloration on the surface of the analysis sample after sintering. When measured by glow discharge mass spectrometry, zirconium (atomic number 40) and yttrium (atomic number 39) were less than 1 mass ppm, so that the analytical values ​​substantially the same as in Example 1 were obtained. (refer to Table 2)

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Abstract

A method for preparing a sample for analyzing high-purity ruthenium powder by glow discharge mass spectrometry (GDMS) is provided. In this method, in the process of analyzing the grade of ruthenium powder using a glow discharge mass spectrometer, the material is yttrium-stabilized zirconia. The analysis sample of ruthenium powder.

Description

technical field [0001] The invention relates to a preparation method of a sample for analyzing ruthenium (ruthenium) powder by glow discharge mass spectrometry (GDMS). Background technique [0002] High-purity ruthenium powder is used for targets used in the manufacture of semiconductors and hard disks, and as a raw material for ruthenium paste for resistors. Therefore, it is necessary to analyze trace impurities contained in ruthenium. The analysis methods of high-purity metals can be roughly divided into wet analysis methods and dry analysis methods. [0003] First, as the analysis method by the former wet analysis method, the aqueous solution in which the metal is decomposed is quantitatively analyzed by inductively coupled plasma emission spectrometry (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS). Methods. However, ruthenium is difficult to be attacked by all acids to the extent that it slowly dissolves in oxidizing acids or aqua regia. Therefore...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 永井灯文上村宪一庵下高宏
Owner JX NIPPON MINING & METALS CO LTD
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