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X-ray fluorescence melting sample preparation method of aluminum nitride

A technology of fusion sample preparation and aluminum nitride, which is applied to the use of wave/particle radiation for material analysis, measuring devices, instruments, etc., and can solve problems such as difficult molding

Active Publication Date: 2021-09-10
GUIZHOU BRANCH CHINA ALUMINUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the technical problems of difficult melting, opaque and difficult to form in the conventional aluminum nitride XRF melting sample preparation, the present invention provides an X-ray fluorescence melting sample preparation method of aluminum nitride, which can produce transparent, smooth, Uniform samples, which solve the problem of difficult forming of conventional aluminum nitride melting samples, and develop a new method for aluminum nitride melting samples

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  • X-ray fluorescence melting sample preparation method of aluminum nitride
  • X-ray fluorescence melting sample preparation method of aluminum nitride
  • X-ray fluorescence melting sample preparation method of aluminum nitride

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Embodiment 1

[0091] In this embodiment, an X-ray fluorescence fusion sample preparation method of aluminum nitride specifically includes:

[0092] (1) Acid hydrolysis in a platinum yellow crucible: Weigh 0.5 g of aluminum nitride powder sample into a platinum yellow crucible, add 3 mL of sulfuric acid solution (pure water: pure sulfuric acid = 1:2), and place the platinum yellow crucible in an oven , first keep it at 110°C for 10 minutes, then keep it at 200°C for 20 minutes, so that the aluminum nitride can be fully acid-decomposed into aluminum sulfate. After acidolysis, there is no white spot on the upper half of the crucible, and no material loss outside the crucible.

[0093] Wherein, the platinum yellow crucible is made of platinum:gold=95:5 (mass ratio), has a height of 3cm-5cm, a diameter of 3cm-5cm, and a volume of 30mL-50mL.

[0094] (2) Removal of sulfuric acid: place the platinum yellow crucible on an electric furnace and keep it at 300°C for 30 minutes to allow the sulfuric a...

Embodiment 2

[0098] In this embodiment, an X-ray fluorescence fusion sample preparation method of aluminum nitride specifically includes:

[0099] (1) Acid hydrolysis in a platinum yellow crucible: Weigh 0.8g aluminum nitride powder sample into a platinum yellow crucible, add 4.5mL sulfuric acid solution (pure water: pure sulfuric acid = 1:2), put the platinum yellow crucible in an oven In the process, first keep it at 130°C for 8 minutes, and then keep it at 200°C for 25 minutes, so that the aluminum nitride can be fully acid-decomposed into aluminum sulfate. After acidolysis, there is no white spot on the upper half of the crucible, and no material loss outside the crucible.

[0100] (2) Removal of sulfuric acid: place the platinum yellow crucible on an electric furnace and keep it at 400°C for 25 minutes to allow the sulfuric acid to volatilize and escape.

[0101] (3) Pyrolysis of aluminum sulfate: Place the platinum yellow crucible in step (2) in a high-temperature furnace and burn a...

Embodiment 3

[0104] In this embodiment, an X-ray fluorescence fusion sample preparation method of aluminum nitride specifically includes:

[0105](1) Acid hydrolysis in a platinum yellow crucible: Weigh 1.0 g of aluminum nitride powder sample into a platinum yellow crucible, add 5.5 mL of sulfuric acid solution (pure water: pure sulfuric acid = 1:2), and place the platinum yellow crucible in an oven In the process, first keep it at 150°C for 5 minutes, and then keep it at 200°C for 30 minutes, so that the aluminum nitride can be fully acid-decomposed into aluminum sulfate. After acidolysis, there is no white spot on the upper half of the crucible, and no material loss outside the crucible.

[0106] (2) Removal of sulfuric acid: place the platinum yellow crucible in a high-temperature furnace and keep it at 500°C for 20 minutes to allow the sulfuric acid to volatilize and escape.

[0107] (3) Pyrolysis of aluminum sulfate: Place the platinum yellow crucible in step (2) in a high-temperatur...

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Abstract

The invention provides an X-ray fluorescence melting sample preparation method of aluminum nitride, and belongs to the technical field of aluminum nitride impurity component analysis and detection. The method comprises the following steps: adding an acid liquor into aluminum nitride for acidolysis to obtain acidolysis gel; burning the acidolysis gel to obtain aluminum oxide; and adding a melting reagent and a release agent into the aluminum oxide, melting, and pouring a sample sheet to obtain a sample sheet. According to the method, the transparent, smooth and uniform sample sheet can be prepared, the problem that forming is difficult in conventional aluminum nitride melting sample preparation is solved, and a new method for aluminum nitride melting sample preparation is developed.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection of aluminum nitride impurity components, and in particular relates to an X-ray fluorescence melting sample preparation method of aluminum nitride. Background technique [0002] Aluminum nitride powder is a powder material with excellent performance. It is the basic key material for the preparation of high-performance aluminum nitride ceramics. Aluminum nitride ceramics with good thermal conductivity, electrical, mechanical and chemical stability are widely used in integrated Circuits, semiconductors, new energy and other industries have extremely important uses in the fields of electronic technology, high-speed rail, aerospace, and military industry. Excessively high impurity elements in aluminum nitride powder will seriously affect the thermal conductivity of downstream aluminum nitride ceramics, so the analysis of impurity elements in aluminum nitride powder is an important task, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202G01N23/223
CPCG01N23/2202G01N23/223G01N2223/076G01N2223/1016G01N2223/652
Inventor 白万里
Owner GUIZHOU BRANCH CHINA ALUMINUM IND