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Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry

A technology of fluorescence spectroscopy and impurity content, which is applied in the detection field of silicon carbide, can solve the problems of difficult sample preparation, failure to meet the requirements of chromium and titanium detection, and high hardness of silicon carbide samples, so as to improve accuracy and speed, and greatly popularize Use value, effect of reducing workload

Active Publication Date: 2010-06-02
CHEM MINERALS & METALLIC MATERIALS INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0005] 1. The detection requirements of silicon carbide are generally silicon carbide, ferric oxide, aluminum oxide, calcium oxide, magnesium oxide, phosphorus, sulfur, etc., but chemical analysis methods are used, and various components are tested separately. Meet the requirements of rapid and effective detection of various components at the same time, but cannot meet the requirements of some users for detection of chromium, titanium, etc.
[0007] 3. Silicon carbide samples have high hardness and difficult sample preparation

Method used

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  • Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry
  • Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry

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preparation example Construction

[0048] (1) Preparation of test samples

[0049]Weigh a certain amount of silicon carbide sample, grind it, then weigh the finely ground sample, add binder (wax powder) according to the ratio of 5:1, grind it in the mortar, and keep the pressure under 20-40T for 20~ 40s, pressed into test pieces.

[0050] Through the experimental research on sample processing materials, grinding equipment, and time, it is determined that the preparation method of silicon carbide samples is as follows: weigh about a certain amount of silicon carbide samples, and use tungsten carbide ball milling equipment to grind for several minutes to achieve stable test results. Controllable, sufficient fineness, and small head loss requirements.

[0051] (2) Preparation of standard samples

[0052] ① Sample preparation for purified silicon carbide

[0053] Weigh 120# abrasive grade silicon carbide, and grind it for 6 minutes with a ball mill made of tungsten carbide;

[0054] ②Silicon carbide purificatio...

Embodiment

[0071] (1) Preparation of test samples

[0072] Weigh 1.5g of silicon carbide sample, grind it with a tungsten carbide ball mill for 6 minutes, then accurately weigh 1.0g of the ground sample, add 0.2g of wax powder, grind it evenly, hold the pressure at 30T for 30s, and press it into a test samples.

[0073] (2) Preparation of standard samples

[0074] ① Sample preparation for purified silicon carbide

[0075] Weigh 25.0000g of high-grade 120# abrasive grade silicon carbide, and grind it for 6 minutes with a ball mill made of tungsten carbide.

[0076] ②Silicon carbide purification

[0077] i. Removal of volatile substances in silicon carbide

[0078] Weigh 20.0000g of the ground silicon carbide sample, place it in a platinum dish, put it in a muffle furnace at 800°C and burn it for 1.5h to remove volatile substances, take it out and cool it.

[0079] ii. Remove impurity silicon in silicon carbide

[0080] Use a dropper to wet the silicon carbide sample in step i with p...

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Abstract

The invention relates to a method for detecting the content of carborundum impurities by applying an X-ray fluorescent spectrometry, comprising the following steps of: firstly, preparing a test sample wafer; secondly, preparing a standard sample wafer: (1) purifying a sample of carborundum; (2) purifying the carborundum to prepare puried carborundum; and (3) artificially preparing a standard sample and finally pressing the standard sample into a standard carborundum sample wafer; thirdly, establishing a working curve of the X-ray fluorescent spectrometry by the standard sample wafer; and fourthly, placing the prepared test sample wafer in an X-ray fluorescent spectrograph, measuring the sample wafer by the established working curve and automatically calculating the contents of various elements in the sample. By adopting the method, the workload for preparing standard series can be greatly reduced and the accuracy and the speed for preparation can be improved, thereby avoiding the defects of the traditional method for detecting the carborundum. The method is concise and rapid, meets the requirement of trade development, has great generalization and application values, and can be widely suitable for testing various samples by the X-ray fluorescent spectrum.

Description

technical field [0001] The invention relates to a detection method of silicon carbide, in particular to a method suitable for scientific research units, colleges, testing centers and corresponding manufacturers to detect the impurity content of silicon carbide by X-ray fluorescence spectroscopy. Background technique [0002] X-ray fluorescence spectrometry is a modern general analysis method for elemental analysis of various materials. It is widely used in environmental protection, geology, metallurgy, cement, inspection and quarantine and other departments. Good sex and other characteristics. The application of X-ray fluorescence spectrometer is mainly for quantitative analysis, and the content of each element in the sample can be obtained by measuring the prepared sample. The preparation of samples is mainly two kinds of sample preparation by molten glass method and pressing. The quality of sample preparation directly affects the accuracy of measurement results. Tablet p...

Claims

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Application Information

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IPC IPC(8): G01N23/223
Inventor 魏红兵谷松海宋义郭芬潘宏伟魏伟陈焱
Owner CHEM MINERALS & METALLIC MATERIALS INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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