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Pretreatment method for detecting boron element of silicon crystal by controlling digestion reaction heat with dry ice

A silicon crystal and reaction heat technology, which is used in thermal excitation analysis, preparation of test samples, material excitation analysis, etc. The effect of obvious retention, shortening detection cost and shortening detection time

Inactive Publication Date: 2017-11-24
DALIAN UNIV OF TECH QINGDAO NEW ENERGY MATERIALS TECH RES INST CO LTD
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Problems solved by technology

[0002] At present, in the pretreatment process of polysilicon detection by ICP-AES, whether it is a powder sample or a granular sample, a large amount of heat of reaction is generated during the digestion process, which leads to an instantaneous rise in the temperature of the reaction system and the formation of fluoboric acid, which is decomposed into Boron trifluoride is volatile, causing serious loss of boron element, resulting in seriously low accuracy of test results, and the results have no practical significance

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  • Pretreatment method for detecting boron element of silicon crystal by controlling digestion reaction heat with dry ice

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Embodiment Construction

[0021] The present invention is described below based on examples, but the present invention is not limited to these examples.

[0022] The invention provides a pretreatment method for detecting silicon crystal boron element through controlled digestion reaction heat of dry ice, comprising the following steps:

[0023] a. Accurately weigh a certain amount of sample according to the actual impurity content of the sample and place it in a 100ml PTFE beaker. Parallel experiments are required;

[0024] b. Accurately add 5g of high-purity dry ice, the purity of which is 99.995%;

[0025] c. Accurately measure 5.0ml of hydrofluoric acid and add it to the beaker, adding it carefully;

[0026] d. Finally, slowly add 2.0ml of 70% nitric acid, the phenomenon is severe, so be careful to add it dropwise;

[0027] e. React until the sample is completely dissolved;

[0028] f. Volatile silicon at low temperature, constant volume after acidity adjustment, ICP-AES detection.

[0029] The ...

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Abstract

The invention relates to the field of detection of content of a boron element in a silicon crystal, and in particular relates to a pretreatment method for detecting the boron element in the silicon crystal by controlling digestion reaction heat with dry ice. The pretreatment method is characterized in that temperature of a reaction system is controlled by adding moderate amount of dry ice in a silicon crystal digestion process, so that the boron element easy to be lost due to gasification is reserved to the utmost extent. The pretreatment method provided by the invention has the advantages that the boron element and other metal elements in polycrystalline silicon can be detected at the same time, the boron element reserving effect is obvious, the pretreatment method is simple and easy to operate, detection time is shortened, and detection cost is reduced.

Description

technical field [0001] The invention relates to the field of detection of boron element content in silicon crystals, in particular to a pretreatment method for detecting the boron element of silicon crystals by controlling the digestion reaction heat of dry ice. Background technique [0002] At present, in the pretreatment process of polysilicon detection by ICP-AES, whether it is a powder sample or a granular sample, a large amount of heat of reaction is generated during the digestion process, which leads to an instantaneous rise in the temperature of the reaction system and the formation of fluoboric acid, which is decomposed into Boron trifluoride is volatile, causing serious loss of boron element, resulting in a serious low accuracy of test results, and the results have no practical significance. Contents of the invention [0003] In view of this, the object of the present invention is to provide a pretreatment method for controlling the digestion reaction heat of dry ...

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Application Information

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IPC IPC(8): G01N1/44G01N21/73
CPCG01N1/44G01N21/73
Inventor 池明刘瑶张磊
Owner DALIAN UNIV OF TECH QINGDAO NEW ENERGY MATERIALS TECH RES INST CO LTD
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