CN111650295A - Method for detecting carbon content of silicon powder - Google Patents
Method for detecting carbon content of silicon powder Download PDFInfo
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- CN111650295A CN111650295A CN202010431866.3A CN202010431866A CN111650295A CN 111650295 A CN111650295 A CN 111650295A CN 202010431866 A CN202010431866 A CN 202010431866A CN 111650295 A CN111650295 A CN 111650295A
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- silicon powder
- detecting
- carbon content
- gas
- detection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention discloses a method for detecting carbon content of silicon powder, which relates to the technical field of silicon powder detection and comprises the following steps: (1) sampling silicon powder; (2) burning the silicon powder; (3) collecting gas; (4) detecting and calculating; (5) and detecting the grouping. According to the method for detecting the carbon content of the silicon powder, the silicon powder is conveniently combusted through the combustion furnace, the combustion temperature of the combustion furnace is 950-.
Description
Technical Field
The invention relates to the technical field of silicon powder detection, in particular to a method for detecting carbon content of silicon powder.
Background
The silicon powder is also called micro silicon powder, known as silica fume, and is formed by collecting and treating smoke dust escaping with waste gas in the process of smelting industrial silicon and ferrosilicon at high temperature by an industrial electric furnace through a special collecting device. The method for preparing the silicon powder by taking the silicon briquette as the raw material has a plurality of methods, good effect and more applications. The carbon content in the silicon powder has a certain influence on the quality of the product, so that the carbon content in the silicon powder needs to be detected
The existing detection method for carbon content of silicon powder has long detection time and poor detection precision, and the silicon powder with complex components is easily interfered by other component elements in the detection process of the carbon content, so that the detection data is inaccurate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for detecting the carbon content of silicon powder, which solves the problems that the existing method for detecting the carbon content of the silicon powder, which is provided in the background art, has long detection time and poor detection precision, and the silicon powder with complex components is easily interfered by other component elements in the detection process of the carbon content, so that the detection data is inaccurate.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for detecting the carbon content of silicon powder comprises the following steps:
(1) sampling silicon powder;
(2) burning the silicon powder;
(3) collecting gas;
(4) and detecting and calculating
(5) And detecting the grouping.
Optionally, the method for detecting the carbon content of the silicon powder comprises the following specific steps:
(1) silica powder sampling
Weighing a silicon powder sample, putting the silicon powder sample to be detected into a crucible, adding a fluxing agent, and then putting the crucible into a combustion furnace;
(2) burning silica powder
Feeding high-purity oxygen into the combustion furnace through an oxygen supply device, so that the silicon powder is melted and combusted in the combustion furnace;
(3) gas collection
Collecting and collecting the combusted mixed gas, separating carbon dioxide gas in the mixed gas by adopting a gas chromatograph, detecting, and sending the detected carbon dioxide gas into a carbon dioxide absorption liquid;
(4) and detecting and calculating
During detection, the separated carbon dioxide gas sample group is quantitatively detected through an infrared analyzer, and according to the determination principle of an infrared spectroscopy, a characteristic spectral line generated by high-temperature combustion is detected, so that the carbon concentration is measured, and the percentage of the carbon content is calculated through conversion;
(5) packet detection
In the detection process, the carbon dioxide gas is divided into three control groups, three groups of standard gas samples are taken, then each control group is detected respectively, the detection data is recorded, and the three groups of detection data are averaged to obtain an average value, so that the detection precision is improved, and the detection error is reduced.
Optionally, the flux is pure iron flux.
Optionally, the combustion temperature of the combustion furnace is 950-.
Optionally, the combustion furnace is a high-frequency infrared combustion furnace, and the infrared analyzer is a high-frequency combustion infrared analyzer.
Optionally, the carbon dioxide absorption liquid is mainly a calcium hydroxide solution.
The invention provides a method for detecting the carbon content of silicon powder, which has the following beneficial effects: according to the method for detecting the carbon content of the silicon powder, the silicon powder is conveniently combusted through the combustion furnace, the combustion temperature of the combustion furnace is 950-.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
A method for detecting the carbon content of silicon powder comprises the following steps:
(1) sampling silicon powder;
(2) burning the silicon powder;
(3) collecting gas;
(4) and detecting and calculating
(5) And detecting the grouping.
The method for detecting the carbon content of the silicon powder comprises the following specific steps:
(1) silica powder sampling
Weighing a silicon powder sample, putting the silicon powder sample to be detected into a crucible, adding a fluxing agent, and then putting the crucible into a combustion furnace;
the flux is pure iron flux which is used for flux during combustion of a sample furnace in carbon sulfur analysis, and carbon sulfur in metal and non-metal materials such as steel, alloy and the like is analyzed and determined;
(2) burning silica powder
Feeding high-purity oxygen into the combustion furnace through an oxygen supply device, so that the silicon powder is melted and combusted in the combustion furnace;
the combustion temperature of the combustion furnace is 950-;
(3) gas collection
Collecting and collecting the combusted mixed gas, separating carbon dioxide gas in the mixed gas by adopting a gas chromatograph, detecting, and sending the detected carbon dioxide gas into a carbon dioxide absorption liquid;
the carbon dioxide absorption liquid is mainly a calcium hydroxide solution, and the calcium hydroxide solution can absorb carbon dioxide gas;
(4) and detecting and calculating
During detection, the separated carbon dioxide gas sample group is quantitatively detected through an infrared analyzer, and according to the determination principle of an infrared spectroscopy, a characteristic spectral line generated by high-temperature combustion is detected, so that the carbon concentration is measured, and the percentage of the carbon content is calculated through conversion;
the combustion furnace is a high-frequency infrared combustion furnace, and the infrared analyzer is a high-frequency combustion infrared analyzer;
(5) packet detection
In the detection process, the carbon dioxide gas is divided into three control groups, three groups of standard gas samples are taken, then each control group is detected respectively, the detection data is recorded, and the three groups of detection data are averaged to obtain an average value, so that the detection precision is improved, and the detection error is reduced.
In summary, the method for detecting the carbon content of the silicon powder comprises the following steps:
(1) and silicon powder sampling: weighing a silicon powder sample, putting the silicon powder sample to be detected into a crucible, adding a fluxing agent, and then putting the crucible into a combustion furnace;
(2) and silicon powder combustion: feeding high-purity oxygen into the combustion furnace through an oxygen supply device, so that the silicon powder is melted and combusted in the combustion furnace;
(3) and gas collection: collecting and collecting the combusted mixed gas, separating carbon dioxide gas in the mixed gas by adopting a gas chromatograph, detecting, and sending the detected carbon dioxide gas into a carbon dioxide absorption liquid;
(4) and detection and calculation: during detection, the separated carbon dioxide gas sample group is quantitatively detected through an infrared analyzer, and according to the determination principle of an infrared spectroscopy, a characteristic spectral line generated by high-temperature combustion is detected, so that the carbon concentration is measured, and the percentage of the carbon content is calculated through conversion;
(5) grouping detection: in the detection process, the carbon dioxide gas is divided into three control groups, three groups of standard gas samples are taken, then each control group is detected respectively, the detection data is recorded, and the three groups of detection data are averaged to obtain an average value, so that the detection precision is improved, and the detection error is reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The method for detecting the carbon content of the silicon powder is characterized by comprising the following steps of:
(1) sampling silicon powder;
(2) burning the silicon powder;
(3) collecting gas;
(4) detecting and calculating;
(5) and detecting the grouping.
2. The method for detecting the carbon content of the silicon powder according to claim 1, wherein the method for detecting the carbon content of the silicon powder comprises the following specific steps:
(1) silica powder sampling
Weighing a silicon powder sample, putting the silicon powder sample to be detected into a crucible, adding a fluxing agent, and then putting the crucible into a combustion furnace;
(2) burning silica powder
Feeding high-purity oxygen into the combustion furnace through an oxygen supply device, so that the silicon powder is melted and combusted in the combustion furnace;
(3) gas collection
Collecting and collecting the combusted mixed gas, separating carbon dioxide gas in the mixed gas by adopting a gas chromatograph, detecting, and sending the detected carbon dioxide gas into a carbon dioxide absorption liquid;
(4) and detecting and calculating
During detection, the separated carbon dioxide gas sample group is quantitatively detected through an infrared analyzer, and according to the determination principle of an infrared spectroscopy, a characteristic spectral line generated by high-temperature combustion is detected, so that the carbon concentration is measured, and the percentage of the carbon content is calculated through conversion;
(5) packet detection
In the detection process, the carbon dioxide gas is divided into three control groups, three groups of standard gas samples are taken, then each control group is detected respectively, the detection data is recorded, and the three groups of detection data are averaged to obtain an average value, so that the detection precision is improved, and the detection error is reduced.
3. The method for detecting the carbon content of the silicon powder according to claim 2, wherein the method comprises the following steps: the fluxing agent is pure iron fluxing agent.
4. The method for detecting the carbon content of the silicon powder according to claim 2, wherein the method comprises the following steps: the combustion temperature of the combustion furnace is 950-.
5. The method for detecting the carbon content of the silicon powder according to claim 2, wherein the method comprises the following steps: the combustion furnace is a high-frequency infrared combustion furnace, and the infrared analyzer is a high-frequency combustion infrared analyzer.
6. The method for detecting the carbon content of the silicon powder according to claim 2, wherein the method comprises the following steps: the carbon dioxide absorption liquid is mainly calcium hydroxide solution.
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CN202010431866.3A CN111650295A (en) | 2020-05-20 | 2020-05-20 | Method for detecting carbon content of silicon powder |
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CN202010431866.3A CN111650295A (en) | 2020-05-20 | 2020-05-20 | Method for detecting carbon content of silicon powder |
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2020
- 2020-05-20 CN CN202010431866.3A patent/CN111650295A/en not_active Withdrawn
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Application publication date: 20200911 |