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A Micro-Hot Stage Device for Measuring Dissolved Gases in High Temperature Molten Salt System Based on Raman Spectroscopy

A technology of dissolved gas and high-temperature molten salt, applied in the field of spectral analysis, can solve the problems of short length of silicon carbide rod, large temperature gradient in the heating area, and small heating area, and achieve uniform heating temperature, reduce temperature gradient, and increase temperature. fast effect

Active Publication Date: 2019-06-18
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, the length of the silicon carbide rod used in the microscopic heating stage is relatively short, and the heating area is relatively close to the cold end of the silicon carbide rod, resulting in a small heating area, a large temperature gradient in the heated area of ​​the sample pool, and uneven heating of the sample pool.
In addition, when the gas is ventilated to the sample cell in the micro-heating stage, the quartz plate covered above will be blown up, which on the one hand destroys the airtightness of the hot-stage reactor, and on the other hand makes the online detection of the Raman spectrum impossible.

Method used

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  • A Micro-Hot Stage Device for Measuring Dissolved Gases in High Temperature Molten Salt System Based on Raman Spectroscopy
  • A Micro-Hot Stage Device for Measuring Dissolved Gases in High Temperature Molten Salt System Based on Raman Spectroscopy
  • A Micro-Hot Stage Device for Measuring Dissolved Gases in High Temperature Molten Salt System Based on Raman Spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] At 973K, the Li 2 O-LiCl-Li 2 SO 4 CO in molten salt system 2 Raman Spectroscopy Determination of Dissolved Amounts.

[0047] Use crucible: corundum crucible;

[0048] Drugs: Li 2 The manufacturer of O is Shanghai Jingchun Biochemical Technology Co., Ltd., with a purity of 99.9%; the manufacturer of LiCl is Shanghai Jingchun Biochemical Technology Co., Ltd., with a purity greater than 99%; 2 CO 3 The manufacturer is Sinopharm Chemical Reagent Co., Ltd., with a purity of 98%; Li 2 SO 4 The manufacturer is Sinopharm Chemical Reagent Co., Ltd., with a purity of 99%;

[0049] Raman spectrometer: HR800 microlaser Raman spectrometer from Horiba JobinYvon, Japan;

[0050] Laser: 177-G1205 argon ion 488nm laser from Spectra-Physics

[0051] Microscope (lens): Japan Olympus microscope (SLMPLN 50X microscope lens);

[0052] Temperature controller: Beijing Chaoyang Automatic Instrument Factory CKW-3100;

[0053] According to the experimental measurement of Raman spectr...

Embodiment 2

[0058] At 1073K, molten NaOH absorbs CO 2 Generate Na 2 CO 3 Determination by Raman spectroscopy.

[0059] Use crucible: corundum crucible;

[0060] Drugs: Na 2 SO 4The manufacturer is Sinopharm Chemical Reagent Co., Ltd., with a purity of 99%; Na 2 CO 3 The manufacturer of NaOH is Sinopharm Chemical Reagent Co., Ltd., with a purity of 99.8%; the manufacturer of NaOH is Sinopharm Chemical Reagent Co., Ltd., with a purity of 96%.

[0061] Cylinder: CO 2 , the manufacturer of the carbon dioxide cylinder is Sifang Gas Co., Ltd., the purity is 99.9%;

[0062] Raman spectrometer: HR800 microlaser Raman spectrometer from Horiba JobinYvon, Japan;

[0063] Laser: the built-in 633nm laser of the spectrometer;

[0064] Microscope (lens): Japan Olympus microscope (SLMPLN 50X microscope lens);

[0065] Temperature controller: Beijing Chaoyang Automatic Instrument Factory CKW-3100;

[0066] Such as Figure 6 As shown, according to the experimental measurement of Raman spectrum...

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Abstract

The invention belongs to the technical field of Roman spectrum analysis and develops a microscope heat state device used for measuring gas solubility in a high-temperature molten salt system on the basis of the Roman spectroscopy. The microscope heat stage device comprises a heat stage furnace and a heat stage reactor; the heat stage furnace comprises a heat stage furnace shell, more than two silicon carbide rods, stainless steel clamps and power lines; the heat stage reactor comprises a heat stage reaction base, a heat stage reactor flange cover, a heat stage screw piston, a sample pool and a quartz observation tablet. A sealed quartz window is arranged in the upper portion of the sample pool, volatile of high-temperature molten salt is prevented from polluting the surface of a lens, and Roman incident laser is ensured to pass through the quartz observation window; the heat stage reaction is cooled through water path circulation of the heat stage reaction flange cover, and temperature nearby the microscope heat stage is ensured not to be so high; the microscope lens is close to the surface of the sample pool, which is suitable for detection of the micro-Raman spectrum; the silicon carbide rods are long and far from cold ends of the silicon carbide rods, even heating of a crucible is guaranteed, and temperature gradient in the sample pool is decreased.

Description

technical field [0001] The invention belongs to the technical field of spectral analysis, and in particular relates to a micro-heating stage device for measuring the amount of gas dissolved in a high-temperature molten salt system based on Raman spectroscopy. Background technique [0002] In the process of producing metal by molten salt electrolysis, the dissolution of anode gas and the interaction with the cathode metal are important factors affecting the current efficiency of molten salt electrolysis. Therefore, it is meaningful to detect the amount of gas dissolved in molten salt, which can provide parameter feedback for molten salt electrolysis. [0003] On the other hand, because molten salt has the advantages of wide chemical window and high current efficiency, there have been many research reports on the electrolysis of gas in molten salt system, such as the electrolysis of CO in molten salt 2 Preparation of C material and O 2 , not only can realize the CO 2 effect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65
CPCG01N21/65
Inventor 胡宪伟邓文涛王志鑫石忠宁高炳亮王兆文于江玉
Owner NORTHEASTERN UNIV LIAONING
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