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

Abstract

The invention belongs to the technical field of Raman spectroscopy and develops a microscopic hot stage device based on Raman spectroscopy to measure the amount of dissolved gas in a high-temperature molten salt system. The microscopic hot stage includes a hot stage furnace body and a hot stage reactor; the hot stage furnace body includes a hot stage furnace shell, more than two silicon carbide rods, stainless steel clamps and power cords; the hot stage reactor includes a hot stage reactor Bottom, hot stage reactor flange cover, hot stage screw piston, sample cell and quartz viewing piece. The upper part of the sample pool of the present invention is a sealed quartz window, which prevents volatiles of high-temperature molten salt from contaminating the lens surface and ensures that the Raman incident laser can pass through the quartz window. The hot stage reactor is cooled by the water circuit provided by the flange cover of the hot stage reactor to ensure that the temperature near the microscopic hot stage will not be too high. The microscope lens is close to the surface of the sample cell and is suitable for the measurement of micro-Raman spectra. The length of the silicon carbide rod is longer and farther from the cold end of the silicon carbide rod, ensuring uniform heating of the crucible and reducing the temperature gradient in the sample cell.

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...

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.

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