A microscopic hot stage and sample cell system for electrochemical in-situ Raman spectroscopy

Abstract

A microscope hot stage and sample pool system used for electrochemistry in-situ Raman spectrum measurement comprises a hot stage body, a hot stage cover, a sealed cabin, silicon carbide rods, a sample pool and a base. An insulating layer is arranged on the inner side of the bottom of the hot stage body. A heat preservation layer is arranged on the insulating layer. The sealed cabin and the silicon carbide rods are arranged on the upper portion of the heat preservation layer. The silicon carbide rods surround the sealed cabin. A heat preservation layer is arranged between the silicon carbide rods and the inner wall of the hot stage body. The sample pool is arranged in the sealed cabin. A base installation hole for a base upper supporting column to be inserted therein, silicon carbide rod wire through holes, a thermocouple wire through hole and an electrode wire through hole are formed in the outer side of the bottom of the hot stage body. By means of the microscope hot stage and sample pool system, protection gas can be introduced, the sealed cabin allowing samples to be dynamically added is used in cooperation with the sample pool, the silicon carbide rods convenient to install and high in heating amount are used as heating bodies, a cooling pore way with the L-shaped section is designed on the hot stage cover, cooling gas can be introduced at any time to cool a microscope lens, and advantages are provided for high-temperature fused salt Raman tests due to the design.

Description

technical field [0001] The invention belongs to the technical field of electrochemical and optical analysis, and in particular relates to a micro-heating stage and a sample cell system for electrochemical in-situ Raman spectrum measurement. Background technique [0002] Spectroelectrochemistry is a research method that combines electrochemical testing techniques with various spectroscopic techniques. According to the test method, spectroelectrochemistry can be divided into two types: in situ and ex situ. Spectroelectrochemical technology not only has the characteristics of high energy resolution of spectroscopic technology, but also has the characteristics of high sensitivity of electrochemical testing technology. Dynamic spectroscopy (time-resolved spectroscopy) enables people to dynamically obtain optical and electrical signals in experiments, which enables the identification and capture of unstable intermediates at the molecular level, monitoring the instantaneous state ...

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Problems solved by technology

[0007] The above test devices generally have the following problems: 1. The dynamic addition method of the sample is not considered when designing the sample cell. It is often necessary to add the sample to the sample cell before the test and then seal the sample cell. Due to the solid sample Melting and volatilization of the sample under high temperature conditions make the height of the liquid level lower than that of the solid sample before melting, which is unfavorable for the Raman microscope lens with limited focal length; 2. The heating body of the test device is often made of metal Resistance wire, and when using resistance wire to heat, in order to achieve a higher operating temperature, a longer resistance wire is often required, but due to limited space, this will bring a lot of inconvenience; 3. The microscope lens equipped with the test device is far from the high temperature area Due to the limited focal length of the Raman microscope lens during measurement, the lens is very close to the liquid surface of the sample, and the large amount of thermal radiation generated in this way will cause serious corrosion to the Raman microscope lens, which was not considered by previous researchers. The link of cooling and protecting the lens

This patent has made great improvements and innovations to the above-mentioned several test devices, and uses a quartz cover to seal the crucible sample cell, but the sample cell still has great restrictions on the use of protective gas, and the patent uses a metal resistance wire Heating the analyte

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