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

Abstract

A microscopic hot stage and sample pool system for electrochemical in-situ Raman spectroscopy measurement, including a hot stage main body, a hot stage cover, a sealed cabin, a silicon carbon rod, a sample pool and a base; an insulation is provided on the inside of the bottom of the hot stage main body layer, an insulation layer is provided on the insulation layer, the sealed cabin and silicon carbon rods are arranged on the upper part of the insulation layer, and the silicon carbon rods are arranged around the sealed cabin, and an insulation layer is also provided between the silicon carbon rods and the inner wall of the main body of the hot stage; sample The pool is placed in a sealed cabin; the outside of the bottom of the main body of the hot stage is provided with base mounting holes for the insertion of the pillars on the base, silicon carbon rod wire through holes, thermocouple wire through holes and electrode wire through holes. The invention uses a sealed cabin that can pass protective gas and can dynamically add samples with a sample pool, uses a silicon carbon rod that is easy to install and has high calorific value as the heating body, and also designs a cooling unit with an L-shaped cross section on the hot stage cover. The pore channel allows cooling air to be introduced at any time to cool the microscope lens. These designs provide favorable conditions for high-temperature molten salt Raman testing.

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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