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A temperature-controllable infrared in-situ reaction cell based on high vacuum conditions from low temperature to high temperature

An in-situ reaction, infrared technology, applied in instruments, measuring devices, scientific instruments, etc., can solve the problems of the infrared cell being difficult to achieve high vacuum and low temperature, in-situ high temperature treatment of difficult samples, increasing sample consumption, etc., to prevent corrosion. , the effect of reducing the dosage and eliminating the interference of the air background

Active Publication Date: 2021-02-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional infrared pools are difficult to meet the requirements of high vacuum and low temperature
[0004] Usually powder samples need to be diluted with potassium bromide for infrared transmission testing. Such samples are likely to have water absorption peaks during the test, and potassium bromide has a low melting point, making it difficult to perform in-situ high-temperature treatment on samples.
Pressing the sample directly without dilution will greatly increase the sample consumption

Method used

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  • A temperature-controllable infrared in-situ reaction cell based on high vacuum conditions from low temperature to high temperature
  • A temperature-controllable infrared in-situ reaction cell based on high vacuum conditions from low temperature to high temperature
  • A temperature-controllable infrared in-situ reaction cell based on high vacuum conditions from low temperature to high temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Low temperature CO adsorption test of ZnO powder. First take a few milligrams of ZnO powder and press it on the center of a 2cm*1cm tungsten mesh. Install the tungsten mesh sample on the sample holder, and weld the thermocouple near the zinc oxide sample. Place the cold head on the three-dimensional translation stage, and rotate it to a suitable position so that the sample plane is perpendicular to the optical path, and seal and fix it with a copper gasket. Connect an external power supply and a K-type thermocouple thermometer. Turn on the molecular pump unit to evacuate the system, and add liquid nitrogen to the cold head cold trap when the vacuum drops to a certain level. After the sample is degassed through the external power supply parameters, the background is collected after returning to the liquid nitrogen temperature. Use leak valve to feed 10 -3 After mbarCO, the spectrum was collected, and the CO adsorption peak was obtained as shown in the figure. After ...

Embodiment 2

[0059] SiO 2 The supported PtFe catalyst is pressed on the tungsten grid and loaded. After installation, vacuum the system to the proper pressure. Close the suction angle valve and let H 2 And turn on the heating power to carry out activation pretreatment on the sample. After the treatment, the angle valve was opened to evacuate the system, and the temperature was naturally cooled to room temperature, and the background was collected under vacuum. Use a leak valve to feed 10 mbar CO to saturation, then evacuate and collect spectra to obtain the infrared signal of CO adsorbed on the surface. At this time, use the leakage valve to feed and maintain 5*10 -4 mbar oxygen, continuous spectrum collection can get the weakening of the surface CO infrared signal, and thus obtain the CO reaction rate on the surface of the PtFe catalyst, see Figure 6 .

Embodiment 3

[0061] Vapor deposition of CeO on silicon wafers 2 The thin film sample is coated with water and mounted on the sample holder. After installing the cold head, in N 2 The spectrum was collected under atmospheric pressure. After turning on the molecular pump group, pump the cavity to a vacuum of 10 -6 mbar, get spectrum again to get H 2 O in CeO 2 of chemical adsorption.

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Abstract

The invention relates to a temperature-controllable infrared in-situ reaction pool based on high vacuum conditions from low temperature to high temperature. The device consists of two parts, one part is fixed on the main part of the infrared cavity of the infrared spectrometer, including a cubic cavity with a light entrance window and a light exit window, a steel plate for sealing the spectrometer, an air system, and a vacuum pumping system interface , cold head interface, vacuum gauge interface and three-dimensional translation stage, and the other part is a detachable cold head part that integrates sample clamping and temperature adjustment and control. The in-situ cell can achieve air intake and vacuum maintenance under high vacuum conditions, and precise control from low temperature (110K) to high temperature (above 1000K), so that the gas adsorption and reaction of powder samples and film samples under different conditions can be studied in situ and It can effectively eliminate the influence of background atmosphere.

Description

technical field [0001] The invention relates to an infrared test in-situ pool capable of temperature control from low temperature to high temperature under high vacuum based on transmission infrared and a method for using the same, which belongs to the field of chemical in-situ reaction test. Background technique [0002] In situ infrared spectroscopy is an important means to study catalyst adsorption and catalytic reaction in the field of catalysis, and in situ spectral cell is an indispensable device for in situ infrared characterization. In the usual in-situ reaction cell, the light path is exposed to the atmosphere, and changes in water vapor and carbon dioxide components in the air will interfere with the spectrum. As for the gas adsorption signal, the wave number is usually close to that of the gas phase signal. It is necessary to reduce the gas phase signal to eliminate its interference, and the reaction chamber also needs to meet the requirements of medium and high v...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/01
CPCG01N21/01G01N2021/0112
Inventor 杨帆凌云健曹云君包信和赵嘉峰高筱陈栋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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