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In-situ sum frequency vibration spectrum detection device with laser heating

A laser heating and vibrational spectroscopy technology, applied in the field of in-situ and frequency vibrational spectroscopy characterization, can solve the problem of difficult to achieve high temperature and high pressure conditions of the actual catalytic system, complex total internal reflection and frequency vibrational spectroscopy devices, and frequency vibrational spectroscopy signal-to-noise ratio. It can avoid the interference of side reactions, facilitate disassembly and replacement, and achieve the effect of high heating efficiency.

Active Publication Date: 2020-04-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above problems, the object of the present invention is to provide an in-situ and frequency vibration spectroscopy detection device equipped with laser heating, to solve the problem that the existing total internal reflection and frequency vibration spectroscopy devices are relatively complicated, and it is difficult to achieve the high temperature and high pressure conditions of the actual catalytic system. , and due to the low concentration of surface species, the scattering of the signal by the powder material, the inhomogeneity of the powder surface, etc., the signal-to-noise ratio of the obtained sum frequency vibration spectrum is very poor

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  • In-situ sum frequency vibration spectrum detection device with laser heating
  • In-situ sum frequency vibration spectrum detection device with laser heating
  • In-situ sum frequency vibration spectrum detection device with laser heating

Examples

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Embodiment 1

[0044] According to the following conditions, the sodium dodecyl sulfate (SDS) sum-frequency vibration spectrum and the influence of annealing temperature on the spectrum were measured on the z-cutα quartz crystal:

[0045] In this embodiment, the material of the front window 1 is calcium fluoride, the material of the sample 2 is z-cutα quartz crystal, and the material of the rear window 3 and the lens 16 is zinc selenide. Laser 32 for CO 2 For the laser, the temperature measurement method is to use a thermocouple 34 to measure the temperature. The thermocouple 34 is glued to the edge of the rear surface of the quartz crystal to ensure that the heating laser will not directly shine on the thermocouple 34.

[0046] In this embodiment, the size of the quartz crystal is Φ16×2mm, and 15 μL of 0.27 mmol / L SDS ethanol solution is dropped on the surface of the quartz crystal, with an area of ​​about 40 mm. 2 . Then disassemble the stainless steel outer wall, press the quartz crysta...

Embodiment 2

[0050] According to the following conditions, the sum-frequency vibration spectra of z-cutα quartz crystals dropped with Pt nanoparticles under different CO pressures were measured:

[0051] In this embodiment, the material of the front window 1 is calcium fluoride, the material of the sample 2 is z-cutα quartz crystal, and the material of the rear window 3 and the lens 16 is zinc selenide. Laser 32 for CO 2 For the laser, the temperature measurement method is to use a thermocouple 34 to measure the temperature. The thermocouple 34 is glued to the edge of the rear surface of the quartz crystal to ensure that the heating laser will not directly shine on the thermocouple.

[0052] In this embodiment, the size of the quartz crystal is Φ16×2 mm, and the particle size of the Pt nanoparticles used is about 50 nm. Take 1 mg of Pt powder, add 7 mL of ethanol, and ultrasonically obtain the ethanol dispersion of Pt nanoparticles. Take 35 μL of the dispersion and drop it on the surface ...

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Abstract

The invention belongs to the technical field of in-situ sum frequency vibration spectrum characterization, and particularly relates to an in-situ sum frequency vibration spectrum detection device withlaser heating. The device comprises a sample table, a laser heating and temperature control system and a gas path system. The sample table comprises a sample pool, an adjusting mechanism and a box body which are connected in sequence. An optical element is arranged in the box body, the laser heating and temperature control system is used for emitting laser into the box body, the optical element is used for turning and focusing the laser onto a sample in the sample pool and carrying out laser heating and temperature control on the sample, and the gas path system is used for vacuumizing the sample pool and providing atmospheres with different pressures for the sample pool. The device is small in size and convenient to disassemble and replace, the position of a sample can be adjusted in an x-y plane, and the sample can be rotated by 360 degrees. According to the invention, the change of the surface structure can be represented in situ at different temperatures and pressures.

Description

technical field [0001] The invention belongs to the technical field of in-situ sum-frequency vibration spectrum characterization, in particular to an in-situ sum-frequency vibration spectrum detection device equipped with laser heating. Background technique [0002] Under actual reaction conditions, in situ characterization of catalytic reactions is a very meaningful but challenging topic, especially for heterogeneous catalysis reactions, where in situ detection is even more difficult, because in heterogeneous catalysis reactions occur in For catalyst surfaces, in situ detection means identifying surface signals while avoiding bulk signal interference from catalysts, reactants, and products. [0003] Vibrational spectroscopy, such as infrared and Raman spectroscopy, is commonly used in catalysis research to characterize intermolecular interactions. However, infrared and Raman spectroscopy respond to both bulk and surface molecules. In situ detection, it is necessary to consi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/25G01N21/64G01N21/65
CPCG01N21/25G01N21/64G01N21/65G01N2021/6417
Inventor 罗婷任泽峰张瑞丹彭星星
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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