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Transfer method of air sensitive sample applied to X-ray photoelectron spectrometer

A technology of photoelectron spectroscopy and transfer method, which is applied to the transfer of air-sensitive samples and the field of air-sensitive sample transfer, which can solve the problems of high cost and complicated operation steps.

Active Publication Date: 2021-10-15
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the deficiencies in the background technology, the purpose of the present invention is to provide a method for transferring air-sensitive samples applied to X-ray photoelectron spectrometers, which can effectively avoid changes in the state of sensitive samples exposed to the air, and realize air-sensitive samples very conveniently. The sample is transferred to the XPS analysis room for testing. This method can replace the complex and expensive online in-situ XPS sample pretreatment process, and it can also be used as a supplement for the sample transfer by the inert gas conveyor. The present invention makes up for the shortcomings of the prior art and provides Transfer of air-sensitive samples to XPS analysis chamber for testing opens up new method

Method used

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  • Transfer method of air sensitive sample applied to X-ray photoelectron spectrometer
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  • Transfer method of air sensitive sample applied to X-ray photoelectron spectrometer

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Experimental program
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Effect test

Embodiment 1

[0028] Step 1, install a three-way joint on a top of the U-shaped quartz tube, wherein one joint 1 of the joint is connected to the quartz tube, the other joint 2 is the inlet of the reducing atmosphere, and the third joint 3 of the joint is sealed with a silicone rubber gasket;

[0029] Step 2: Put the 2 g CuO / CNT sample to be reduced into a U-shaped quartz tube at room temperature, put the quartz tube into a constant temperature furnace, and continuously flow 50 mL / min of 10% H 2 / Ar gas, in 10%H 2 / Ar atmosphere 350 ℃ reduction for 2 hours;

[0030] Step 3: After the reduction is completed, after the temperature of the U-shaped quartz tube drops to room temperature, inject 2 g of isooctane into the silicone rubber pad;

[0031] Step 4, turn off the reducing gas, remove the tee joint, and take out the mixed system containing isooctane and CuO / CNT samples from the U-shaped quartz tube together;

[0032] Step 5, immobilize the mixed system containing isooctane and CuO / CNT sa...

Embodiment 2

[0036] Step 1, install a three-way joint on a top of the U-shaped quartz tube, wherein one joint 1 of the joint is connected to the quartz tube, the other joint 2 is the inlet of the reducing atmosphere, and the third joint 3 of the joint is sealed with a silicone rubber gasket;

[0037] Step 2: Put 1 g of the Pt / R-MOF-5 sample to be reduced into a U-shaped quartz tube at room temperature, put the quartz tube into a constant temperature furnace, and continuously flow 50 mL / min of 10% H 2 / Ar gas, in 10%H 2 / Ar atmosphere 250 ℃ reduction for 1 hour;

[0038] Step 3: After the reduction is completed, after the temperature of the U-shaped quartz tube drops to room temperature, inject 1 g of n-decane into the silicone rubber pad;

[0039] Step 4, turn off the reducing gas, remove the tee joint, and take out the mixed system containing n-decane and Pt / R-MOF-5 samples from the U-shaped quartz tube together;

[0040] Step five, immobilize the mixed system containing n-decane and Pt...

Embodiment 3

[0044] Step 1, install a three-way joint on a top of the U-shaped quartz tube, wherein one joint 1 of the joint is connected to the quartz tube, the other joint 2 is the inlet of the reducing atmosphere, and the third joint 3 of the joint is sealed with a silicone rubber gasket;

[0045] Step 2, put the 2 g Ag / HY sample to be reduced into a U-shaped quartz tube, put the quartz tube into a constant temperature furnace, and continuously feed 50 mL / min 10%H 2 / Ar gas, in 10%H 2 Reduction at 180 °C for 1.5 hours in / Ar atmosphere;

[0046] Step 3: After the reduction is completed, after the temperature of the U-shaped quartz tube drops to room temperature, inject 3 g of n-hexane into the silicone rubber pad;

[0047] Step 4, turn off the reducing gas, remove the tee joint, and take out the mixed system containing n-hexane and Ag / HY samples from the U-shaped quartz tube together;

[0048] Step 5: Immobilize the mixed system containing n-hexane and Ag / HY samples on the XPS special...

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Abstract

The invention discloses a transfer method of an air sensitive sample applied to an X-ray photoelectron spectrometer, the method comprises the following steps of: directly placing a pre-reduced air-sensitive sample in a low-boiling-point hydrocarbon solvent, immobilizing a mixed system of the low-boiling-point hydrocarbon solvent and the sample on an XPS special sample table, transferring the mixed system to an XPS pre-vacuumizing chamber, and after pre-vacuumizing until the vacuum degree is at least 5 * 10 <-8 > Torr, transferring to an XPS analysis chamber for XPS analysis. According to the method, the inert and volatile hydrocarbon substances are utilized, the solvent is completely pumped away through XPS pre-vacuumizing, it is guaranteed that the sample is not directly exposed in the air, the problem of transferring of the XPS sample sensitive to the air under the air isolation condition is simply and ingeniously solved, and the in-situ online treatment process of the air-sensitive sample which is tedious in operation and high in cost can be replaced.

Description

technical field [0001] The invention belongs to the technical field of testing, and relates to an air-sensitive sample transfer method, in particular to an air-sensitive sample transfer method applied to an X-ray photoelectron energy spectrometer. Background technique [0002] X-ray Photoelectron Spectroscopy (XPS) is a commonly used material surface analysis technology instrument, mainly for high-sensitivity test and analysis of element composition and valence state in the depth range of several nanometers on the surface of solid materials (Chinese invention patent CN202011484825.7). XPS characterization technology can be used to study the valence state and content (semi-quantitative) of each constituent element of composite materials containing metals and metal oxides. However, many composite materials containing metals and metal oxides are easily exposed to air and oxygen The reaction will change the properties of the material, resulting in the XPS test results not reflec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2273
CPCG01N23/2273
Inventor 薛青松邢俊玲
Owner EAST CHINA NORMAL UNIV
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