CN-121994555-A - Preparation method of molybdenum disulfide-containing transmission electron microscope sample

Abstract

The invention provides a preparation method of a transmission electron microscope sample containing molybdenum disulfide, which comprises the following steps of 1, carrying out ultrasonic dispersion on a sample to be detected and an organic solvent, 2, dripping supernatant obtained after dispersion in the step 1 on a carbon film, then drying the carbon film under a vacuum condition, and 3, putting the dried carbon film into a carbon spraying instrument for carbon spraying and film coating to obtain the transmission electron microscope sample. The preparation method of the molybdenum disulfide-containing transmission electron microscope sample can not only avoid the problem that molybdenum disulfide is easily oxidized by air in the process of preparing the transmission electron microscope sample, but also is simple, has short preparation time, can rapidly acquire high-resolution transmission electron microscope images of molybdenum disulfide stripe phases, and is further used for researching the structure and performance of a catalyst.

Inventors

• ZHANG RUOLIN
• ZHANG JINGYUAN
• XU HUA
• CHEN FEI
• GAO ZHAO
• WANG FEI
• LIN JUN
• AN MI
• WANG CHUNYAN
• HUO MINGCHEN

Assignees

• 中国石油天然气股份有限公司

Dates

Publication Date

20260508

Application Date

20241101

Claims (10)

1. 1. The preparation method of the transmission electron microscope sample containing molybdenum disulfide is characterized by comprising the following steps of: Step 1, performing ultrasonic dispersion on a sample to be tested and an organic solvent; Step 2, dripping the supernatant liquid dispersed in the step 1 on a carbon film, and then drying the carbon film under a vacuum condition; And step 3, placing the dried carbon film into a carbon spraying instrument, and spraying carbon to coat the film to obtain a transmission electron microscope sample.
2. 2. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the sample to be tested is a hydrogenation catalyst in a sulfurized state, and an active component of the hydrogenation catalyst comprises molybdenum.
3. 3. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the hydrogenation catalyst uses a molybdenum disulfide stripe phase as an active component.
4. 4. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the organic solvent is at least one of absolute ethanol, n-hexane and absolute methanol.
5. 5. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein in the ultrasonic dispersion, the ultrasonic dispersion frequency is 20-120Hz, and the dispersion time is 5-10min.
6. 6. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein in step 1, the sample to be measured is subjected to ultrasonic dispersion after being ground with an organic solvent.
7. 7. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the carbon film is a micro-grid support film, an ultra-thin carbon support film or a pure carbon support film.
8. 8. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the liquid obtained in step 2 is dripped into the carbon film, the liquid drop below the carbon film is sucked dry, and then the carbon film is dried under vacuum.
9. 9. The method for preparing the molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the drying condition is that the vacuum degree is less than 400Pa and the drying time is 5-20min.
10. 10. The method for preparing a molybdenum disulfide-containing transmission electron microscope sample according to claim 1, wherein the thickness of the carbon spray coating is 2-50nm.

Description

Preparation method of molybdenum disulfide-containing transmission electron microscope sample Technical Field The invention belongs to the field of catalyst evaluation, and particularly relates to a preparation method of a molybdenum disulfide transmission electron microscope sample. Background In industrial production, 80% of the production process needs catalyst, and the hydrogenation catalyst product is an important traffic fuel and is a national economic pulse. Common hydrogenation catalysts are gasoline hydrogenation catalysts, diesel hydrogenation catalysts, aviation kerosene hydrogenation catalysts, lubricating oil hydrogenation catalysts, residual oil hydrogenation catalysts and the like. With the increasing strictness of environmental protection regulations, the content of sulfur and polycyclic aromatic hydrocarbon in gasoline and diesel oil is limited, the quality of diesel oil products is upgraded from national IV standard to national V standard, the sulfur mass fraction is required to be reduced from 50 mug/g to 10 mug/g, the quality fraction of polycyclic aromatic hydrocarbon is upgraded from national V standard to national VI standard, and the quality fraction of polycyclic aromatic hydrocarbon is reduced from 11% to 7%. The dual quality requirements of low sulfur, low aromatics and the impact of poor quality feedstocks make catalytic hydrogenation processes very challenging. Further enhancement of the activity of hydrogenation catalysts has become an important point of research. The premise of improving the activity of the catalyst is to deeply know the key active components of the catalyst, and a Transmission Electron Microscope (TEM) is a microscope with high resolution and high magnification, and can provide information on the tissue structure, crystal structure, chemical components and the like of the superfine material. The work of using TEM to study the morphology and distribution of the molybdenum disulfide active phase in hydrogenation catalysts has been increasingly appreciated by broad catalyst developers. The molybdenum disulfide active phase is easily oxidized when being exposed in the air, and the preparation technology of the transmission electron microscope sample directly relates to the microstructure of the active phase, so that the intrinsic information of the sample is particularly important. The molybdenum disulfide streak phase sample will react with oxygen in the air, converting from molybdenum disulfide to molybdenum oxide. How to solve the problem of oxidization of the molybdenum disulfide streak phase sample becomes a key for shooting the high-resolution transmission electron microscope image of the molybdenum disulfide streak phase sample. At present, in order to prevent the molybdenum disulfide stripe phase sample from being combined with air, the catalyst needs to be embedded by adopting epoxy resin, after the epoxy resin is solidified, a slice is cut by using an ultrathin slice and is transferred to an ultrathin carbon film for observation, and the sample preparation time needs 2 days. Long time and high cost. Thus, there is still a need in the art for further research into the preparation of molybdenum disulfide transmission electron microscope samples. Disclosure of Invention The invention mainly aims to provide a preparation method of a transmission electron microscope sample containing molybdenum disulfide, which aims to solve the problem that molybdenum disulfide is easily oxidized by air in the process of preparing the transmission electron microscope sample in the prior art. In order to achieve the above purpose, the invention provides a preparation method of a transmission electron microscope sample containing molybdenum disulfide, which comprises the following steps: Step 1, performing ultrasonic dispersion on a sample to be tested and an organic solvent; Step 2, dripping the supernatant liquid dispersed in the step 1 on a carbon film, and then drying the carbon film under a vacuum condition; And step 3, placing the dried carbon film into a carbon spraying instrument, and spraying carbon to coat the film to obtain a transmission electron microscope sample. The preparation method of the molybdenum disulfide-containing transmission electron microscope sample comprises the steps that the sample to be detected is a hydrogenation catalyst in a vulcanized state, and the active component of the hydrogenation catalyst comprises molybdenum. The preparation method of the molybdenum disulfide-containing transmission electron microscope sample provided by the invention comprises the step of taking a molybdenum disulfide stripe phase as an active component of the hydrogenation catalyst. The preparation method of the molybdenum disulfide-containing transmission electron microscope sample provided by the invention comprises the step of preparing a molybdenum disulfide-containing transmission electron microscope sample from a solvent. The preparation method of the molybd