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CN-117568751-B - Amorphous Pd-MoS2Film, preparation method and application thereof

CN117568751BCN 117568751 BCN117568751 BCN 117568751BCN-117568751-B

Abstract

The invention provides an amorphous Pd-MoS 2 film, a preparation method and application thereof, and belongs to the technical field of hydrogen evolution catalyst development. According to the invention, the Pd thin sheet is tightly attached to the MoS 2 target material, the amorphous Pd-MoS 2 thin film is prepared by utilizing a magnetron sputtering method, the adjacent Mo position is replaced by Pd doping to change the energy band structure of MoS 2 , the conductive electronic state is introduced around the Fermi level, the metal characteristic of MoS 2 is increased, the conductivity and the catalytic activity are improved, and the problem of insufficient performance of the hydrogen evolution catalyst in the prior art is solved. The amorphous Pd-MoS 2 film provided by the invention has the characteristics of good conductivity, excellent catalytic hydrogen evolution performance and the like when being used as a hydrogen evolution catalyst.

Inventors

  • WANG YANYAN
  • ZHANG YIMING
  • GUO JIANPING
  • LI ZEYAN
  • LI JIANGANG
  • LIAN HUIQIN

Assignees

  • 北京石油化工学院
  • 北京建筑材料科学研究总院有限公司

Dates

Publication Date
20260505
Application Date
20231120

Claims (7)

  1. 1. The preparation method of the amorphous Pd-MoS 2 film is characterized by comprising the following steps of: tightly attaching the Pd sheet to the MoS 2 target to obtain a composite target; coating a substrate material by using the composite target material to obtain an amorphous Pd-MoS 2 film; The method for coating the film is magnetron sputtering; In the composite target, the atomic number ratio of Pd to MoS 2 is 1:8-120; the substrate material is one or more of ITO glass and FTO glass; covering part of the substrate material before coating, wherein the covered area accounts for 5-50% of the total surface area; The material adopted by the cover is one or more of double faced adhesive tape, high temperature adhesive tape or correction fluid.
  2. 2. The method of claim 1, wherein the Pd flakes are sonicated one or more times prior to being applied against the MoS 2 target.
  3. 3. The method of claim 1, wherein the substrate material is subjected to one or more ultrasonic treatments prior to coating.
  4. 4. A method according to claim 2 or 3, wherein the liquid medium used for the ultrasonic treatment is one or more of water, ethanol, acetone and hydrochloric acid; The ultrasonic frequency of the ultrasonic treatment is 5-20 Hz, and the power density is 50-150W; the ultrasonic treatment time is 0.1-1 h.
  5. 5. The method according to claim 1, wherein the magnetron sputtering employs a vacuum degree of 1 x 10 -2 ~1×10 -5 Pa; the sputtering air pressure adopted by the magnetron sputtering is 0.5-5 Pa; The power adopted by the magnetron sputtering is preferably 30-200W.
  6. 6. An amorphous Pd-MoS 2 film obtained by the production method according to any one of claims 1 to 5.
  7. 7. Use of the amorphous Pd-MoS 2 film of claim 6 as a hydrogen evolution catalyst.

Description

Amorphous Pd-MoS 2 film and preparation method and application thereof Technical Field The invention relates to the technical field of hydrogen evolution catalyst development, in particular to an amorphous Pd-MoS 2 film, a preparation method and application thereof. Background Hydrogen is a very clean and efficient energy carrier with very high combustion value per unit mass, and the by-product after combustion is water only, which can be produced in large scale by electrolysis of water. In practical reactions, however, the reaction intermediates formed at the electrode surface need to overcome a relatively high energy barrier and therefore require a suitable catalyst to reduce the overpotential required for electrolysis of the water. The molybdenum disulfide (MoS 2) has rich resources, good catalytic performance and cheaper price, is a layered compound similar to graphite, has more exposed Mo-S edges of monoatomic layer MoS 2, has more electrocatalytic hydrogen production active sites, and has wide application prospect in the aspect of replacing noble metal platinum to become a catalyst which is cheaper and has better hydrogen evolution catalytic performance. However, pure MoS 2 has poor conductivity, and catalytic active sites are distributed at edge positions, so that too good crystallinity is unfavorable for full play of catalytic performance. Chinese patent CN114507875A discloses a molybdenum disulfide catalyst with adjustable phase composition and large interlayer spacing, a preparation method and application thereof, and combines strain effect induced by phase engineering and intercalation ions, and the molybdenum disulfide catalyst prepared by ethanol preferential reduction strategy has higher 1T phase content (73.5%) and additional ammonium ion intercalation, and the insertion of ammonium ions ensures that the molybdenum disulfide catalyst has larger interlayer spacing (0.95 nm), more active sites and faster charge transfer rate. In addition, the basal plane local tensile strain caused by the insertion of ammonium ions further optimizes the hydrogen adsorption of sulfur atoms on the surface of the catalyst. However, the existing molybdenum disulfide catalyst product has complex preparation method, is unfavorable for actual production, and has catalytic performance to be improved. Disclosure of Invention The invention aims to provide an amorphous Pd-MoS 2 film, a preparation method and application thereof, and the preparation is simple, and the obtained amorphous Pd-MoS 2 film has good conductivity and can effectively improve the catalytic hydrogen evolution efficiency. In order to achieve the above object, the present invention provides the following technical solutions: the invention provides a preparation method of an amorphous Pd-MoS 2 film, which comprises the following steps: tightly attaching the Pd sheet to the MoS 2 target to obtain a composite target; coating a substrate material by using the composite target material to obtain an amorphous Pd-MoS 2 film; The coating method is magnetron sputtering. Preferably, in the composite target, the atomic number ratio of Pd to MoS 2 is 1:8-120. Preferably, the Pd sheet is subjected to one or more ultrasonic treatments before being closely attached to the MoS 2 target. Preferably, the substrate material is one or more of ITO glass and FTO glass. Preferably, the substrate material is subjected to one or more ultrasonic treatments prior to coating. Preferably, the liquid medium adopted in the ultrasonic treatment is one or more of water, ethanol, acetone or hydrochloric acid; The ultrasonic frequency of the ultrasonic treatment is 5-20 Hz, and the power density is 50-150W; the ultrasonic treatment time is 0.1-1 h. Preferably, the substrate material covers part of the substrate material before coating, and the covered area accounts for 5-50% of the total surface area; The material adopted by the cover is one or more of double faced adhesive tape, high temperature adhesive tape or correction fluid. Preferably, the vacuum degree adopted by the magnetron sputtering is 1×10 -2～1×10-5 Pa; the sputtering air pressure adopted by the magnetron sputtering is 0.5-5 Pa; The power adopted by the magnetron sputtering is preferably 30-200W. The invention also provides the amorphous Pd-MoS 2 film obtained by the preparation method. The invention also provides application of the amorphous Pd-MoS 2 film in serving as a hydrogen evolution catalyst. The invention has the beneficial effects that: According to the invention, the Pd thin sheet is tightly attached to the MoS 2 target, the amorphous Pd-MoS 2 thin film is prepared by utilizing a magnetron sputtering method, the adjacent Mo position is replaced by Pd doping to change the energy band structure of MoS 2, and the conductive electronic state is introduced around the Fermi level, so that the metal characteristic of MoS 2 is increased, and the conductivity and the catalytic activity are improved. In addition, the amor