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A noble metal single atom doped hf 3 no 4 Thin film and its preparation method

A precious metal, hf3n4 technology, applied in metal material coating process, ion implantation plating, vacuum evaporation plating, etc., can solve the problems of environmental threats, mechanical properties degradation, etc., and achieve the improvement of friction and wear resistance, hardness and toughness Enhanced, reproducible results

Active Publication Date: 2020-01-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to reports in the literature, the doped metal content in the nanocomposite film is about 5-10 at.%. Higher metal content will not only cause a certain threat to the environment, but may also lead to a decrease in mechanical properties.

Method used

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  • A noble metal single atom doped hf  <sub>3</sub> no  <sub>4</sub> Thin film and its preparation method
  • A noble metal single atom doped hf  <sub>3</sub> no  <sub>4</sub> Thin film and its preparation method
  • A noble metal single atom doped hf  <sub>3</sub> no  <sub>4</sub> Thin film and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Clean and dry the substrate; specifically: soak the substrate in a diluted hydrofluoric acid solution for 3 to 5 minutes to remove the oxide layer on the substrate surface, hydrofluoric acid in the hydrofluoric acid solution and deionized The volume ratio of water is 1:10-12. Then ultrasonically clean the substrate in acetone solution for 15-25 minutes; then put the substrate in alcohol and ultrasonically clean it for 15-25 minutes; finally, ultrasonically clean the substrate in deionized water for 15-20 minutes, take it out and place it in a drying oven for 40-60 ℃ dry 0.5 ~ 1h.

[0034] 2) Using magnetron sputtering equipment, put the cleaned and dried substrate into the vacuum chamber of the magnetron sputtering device, adjust the deposition angle to 60°, and the distance between the target and the substrate to be 16cm. The temperature is set to 25°C, the bias voltage of the substrate is adjusted to -50V, and the cavity is evacuated to 4×10 -4 Below Pa.

[0035...

Embodiment 2

[0039] Steps 1), 2) are the same as the implementation case 1.

[0040] 3) Introduce the sputtering gas argon and the reaction gas ammonia and nitrogen; set the gas flow rate of argon to 60sccm, and the gas flow ratio of nitrogen and ammonia to 5:60; adjust the working pressure of the vacuum chamber to 0.8Pa; Hf The sputtering current of the target was 0.5A, and the sputtering time was 65 minutes.

[0041] 4) After the sputtering is finished, take out the sample for use.

[0042] 5) After XRD and XPS tests were carried out on the prepared samples, it was confirmed that the Hf prepared in this case x N y The N / Hf atomic ratio y:x of the film is less than 1.33, so in order to obtain the nitrogen-rich phase Hf 3 N 4 It is necessary to further increase the nitrogen content.

Embodiment 3

[0044] Steps 1), 2) are the same as the implementation case 1.

[0045] 3) Introduce the sputtering gas argon and the reaction gases ammonia and nitrogen; set the gas flow rate of argon to 60 sccm, and the gas flow ratio of nitrogen and ammonia to 10:60; adjust the working pressure of the vacuum chamber to 0.8Pa; Hf The sputtering current of the target was 0.5A, and the sputtering time was 70 minutes.

[0046] 4) After the sputtering is finished, take out the sample for use.

[0047] 5) The prepared samples were tested by XRD, TEM, SAED and XPS to confirm that the Hf prepared in this case x N y The N / Hf atomic ratio y:x of the thin film is infinitely close to 1.33, so a Th 3 P 4 Structure of Hf 3 N 4 Thin films, but without noble metal single-atom doping.

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Abstract

The invention discloses a noble metal single-atom-doped Hf3N4 thin film and a preparation method thereof, and belongs to the technical field of functional film material preparation. The atomic percentage contents of noble metal, Hf and N elements in the thin film are 0.59-1.48 at.%, 42-43 at.% and 56-57 at.% respectively; and the thickness of the thin film is 800-1000 nm, and the noble metal in the thin film exists in the form of a single atom. The preparation method comprises the steps of cleaning a substrate, carrying out vacuumizing, setting the temperature, carrying out magnetron sputtering on the substrate, and the like. According to the thin film and the preparation method thereof, the preparation method with a magnetron sputtering low-energy deposition technology is adopted, and thenoble metal single-atom-doped Hf3N4 thin film is successfully prepared. The preparation method has the advantages of a simple process, low cost, high repeatability, high yield, mass industrial production and the like. No by-products are generated in the preparation process, the hardness and toughness of a prepared sample are remarkably improved, and the friction resistance and abrasion resistanceof the film can be greatly improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional film materials, and in particular relates to a Hf3N4 film doped with a noble metal single atom and a preparation method thereof. Background technique [0002] At present, due to the increasingly serious energy and environmental problems, the energy consumed by transportation due to friction and wear accounts for 19% of the world's energy, and the annual emissions of gases account for about 23% of the total greenhouse gas emissions. With the ever-increasing number of motor vehicles, these numbers will undoubtedly increase and maintaining sustainability in transportation presents important challenges. So far, the implementation of new pollution emission efficiency and standards for vehicles has been the main driving force for the development of cleaner and energy-efficient lubricants. Most of the research basically involves reducing the viscosity of base oils and exploring new alt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/06C23C14/35
CPCC23C14/0036C23C14/0641C23C14/35
Inventor 文懋任萍张侃郑伟涛
Owner JILIN UNIV