Fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film and preparation method thereof

Patent metadata

Field	Value
Publication number	US-12584209-B2
Application number	US-202218715117-A
Country	US
Kind code	B2
Filing date	Apr 27, 2022
Priority date	Apr 29, 2021
Publication date	Mar 24, 2026
Grant date	Mar 24, 2026

Abstract

A fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film and a preparation method thereof are provided. The film includes a magnesium-scandium composite film layer, a palladium catalytic layer, and a fluorocarbon film layer that are sequentially arranged on a substrate. The preparation method includes: growing the magnesium-scandium composite film layer on the substrate first, then growing the palladium catalytic layer in situ on the magnesium-scandium layer, and finally depositing the fluorocarbon film layer on Pd. According to the present invention, the catalytic effect of palladium is utilized to promote reversible conversion between hydrogen and hydrogen atoms during hydrogen absorption and dehydrogenation stages, and a composite scandium element is added to accelerate diffusion of the hydrogen atoms in a magnesium matrix and accelerate formation and decomposition of a hydride, such that the film can be repeatedly and rapidly switched between a reflective state and a transparent state.

First claim

What is claimed is:

1 . A fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film, consisting of
a magnesium-scandium composite film layer, a palladium catalytic layer, and a fluorocarbon film layer, wherein the magnesium-scandium composite film layer, the palladium catalytic layer, and the fluorocarbon film layer are sequentially arranged on a substrate; and wherein a hydrogen absorption reaction time of the film is between 5 and 45 seconds, and a hydrogen desorption reaction time of the film is between 70 and 750 seconds.

2 . The fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 1 , wherein in the magnesium-scandium composite film layer, a molar percentage of scandium is 5-75%.

3 . The fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 1 , wherein the magnesium-scandium composite film layer has a thickness of 10-80 nm; the palladium catalytic layer has a thickness of 3-7 nm; and the fluorocarbon film layer has a thickness of 30-150 nm.

4 . The fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 1 , wherein the substrate comprises one of quartz glass, an optical fiber, conductive glass, polymethyl methacrylate, and flexible glass.

5 . A preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 1 , comprising steps of growing the magnesium-scandium composite film layer on the substrate by a magnetron co-sputtering method, then preparing the palladium catalytic layer on the magnesium-scandium composite film layer by a magnetron sputtering method, and finally preparing the fluorocarbon film layer on a surface of the palladium catalytic layer by a plasma vapor deposition method;
wherein the preparation method comprises the following steps: S1, soaking the substrate in a cleaning solution, and then rinsing the substrate; S2, placing a rinsed substrate in a magnetron sputtering reaction chamber, and turning on a vacuum system for vacuuming; S3, heating the rinsed substrate, introducing a first working gas, maintaining a pressure, turning on power supplies of targets after the pressure is stable, closing baffles in front of the targets, and performing pre-sputtering to clean the targets, wherein the targets comprises a palladium target, a magnesium target, and a scandium target; S4, after the pre-sputtering is completed, opening a baffle of the magnesium target and a baffle of the scandium target, loading a co-sputtering process procedure, and depositing the magnesium-scandium composite film layer; S5, after the depositing is completed in the step S4, opening a baffle of the palladium target while maintaining a vacuum degree unchanged, loading a sputtering process procedure of the palladium catalytic layer, and depositing the palladium catalytic layer; S6, after the depositing is completed in the step S5, turning off the power supplies of the targets, purging a sample with the first working gas continuously, then stopping an introduction of the first working gas, and removing a purged sample; and S7, placing the purged sample in a reaction chamber of a reactive ion vapor deposition machine, introducing a second working gas, loading a plasma vapor deposition process procedure, and depositing the fluorocarbon film layer on the surface of the palladium catalytic layer; and after a deposition of the fluorocarbon film layer is completed, taking out a resulting sample to obtain the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film.

6 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the step S1, the cleaning solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:1.

7 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the step S3, the first working gas is argon; in the step S2, the vacuuming is performed to a background vacuum degree of 8×10 −4 -9×10 −5 Pa;
in the step S3, the rinsed substrate is heated to a temperature of 20-25° C., and the pressure is maintained at 0.4-0.6 Pa; and the pre-sputtering is performed for 5-20 min.

8 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the step S4, in the co-sputtering process procedure, sputtering powers used for the magnesium target and the scandium target are 20-100 W and 20-300 W, respectively, and a co-sputtering time is 30-100 s.

9 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the step S5, in the sputtering process procedure, a sputtering power used for the palladium target is 30-80 W, and a sputtering time is 10-60 s.

10 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the step S7, the second working gas is a C 4 F 8 gas; and a working pressure used in the plasma vapor deposition process procedure is 2-6 Pa, the second working gas has a flow rate of 20-50 sccm and a gas excitation power of 400-800 W, and a deposition time is 10-100 s.

11 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film, a molar percentage of scandium in the magnesium-scandium composite film layer is 5-75%.

12 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film, the magnesium-scandium composite film layer has a thickness of 10-80 nm; the palladium catalytic layer has a thickness of 3-7 nm; and the fluorocarbon film layer has a thickness of 30-150 nm.

13 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 5 , wherein in the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film, the substrate comprises one of quartz glass, an optical fiber, conductive glass, polymethyl methacrylate, and flexible glass.

14 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 11 , wherein in the step S1, the cleaning solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:1.

15 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 12 , wherein in the step S1, the cleaning solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:1.

16 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 13 , wherein in the step S1, the cleaning solution is a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:1.

17 . The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 11 , wherein
in the step S3, the first working gas is argon; in the step S2, the vacuuming is performed to a background vacuum degree of 8×10 −4 -9×10 −5 Pa; in the step S3, the rinsed substrate is heated to a temperature of 20-25° C., and the pressure is maintained at 0.4-0.6 Pa; and the pre-sputtering is performed for 5-20 min.

Assignees

• Univ Shanghai Jiaotong

Inventors

• Chen Juan
• Fang Haolan
• Peng Liming
• Liu Junjia
• Shen Wei
• Wang Tingyan
• Chen Yan
• Ding Wenjiang

Classifications

• C23C14/3414

  Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy · CPC title

• C23C14/14

  Metallic material, boron or silicon · CPC title

• C23C14/12

  Organic material · CPC title

• B01J37/0215

  Coating · CPC title

• B01J33/00 Primary

  Protection of catalysts, e.g. by coating · CPC title