# US 2025/0027192 A1 · Fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film and preparation method thereof

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- Number: US 2025/0027192 A1
- Document ID: US20250027192A1
- Status: Published application
- Kind: A1
- Application number: 18/715,117
- Filed: 2022-04-27
- Published: 2025-01-23
- Earliest claimed: 2021-04-29
- Assignees: Shanghai Jiao Tong University
- Applicants: Shanghai Jiao Tong University
- Inventors: Juan CHEN; Haolan FANG; Liming PENG; Junjia LIU; Wei SHEN; Tingyan WANG; Yan CHEN; Wenjiang DING
- Web page: https://patentgrep.com/patent/US20250027192A1

## CPC

- C23C 14/35: by application of a magnetic field, e.g. magnetron sputtering {(C23C14/3457 takes precedence)}
- B01J 23/44: Palladium
- B01J 33/00: Protection of catalysts, e.g. by coating
- B01J 37/0215: {Coating}
- C23C 14/021: {Cleaning or etching treatments}
- C23C 14/12: Organic material
- C23C 14/14: Metallic material, boron or silicon
- C23C 14/185: {by cathodic sputtering}
- C23C 14/205: {by cathodic sputtering}
- C23C 14/3414: {Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy}
- C23C 14/352: {using more than one target (C23C14/56 takes precedence)}
- C23C 16/30: Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C 16/50: using electric discharges {(generation and control of plasma in discharge tubes for surface treatment H01J37/32, H01J37/34)}
- B05D 1/62: {Plasma-deposition of organic layers (plasma deposition in general C23C14/00, C23C16/00)}
- B05D 2203/35: Glass
- B05D 2506/10: Fluorinated polymers
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)

## 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.

## Claims

### Claim 1

A fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film, comprising 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.

### Claim 2 (depends on 1)

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%.

### Claim 3 (depends on 1)

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.

### Claim 4 (depends on 1)

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.

### Claim 5 (depends on 1)

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.

### Claim 6 (depends on 5)

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.

### Claim 7 (depends on 5)

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.

### Claim 8 (depends on 5)

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.

### Claim 9 (depends on 5)

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.

### Claim 10 (depends on 5)

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 C4F8 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.

### Claim 11 (depends on 5)

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%.

### Claim 12 (depends on 5)

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.

### Claim 13 (depends on 5)

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.

### Claim 14 (depends on 11)

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.

### Claim 15 (depends on 12)

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.

### Claim 16 (depends on 13)

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.

### Claim 17 (depends on 11)

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.

### Claim 18 (depends on 12)

The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 12, 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.

### Claim 19 (depends on 13)

The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 13, 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.

### Claim 20 (depends on 11)

The preparation method for the fluorocarbon/palladium/magnesium-scandium hydrogen-chromic film according to claim 11, 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.
