A preparation method and application of a metal hydride surface titanium-based hydrogen barrier coating structure

By preparing a 0.5–2.5 μm thick titanium nitride-based hydrogen barrier layer on the surface of metal hydrides, the problem of material performance degradation caused by hydrogen diffusion at high temperatures was solved, and the hydrogen barrier effect and bonding strength were improved, making it suitable for the nuclear industry and hydrogen storage equipment.

CN121228190BActive Publication Date: 2026-02-24INNER MONGOLIA UNIV OF TECH +1
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Patent Information

Application Number
CN202511812360.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-12-04
Publication Date
2026-02-24
Estimated Expiration
2045-12-04

AI Technical Summary

Technical Problem

Existing technologies address the issue of hydrogen diffusion in metal hydrides under high temperature and strong radiation environments, leading to a decline in material mechanical properties and hydrogen embrittlement cracking. Traditional coatings are prone to aging or have insufficient adhesion at high temperatures, making it difficult to effectively block hydrogen atom diffusion.

Method used

A titanium nitride-based hydrogen barrier layer with a thickness of 0.5–2.5 μm was prepared on the surface of a metal hydride substrate by magnetron sputtering. By controlling process parameters such as argon flow rate, working pressure, RF power supply and magnetron sputtering time, a dense titanium-based hydrogen barrier layer was formed to block the diffusion of hydrogen atoms.

Benefits of technology

It effectively prevents hydrogen atom diffusion, enhances the hydrogen barrier properties of metal hydrides, extends their service life in the nuclear industry and hydrogen storage equipment, and ensures the bonding stability between the coating and the substrate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a preparation method and application of a metal hydride surface titanium-based hydrogen barrier coating structure, which is composed of a metal hydride base and a titanium-based hydrogen barrier layer, and the titanium-based hydrogen barrier layer covers the surface of the metal hydride base; the chemical composition of the titanium-based hydrogen barrier layer is titanium nitride. The preparation method comprises the following steps: (1) polishing, chemical cleaning and drying treatment are sequentially performed on the metal hydride base material to obtain a metal hydride base; (2) the metal hydride base material is placed into a magnetron sputtering film coating chamber, argon is introduced for etching cleaning after vacuumizing; and (3) after the etching cleaning is completed, a titanium target is used as a sputtering target material, and nitrogen is used as a reaction gas to perform magnetron sputtering, so that the metal hydride surface titanium-based hydrogen barrier coating structure is obtained. The metal hydride surface titanium-based hydrogen barrier coating structure can be used as a nuclear material in high-temperature working conditions of nuclear industry or hydrogen storage equipment, and can solve the performance degradation problem of the metal hydride caused by hydrogen diffusion.
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Description

Technical Field

[0001] This invention relates to the field of metal hydride surface protection technology. Specifically, it relates to a method for preparing and applying a titanium-based hydrogen-barrier coating structure for metal hydride surfaces. Background Technology

[0002] In the nuclear industry, metal hydrides are important hydrogen storage materials, and their stable performance is crucial for the safe operation of equipment and energy output. However, under high temperature and strong radiation environments, metal hydrides face serious hydrogen diffusion problems, which can lead to lattice distortion, causing a decline in the material's mechanical properties, hydrogen embrittlement, and other issues. The diffused hydrogen atoms can also corrode surrounding materials, threatening system safety.

[0003] Currently, there are limited methods for preventing hydrogen diffusion in metal hydrides. Traditional organic coatings are prone to aging and decomposition under high temperature and strong radiation, and cannot prevent hydrogen diffusion in the long term. Inorganic coatings prepared by methods such as thermal spraying have problems such as insufficient adhesion to the substrate and loose structure, making it difficult to effectively block the diffusion of hydrogen atoms.

[0004] Micro-arc oxidation and sol-gel coating processes also have several drawbacks. Micro-arc oxidation coatings contain numerous micropores and microcracks, which become convenient channels for hydrogen atom diffusion at high temperatures, leading to a significant decrease in hydrogen barrier performance. Sol-gel coatings exhibit poor uniformity, difficulty in precisely controlling film thickness, and a cumbersome preparation process requiring multiple coating and sintering steps, resulting in low production efficiency. Furthermore, sol-gel coatings exhibit poor stability at high temperatures and are prone to structural changes, further reducing their hydrogen barrier performance.

[0005] Therefore, there is an urgent need to develop a coating preparation technology that is process-controllable, has excellent hydrogen barrier properties, and is firmly bonded to the substrate. Summary of the Invention

[0006] Therefore, the technical problem to be solved by the present invention is to provide a method for preparing and applying a titanium-based hydrogen barrier coating structure on the surface of metal hydrides, so as to solve the problem of performance degradation of metal hydrides caused by hydrogen diffusion and improve their reliability and service life in the fields of nuclear industry and hydrogen storage; the titanium-based hydrogen barrier coating structure on the surface of metal hydrides prepared by the present invention can be applied to the hydrogen protection and performance improvement of metal hydride materials in the fields of nuclear industry and hydrogen storage equipment.

[0007] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0008] A titanium-based hydrogen barrier coating structure for a metal hydride surface is provided, comprising a metal hydride substrate and a titanium-based hydrogen barrier layer, wherein the titanium-based hydrogen barrier layer directly covers the surface of the metal hydride substrate; the chemical composition of the titanium-based hydrogen barrier layer is titanium nitride.

[0009] The aforementioned titanium-based hydrogen-barrier coating structure on the surface of a metal hydride has a metal hydride substrate with a chemical composition of zirconium-based metal hydride or rare earth hydride; the thickness of the titanium-based hydrogen-barrier layer is 0.5–2.5 μm. This invention controls the thickness of the titanium-based hydrogen-barrier layer to 0.5–2.5 μm, which ensures the hydrogen-barrier effect of the titanium-based hydrogen-barrier layer while effectively avoiding the large internal stress caused by an excessively thick titanium-based hydrogen-barrier layer, which could affect its bonding stability with the metal hydride substrate.

[0010] A method for preparing a titanium-based hydrogen-barrier coating structure on a metal hydride surface includes the following steps:

[0011] Step (1): The metal hydride substrate is successively polished, chemically cleaned and dried. After the drying process is completed, the metal hydride matrix is ​​obtained.

[0012] Step (2): Place the metal hydride substrate in the magnetron sputtering coating chamber, evacuate the chamber, and then introduce argon gas for etching and cleaning to further clean and activate the surface.

[0013] Step (3): After etching and cleaning, a titanium target is used as the sputtering target and nitrogen is used as the reaction gas to form a titanium-based hydrogen barrier layer on the surface of the metal hydride substrate by magnetron sputtering. After the magnetron sputtering is completed, the above-mentioned titanium-based hydrogen barrier coating structure on the surface of the metal hydride is obtained.

[0014] In the preparation method of the above-mentioned titanium-based hydrogen barrier coating structure on the surface of metal hydride, the grinding process in step (1) is as follows: first, use 400-grit sandpaper to coarsely grind the metal hydride substrate until the surface is flat, and remove surface oxide layer, burrs and other impurities; then, use 800-grit, 1200-grit and 1500-grit sandpaper to further finely grind until the surface roughness is 0.05-0.3μm, so as to increase the contact area between the coating and the substrate and improve the bonding force.

[0015] In the preparation method of the above-mentioned titanium-based hydrogen barrier coating structure on the surface of metal hydride, the chemical cleaning method in step (1) is as follows: the metal hydride substrate after polishing is placed in acetone and cleaned at an ultrasonic frequency of 35-45 kHz for 15-25 min to remove oil and other organic pollutants; then it is transferred to anhydrous ethanol and cleaned at an ultrasonic frequency of 35-45 kHz for 10-20 min to remove residual impurities.

[0016] In the preparation method of the above-mentioned titanium-based hydrogen barrier coating structure on the surface of metal hydride, the drying conditions in step (1) are: drying at 75-85℃ for 1-3 hours.

[0017] In the preparation method of the above-mentioned titanium-based hydrogen barrier coating structure on the surface of metal hydride, in step (2), the vacuum degree is 0.5×10⁻ before argon gas is introduced. 4 Pa ~ 5 × 10⁻ 4The working pressure is 0.3–1.5 Pa to remove air and impurities from the chamber; the argon purity is greater than or equal to 99.99%; the argon flow rate is 15–30 sccm (if the argon flow rate is greater than 30 sccm, it will increase the surface roughness of the etched surface and damage the sample; if the argon flow rate is less than 15 sccm, it will slow down the etching rate and reduce the etching cleaning efficiency); the working pressure is 0.3–1.5 Pa (if the working pressure during etching cleaning is too high, the probability of ions colliding with neutral molecules during movement will increase, thereby weakening the ion energy, resulting in a decrease in the number and energy of effective ions reaching the substrate surface, thus reducing the etching rate; if the working pressure is too low, the gas molecule density will be insufficient, making it difficult to maintain a stable plasma discharge, which may lead to plasma extinction). Etching can be disrupted by fluctuations or local instability, affecting the repeatability and consistency of etching. The RF power supply should be 100–200W. (Using excessively high power during etching and cleaning will significantly increase the energy and density of ions in the plasma, resulting in excessive physical bombardment of the substrate surface, causing surface roughness or even damage. Insufficient power will lead to low plasma density and weak ion energy, resulting in a significant decrease in etching rate, extending process time, and reducing production efficiency. This is especially true for high aspect ratio structures, such as deep trenches and vias, where the etching rate may be too slow, leading to incomplete etching.) The etching and cleaning time should be 10–20 minutes. If the etching time is too long, it will lead to a decrease in surface precision, damage to the substrate material, and reduced production efficiency. If the etching time is too short, it will lead to incomplete etching and insufficient etching depth, which will affect subsequent processes. This invention effectively removes residual impurities from the surface of the metal hydride substrate by controlling the argon flow rate, working pressure, RF power supply, and etching time within a suitable range during the etching process. This allows the surface of the metal hydride substrate to be fully activated, providing surface conditions for the subsequent deposition of the titanium-based hydrogen barrier layer. This is beneficial for improving the adhesion between the metal hydride substrate and the titanium-based hydrogen barrier layer, as well as the stability of the crystal structure of the titanium-based hydrogen barrier layer.

[0018] In the above method for preparing a titanium-based hydrogen barrier coating structure on the surface of a metal hydride, in step (3), the mass fraction of titanium in the titanium target is greater than or equal to 99.95 wt%; the nitrogen flow rate is 5-20 sccm; the magnetron sputtering power is 100-250 W; the temperature of the magnetron sputtering coating chamber is controlled at 150-280℃; and the magnetron sputtering time is 60-120 min, which is conducive to the growth of coating crystals and ensures the quality and performance of the coating. During magnetron sputtering deposition, excessive nitrogen flow can lead to an overabundance of nitrogen, resulting in a titanium-based hydrogen barrier layer with a high nitrogen content. This nitrogen may form a nitrogen-rich phase within the layer, and the excess nitrogen can increase internal stress, making it more prone to cracking or peeling. It also reduces the layer's density and increases its porosity. Conversely, insufficient nitrogen flow can lead to impurities and reduced hydrogen barrier performance. Excessive magnetron sputtering power can cause a rapid deposition rate, resulting in a lower layer quality, increased stress, and cracking. Insufficient power can lead to a slow deposition rate, low production efficiency, poor adhesion, and easy detachment. High deposition temperature can result in coarse grains and reduced uniformity in the layer, while low temperature can lead to low density and high porosity. By controlling the nitrogen flow rate, magnetron sputtering power, coating chamber temperature, and magnetron sputtering time within the above-mentioned ranges during magnetron sputtering, this invention enables titanium and nitrogen to fully react on the surface of the metal hydride substrate, and allows the formed titanium nitride crystals to grow fully to form a dense and strongly adherent titanium-based hydrogen barrier layer.

[0019] In the preparation method of the above-mentioned titanium-based hydrogen barrier coating structure on the surface of metal hydride, the grinding method in step (1) is as follows: first, use 400-mesh sandpaper to coarsely grind the metal hydride substrate until the surface is flat, and then use 800-mesh, 1200-mesh and 1500-mesh sandpaper to further finely grind until the surface roughness is 0.1μm.

[0020] The chemical cleaning method is as follows: the polished metal hydride substrate is placed in acetone and cleaned at an ultrasonic frequency of 40 kHz for 20 min, and then transferred to anhydrous ethanol and cleaned at an ultrasonic frequency of 40 kHz for 15 min; the drying conditions are: drying at 80℃ for 2 h.

[0021] In step (2), the vacuum degree is 1×10⁻ before argon gas is introduced. 4 Pa; Argon purity equals 99.99%; Argon flow rate is 25 sccm, working pressure is 0.5 Pa; RF power supply power is 150W, etching and cleaning time is 15 min;

[0022] In step (3), the mass fraction of titanium in the titanium target is 99.99 wt%; the nitrogen flow rate is 15 sccm; the magnetron sputtering power is 200 W; the temperature of the magnetron sputtering coating chamber is controlled at 250 °C; and the magnetron sputtering time is 120 min.

[0023] An application of a titanium-based hydrogen barrier coating structure on a metal hydride surface: the above-mentioned titanium-based hydrogen barrier coating structure on a metal hydride surface is used as a nuclear material in the high-temperature conditions of nuclear industry or hydrogen storage equipment.

[0024] The technical solution of the present invention achieves the following beneficial technical effects:

[0025] 1. In the titanium-based hydrogen-barrier coating structure on the metal hydride surface of this invention, the titanium-based hydrogen-barrier layer directly covers the surface of the metal hydride substrate. In the titanium-based hydrogen-barrier layer, titanium and nitrogen elements form a dense and stable crystal structure through chemical bonding, exhibiting a typical face-centered cubic structure with a lattice constant of approximately 0.424 nm. This structure has extremely small lattice gaps, effectively blocking the physical diffusion of hydrogen atoms. Furthermore, the coating exhibits chemical adsorption with hydrogen atoms, capturing them and thus achieving the purpose of hydrogen barrier. This invention controls the thickness of the titanium-based hydrogen-barrier layer to 0.5–2.5 μm, ensuring the hydrogen barrier effect while effectively avoiding the large internal stress caused by an excessively thick titanium-based hydrogen-barrier layer, which could affect its bonding stability with the metal hydride substrate.

[0026] 2. The method for preparing the titanium-based hydrogen barrier coating structure on the surface of a metal hydride according to the present invention employs magnetron sputtering. By precisely controlling the process parameters, a titanium nitride coating is directly applied to the surface of the metal hydride substrate, resulting in a titanium-based coating structure with a tight bond between the titanium-based hydrogen barrier layer and the metal hydride substrate and excellent hydrogen barrier performance. In this invention, the titanium-based hydrogen barrier layer can effectively prevent the diffusion and penetration of hydrogen atoms through both physical barriers and chemical adsorption. The main mechanism of the chemical adsorption effect of the titanium-based hydrogen barrier layer is as follows: the empty d orbitals of Ti atoms in the titanium-based hydrogen barrier layer prepared by the present invention can form coordinate bonds with the 1s electrons of H atoms, adsorbing H atoms around the Ti atoms; at the same time, the Ti atoms at the grain boundaries, dislocations and other defects in the titanium-based hydrogen barrier layer are unsaturated in coordination, resulting in stronger adsorption capacity and stable capture of H atoms; in addition, the hydrogen-nitrogen bond (NH bond) formed between H atoms and nitrogen also plays a certain role in the chemical adsorption of hydrogen atoms. Compared with traditional metal hydride surface coating materials, the titanium-based hydrogen barrier coating prepared by this invention can significantly improve the hydrogen barrier performance of the metal hydride matrix, inhibit hydrogen atom migration, and avoid performance degradation of metal hydrides due to hydrogen diffusion. It can be widely used in nuclear industry, hydrogen storage devices and other fields, providing an efficient and reliable hydrogen protection solution for material systems involving metal hydrides. Attached Figure Description

[0027] Figure 1 A schematic diagram of the coating process of the titanium-based hydrogen barrier coating structure on the surface of the metal hydride in Embodiment 1 of the present invention;

[0028] Figure 2 A schematic diagram of the coating principle of the magnetron sputtering preparation device in Embodiment 1 of the present invention;

[0029] Figure 3 Surface microscopic SEM image, Ti element EDS image and N element EDS image of the titanium-based hydrogen barrier coating structure on the metal hydride surface in Example 1 of this invention;

[0030] Figure 4 Cross-sectional microscopic SEM image of the titanium-based hydrogen barrier coating structure on the surface of the metal hydride in Embodiment 1 of the present invention;

[0031] Figure 5 The cross-sectional EDS total spectrum, Ti element EDS spectrum, and N element EDS spectrum of the titanium-based hydrogen barrier coating structure on the metal hydride surface in Example 1 of this invention;

[0032] Figure 6 A three-dimensional AFM image of the titanium-based hydrogen barrier coating structure on the surface of the metal hydride in Embodiment 1 of the present invention;

[0033] Figure 7 Two-dimensional AFM image of the titanium-based hydrogen barrier coating structure on the surface of the metal hydride in Embodiment 1 of the present invention;

[0034] Figure 8 Laser confocal three-dimensional morphology image of the titanium-based hydrogen barrier coating structure on the surface of the metal hydride in Embodiment 1 of the present invention;

[0035] Figure 9 Comparison of hydrogen barrier performance of titanium-based hydrogen barrier coatings on metal hydride surfaces prepared in Examples 1 to 3 of this invention;

[0036] Figure 10 X-ray diffraction pattern of the titanium-based hydrogen barrier layer prepared in Example 1 of this invention. Detailed Implementation

[0037] Example 1

[0038] The preparation method of the titanium-based hydrogen-barrier coating structure on the surface of the metal hydride in this embodiment includes the following steps:

[0039] Step (1): The metal hydride substrate is successively polished, chemically cleaned and dried. After the treatment is completed, a metal hydride matrix is ​​obtained. The metal hydride substrate used in this embodiment is a zirconium hydride substrate, and the hydrogen-zirconium atomic ratio of zirconium hydride is greater than 1.65.

[0040] The polishing process is as follows: first, use 400-grit sandpaper for coarse polishing until the surface is smooth, and then use 800-grit, 1200-grit, and 1500-grit sandpaper for fine polishing until the surface roughness is 0.1 μm; the chemical cleaning process is as follows: place the polished metal hydride substrate in acetone and clean it at a 40 kHz ultrasonic frequency for 20 min, and then transfer it to anhydrous ethanol and clean it at a 40 kHz ultrasonic frequency for 15 min; the drying process is as follows: dry at 80℃ for 2 h.

[0041] Step (2): Place the metal hydride substrate into the magnetron sputtering deposition chamber and evacuate to a vacuum level of 1×10⁻⁻⁻⁶. 4 Pa, argon gas is introduced, the purity of argon gas is equal to 99.99%; argon gas flow rate is 15 sccm, working gas pressure is 0.5 Pa, radio frequency power is 150W, and etching and cleaning are performed for 15 minutes;

[0042] Step (3): After etching and cleaning, a titanium target is used as the sputtering target (the mass fraction of titanium in the titanium target is equal to 99.99 wt%), and nitrogen is used as the reaction gas for magnetron sputtering. The nitrogen flow rate is 5 sccm, the magnetron sputtering power is 100 W, the temperature of the magnetron sputtering coating chamber is controlled at 150℃, and the magnetron sputtering time is 60 min. After the magnetron sputtering is completed, the sample is taken out after the chamber cools to room temperature, and the titanium-based hydrogen barrier coating structure on the metal hydride surface is obtained. The thickness of the titanium-based hydrogen barrier layer is about 1 μm.

[0043] The performance of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment was tested: using a hydrogen permeability tester, the hydrogen permeability reduction factor (PRF) of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment was 13.2 compared with the untreated metal hydride material; the adhesion was tested by scratch test, and the adhesion between the titanium-based hydrogen barrier layer and the metal hydride matrix reached 42.7 N.

[0044] Figure 3 and Figure 5 Energy dispersive spectroscopy (EDS) analysis confirmed that the atomic ratio of titanium and nitrogen in the coating conformed to the stoichiometry of titanium-based materials. Figure 3 It can be seen that the particles on the coating surface are fine and uniform; through the elemental distribution, it can be seen that the distribution of elements such as Ti and N on the coating surface is relatively uniform, indicating that the elemental bonding and distribution in the TiN coating is ideal. Figure 4 Scanning electron microscopy (SEM) observation showed that the prepared coating surface was smooth and dense, without obvious pores and defects.

[0045] Three-dimensional morphology (Figure 6): The coating surface exhibits microscopic three-dimensional undulations. Atomic force microscopy was used to measure the surface roughness of the coating, yielding Rq: 95.743 nm and Ra: 77.007 nm. The roughness values ​​are much smaller than the coating thickness and will not affect the integrity of the coating. Two-dimensional morphology (Figure 6) Figure 7 ): Showcasing the microscopic texture of the coating surface, exhibiting a granular or clustered structure, through Figure 7 It can be observed that the particles on the coating surface are relatively uniform in size and distribution, indicating that the TiN coating forms a relatively regular film on the surface during magnetron sputtering.

[0046] Figure 8 This provides a three-dimensional view of the coated surface, allowing observation of macroscopic surface undulations, and complements AFM. Figure 8 It can be seen that the overall surface of the coating is relatively smooth, with no obvious abrupt defects in some areas, indicating that the surface quality of the coating is good. This verifies the smoothness of the TiN coating prepared by magnetron sputtering on the metal hydride surface on a macroscopic scale.

[0047] X-ray diffraction analysis showed that the titanium-based hydrogen barrier layer has typical titanium-based face-centered cubic structure characteristics, with a lattice constant of approximately 0.424 nm (see [link to relevant documentation]). Figure 10 This indicates that titanium and nitrogen elements in the titanium-based hydrogen barrier layer form a dense and stable crystal structure through chemical bonding.

[0048] Example 2

[0049] The only difference between this embodiment and embodiment 1 is that in step (2), the argon flow rate is 20 sccm; in step (3), when magnetron sputtering is used for coating, the nitrogen flow rate is 10 sccm, the sputtering power is 150 W, the sputtering time is 90 min, the chamber temperature is 200℃, and a titanium-based hydrogen barrier layer with a thickness of about 1.2 μm is prepared.

[0050] The other steps, process parameters and raw materials are exactly the same as in Example 1.

[0051] Testing showed that the PRF value of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment was 18.1, and the bonding force between the titanium-based hydrogen barrier layer and the metal hydride substrate reached 46.2 N. The surface microstructure and cross-sectional microstructure of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment are basically the same as those in Example 1, and will not be repeated here.

[0052] Example 3

[0053] The only difference between this embodiment and embodiment 1 is that in step (2), the argon flow rate is 25 sccm; in step (3), when magnetron sputtering is used for coating, the nitrogen flow rate is 15 sccm, the sputtering power is 200 W, the sputtering time is 120 min, the chamber temperature is 250℃, and a titanium-based hydrogen barrier coating with a thickness of about 2 μm is prepared.

[0054] The other steps, process parameters and raw materials are exactly the same as in Example 1.

[0055] Testing showed that the PRF value of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment was 22.3, and the bonding force between the titanium-based hydrogen barrier layer and the metal hydride substrate reached 56.7 N. The surface microstructure and cross-sectional microstructure of the titanium-based hydrogen barrier coating structure on the metal hydride surface prepared in this embodiment are basically the same as those in Example 1, and will not be repeated here.

[0056] Table 1. Process parameters and performance values ​​for each embodiment

[0057]

[0058] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of the claims of this patent application.

Claims

1. A method for preparing a titanium-based hydrogen-barrier coating structure on a metal hydride surface, characterized in that, Includes the following steps: Step (1): The metal hydride substrate is successively polished, chemically cleaned and dried. After the drying process is completed, the metal hydride matrix is ​​obtained. Step (2): Place the metal hydride substrate in the magnetron sputtering coating chamber, evacuate the chamber, and then introduce argon gas for etching and cleaning. Step (3): After etching and cleaning, a titanium target is used as the sputtering target and nitrogen is used as the reaction gas to form a titanium-based hydrogen barrier layer on the surface of the metal hydride substrate by magnetron sputtering. After the magnetron sputtering is completed, the titanium-based hydrogen barrier coating structure on the surface of the metal hydride is obtained. The titanium-based hydrogen barrier coating structure on the surface of the metal hydride consists of a metal hydride substrate and a titanium-based hydrogen barrier layer, with the titanium-based hydrogen barrier layer covering the surface of the metal hydride substrate. The chemical composition of the metal hydride substrate is zirconium-based metal hydride. The chemical composition of the titanium-based hydrogen barrier layer is titanium nitride. The thickness of the titanium-based hydrogen barrier layer is 0.5-2.5 μm. The mass fraction of titanium in the titanium target is greater than or equal to 99.95 wt%. The nitrogen flow rate is 5-20 sccm, the magnetron sputtering power is 100-250 W, the temperature of the magnetron sputtering coating chamber is controlled at 150-280 °C, and the magnetron sputtering time is 60-150 min.

2. The method for preparing the titanium-based hydrogen-barrier coating structure on the surface of a metal hydride according to claim 1, characterized in that, In step (1), the grinding process is as follows: first, use 400-grit sandpaper to coarsely grind the metal hydride substrate until the surface is flat, and then use 800-grit, 1200-grit and 1500-grit sandpaper to further finely grind until the surface roughness is 0.05-0.3μm.

3. The method for preparing the titanium-based hydrogen-barrier coating structure on the surface of a metal hydride according to claim 1, characterized in that, In step (1), the chemical cleaning method is as follows: the polished metal hydride substrate is placed in acetone and cleaned at an ultrasonic frequency of 35-45 kHz for 15-25 min, and then transferred to anhydrous ethanol and cleaned at an ultrasonic frequency of 35-45 kHz for 10-20 min.

4. The method for preparing the titanium-based hydrogen-barrier coating structure on the surface of a metal hydride according to claim 1, characterized in that, In step (1), the drying conditions are: drying at 75-85℃ for 1-3 hours.

5. The method for preparing the titanium-based hydrogen-barrier coating structure on the surface of a metal hydride according to claim 1, characterized in that, In step (2), the vacuum degree is 0.5×10⁻ before argon gas is introduced. 4 Pa ~ 5 × 10⁻ 4 Pa; Argon purity greater than or equal to 99.99%; Argon flow rate 15–30 sccm, working pressure 0.3–1.5 Pa; RF power supply power 100–200 W, etching and cleaning time 10–20 min.

6. The method for preparing the titanium-based hydrogen-barrier coating structure on the surface of a metal hydride according to claim 1, characterized in that, In step (1), the polishing method is as follows: first, use 400-grit sandpaper to coarsely polish until the surface is flat, and then use 800-grit, 1200-grit and 1500-grit sandpaper to finely polish until the surface roughness is 0.1μm. The chemical cleaning method is as follows: the polished metal hydride substrate is placed in acetone and cleaned at an ultrasonic frequency of 40 kHz for 20 min, and then transferred to anhydrous ethanol and cleaned at an ultrasonic frequency of 40 kHz for 15 min. The drying conditions are: drying at 80℃ for 2 hours; In step (2), the vacuum degree is 1×10⁻ before argon gas is introduced. 4 Pa; Argon purity equals 99.99%; Argon flow rate is 25 sccm, working pressure is 0.5 Pa; RF power supply power is 150W, etching and cleaning time is 10 min; In step (3), the mass fraction of titanium in the titanium target is 99.99 wt%; the nitrogen flow rate is 15 sccm; the magnetron sputtering power is 200 W; the temperature of the magnetron sputtering coating chamber is controlled at 250 °C; and the magnetron sputtering time is 120 min.

7. The application of a titanium-based hydrogen-barrier coating structure on a metal hydride surface, characterized in that, The titanium-based hydrogen barrier coating structure on the surface of a metal hydride, prepared by the method described in claim 1, is used as a nuclear material in the high-temperature operating conditions of nuclear industry or hydrogen storage equipment.

Citation Information

Patent Citations

  • Hydrogen-containing amorphous carbon film with long wear life and preparation method thereof

    CN119465051A

  • Preparation method of aluminum oxide hydrogen-resistant coating on zirconium hydride surface

    CN119913587A