Metal material with high hydrogen embrittlement resistance and preparation method thereof

Abstract

The invention discloses a metal material with high hydrogen embrittlement resistance and a preparation method thereof. The preparation method comprises the following steps that (1) the surface of a metal sample is pretreated; (2) putting the metal sample into a tubular furnace, and carrying out gas washing on the surface of the metal sample; 3) heating the metal sample to 500-1000 DEG C through a tubular furnace; (4) after the temperature in the tubular furnace reaches the target temperature, mixed gas of oxygen and argon is introduced into the tubular furnace, heat preservation is conducted for 0.5-48 h, and meanwhile the air pressure in the furnace is kept stable; (5) the metal sample is cooled to the room temperature, and the metal material with the high hydrogen embrittlement resistance is obtained.The metal material prepared through the method can effectively inhibit hydrogen absorption and hydrogen diffusion on the metal surface, and the hydrogen embrittlement resistance of the metal material is remarkably improved.

Description

Technical Field

[0001] The present invention belongs to the field of metal materials and relates to a metal material with high hydrogen embrittlement resistance and a preparation method thereof. Background Art

[0002] The problem of hydrogen embrittlement in metals is regarded as one of the most challenging century-old problems in materials science due to its characteristics such as instantaneous suddenness and unpredictability. Every year, globally, catastrophic accidents caused by hydrogen embrittlement are not uncommon, and hydrogen embrittlement has also become a major threat to the service safety of key structural components of metal materials. Metals in the fourth subgroup, such as titanium, zirconium, and their alloys, as high-performance structural materials, play important roles in many key industrial fields including nuclear reactors, aerospace, deep sea, and biomedicine.

[0003] Titanium and titanium alloys are very active and very prone to hydrogen absorption. When the hydrogen content in titanium reaches 0.008 - 0.015%, the precipitation of needle-like hydride phases can be observed. With the further increase of the hydrogen content, the number and volume of hydrides will also increase accordingly. The hydrogen embrittlement sensitivity of titanium is similar to pitting corrosion, and the surface pretreatment state has a great influence on it. The surface of anodized or thermally oxidized has the strongest ability to resist hydrogen absorption and hydrogen embrittlement, followed by pickled or annealed surfaces, while mechanically polished or sandblasted surfaces have the worst ability to resist hydrogen absorption and hydrogen embrittlement. Hydrogen absorption in titanium usually occurs in a hydrogen atmosphere or a hydrogen-containing atmosphere at high temperature (>300°C), as well as in a hydrogen environment generated during crevice corrosion, reduction inorganic acid corrosion, galvanic corrosion, or cathodic protection. Similar to titanium, zirconium and its alloys also have a high affinity for hydrogen. Although the solubility of hydrogen in zirconium at room temperature is extremely low (less than 1 wppm), during production, processing, and long-term service, zirconium alloys will inevitably absorb hydrogen from the environment, resulting in the precipitation of a large number of brittle hydrides. The precipitation of these hydrides significantly increases the ductile-brittle transition temperature of zirconium alloys, triggering various local brittle phenomena. In the nuclear industry, zirconium alloys are often used as the fuel cladding tubes and pressure tubes of pressurized water reactors, so their hydrogen embrittlement problem poses a potential threat to the safe operation of nuclear reactors. To mitigate the hydrogen embrittlement problem of zirconium alloys, it is necessary to strictly control the hydrogen content during their production process. This includes measures such as using vacuum melting, avoiding reducing atmospheres, and welding under inert gas or vacuum protection. In addition, the hydrogen embrittlement resistance of zirconium alloys can also be improved through alloying design. For example, adding certain alloying elements can form a dispersed second phase, which serves as an irreversible trap for hydrogen, reducing the content of mobile hydrogen in the material, thereby reducing the hydrogen embrittlement tendency.

[0004] Previously, many attempts have been made to form a hydrogen diffusion barrier layer on the surface of metal materials by means of atmospheric oxidation treatment to achieve the purpose of suppressing hydrogen embrittlement of the materials. However, the oxide film with a nanoscale thickness formed on the metal surface by atmospheric oxidation is extremely prone to damage or peeling during the assembly or service process of metal components, greatly weakening the inhibitory effect of the oxide film on hydrogen absorption and diffusion. Summary of the Invention

[0005] The purpose of the present invention is to overcome the above-mentioned shortcomings of the prior art, and provide a metal material with high hydrogen embrittlement resistance and a preparation method thereof. The metal material prepared by this method can effectively inhibit hydrogen absorption and hydrogen diffusion on the metal surface, and significantly improve the hydrogen embrittlement resistance of the metal material.

[0006] To achieve the above purpose, the present invention discloses a preparation method of a metal material with high hydrogen embrittlement resistance, including the following steps:

[0007] 1) Pretreat the surface of the metal sample;

[0008] 2) Place the metal sample in a tube furnace and purge the surface of the metal sample;

[0009] 3) Heat the metal sample to 500 - 1000 °C through the tube furnace;

[0010] 4) After the temperature in the tube furnace reaches the target temperature, introduce a mixed gas of oxygen and argon into the tube furnace, then keep it warm for 0.5 - 48 h while keeping the gas pressure in the furnace stable;

[0011] 5) Cool the metal sample to room temperature to obtain a metal material with high hydrogen embrittlement resistance.

[0012] A further improvement of the preparation method of the metal material with high hydrogen embrittlement resistance according to the present invention lies in:

[0013] Further, the operation process of step 1) is:

[0014] Sand the surface of the metal sample until a smooth metal surface is exposed, then ultrasonically clean it in an alcohol solution, and then suspend it in a crucible using a bracket so that the surface of the metal sample evenly contacts the air flow.

[0015] Further, the operation process of step 2) is:

[0016] Send the crucible into the tube furnace chamber, turn on the mechanical pump to pump out the air in the tube furnace chamber, and introduce argon.

[0017] Further, the operation process of step 5) is:

[0018] Cool the metal sample to room temperature by means of air cooling or water quenching to obtain a metal material with high hydrogen embrittlement resistance.

[0019] Further, the heat preservation temperature in step 4) is 500 - 1000 °C.

[0020] Further, in step 4), a mixed gas of 5 vol.% oxygen and argon is introduced into the tubular furnace, and the air pressure in the furnace is controlled to be 400 Pa.

[0021] Further, the metal sample is made of titanium, titanium alloy, zirconium or zirconium alloy.

[0022] The present invention discloses a metal material with high hydrogen embrittlement resistance, which is prepared based on the preparation method of the metal material with high hydrogen embrittlement resistance. The preparation method of the metal material with high hydrogen embrittlement resistance includes the following steps: 1) Pretreat the surface of the metal sample; 2) Place the metal sample in a tubular furnace and wash the surface of the metal sample; 3) Heat the metal sample to 500 - 1000 °C through the tubular furnace; 4) After the temperature in the tubular furnace reaches the target temperature, introduce a mixed gas of oxygen and argon into the tubular furnace, then keep it warm for 0.5 - 48 h while keeping the air pressure in the furnace stable; 5) Cool the metal sample to room temperature to obtain a metal material with high hydrogen embrittlement resistance.

[0023] A further improvement of the metal material with high hydrogen embrittlement resistance according to the present invention lies in:

[0024] Further, an oxide film with a thickness of 0.5 - 30 μm is formed on the surface of the metal material with high hydrogen embrittlement resistance.

[0025] Further, an oxygen permeation zone with a depth of 1 - 200 μm is formed inside the metal material with high hydrogen embrittlement resistance.

[0026] The present invention has the following beneficial effects:

[0027] When the metal material with high hydrogen embrittlement resistance and its preparation method according to the present invention are specifically operated, without changing the metal or alloy composition, only by the high-temperature oxygen permeation process, a gradient structure of an oxide film + oxygen permeation layer is formed on the metal surface and subsurface layer, playing a dual role in inhibiting hydrogen absorption and hydrogen diffusion. Especially even if the surface oxide film is damaged, the internal oxygen permeation layer can still play a role in inhibiting hydrogen diffusion, greatly improving the hydrogen embrittlement resistance of the material. At the same time, it has the characteristics of simple preparation process, high production efficiency, low cost, good controllability, extremely strong practicability, and is convenient for popularization and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The specification drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation to the present invention. In the drawings:

[0029] Figure 1 Schematic diagram of the process equipment required for the present invention;

[0030] Figure 2a Cross-sectional microstructure photograph of the pure zirconium sample after oxygen permeation treatment in Example 1;

[0031] Figure 2b Cross-sectional microstructure photograph of the pure zirconium sample after oxygen permeation treatment and electrochemical hydrogen charging treatment in Example 1;

[0032] Figure 3a Cross-sectional microstructure photograph of the zirconium alloy (Zr-2.5Nb) sample after oxygen permeation treatment in Example 2;

[0033] Figure 3b Cross-sectional microstructure photograph of the Zr-2.5Nb sample after oxygen permeation treatment and electrochemical hydrogen charging treatment in Example 2;

[0034] Figure 3c Cross-sectional microstructure photograph of the Zr-2.5Nb sample after oxygen permeation treatment, removing the oxide film, and then electrochemical hydrogen charging treatment in Example 2;

[0035] Figure 4a Cross-sectional microstructure photograph of the pure titanium sample after oxygen permeation treatment in Example 3;

[0036] Figure 4b Cross-sectional microstructure photograph of the pure titanium sample after oxygen permeation treatment and electrochemical hydrogen charging treatment in Example 3. Detailed implementation manners

[0037] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0038] In the description of the present invention, it should be understood that the terms "include" and "comprise" indicate the presence of the described features, wholes, steps, operations, elements, and / or components, but do not exclude the presence or addition of one or more other features, wholes, steps, operations, elements, components, and / or their combinations.

[0039] It should also be understood that the terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the specification of the present invention and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an", and "the" are intended to include the plural forms.

[0040] It should also be further understood that the term "and / or" used in the specification and appended claims of the present invention refers to any combination and all possible combinations of one or more of the associated listed items, and includes these combinations. For example, A and / or B can represent three cases: A exists alone, A and B exist simultaneously, and B exists alone. In addition, in the present invention, the character " / " generally represents an "or" relationship between the associated objects before and after.

[0041] It should be understood that although terms such as first, second, and third may be used in the embodiments of the present invention to describe preset ranges, etc., these preset ranges should not be limited to these terms. These terms are only used to distinguish the preset ranges from each other. For example, without departing from the scope of the embodiments of the present invention, the first preset range may also be referred to as the second preset range, and similarly, the second preset range may also be referred to as the first preset range.

[0042] Depending on the context, the word "if" as used herein can be interpreted as "when" or "while" or "in response to determining" or "in response to detecting". Similarly, depending on the context, the phrase "if determined" or "if detected (stated condition or event)" can be interpreted as "when determined" or "in response to determining" or "when detected (stated condition or event)" or "in response to detecting (stated condition or event)".

[0043] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. Usually, the components of the present invention described and shown in the accompanying drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed present invention, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of protection of the present invention.

[0044] Various structural schematic diagrams according to the disclosed embodiments of the present invention are shown in the drawings. These figures are not drawn to scale, where for the purpose of clear expression, some details are enlarged and some details may be omitted. The shapes of various regions and layers shown in the figures and their relative sizes and positional relationships are only exemplary, and may actually deviate due to manufacturing tolerances or technical limitations, and those skilled in the art can design regions / layers with different shapes, sizes, and relative positions according to actual needs.

[0045] The metal material with high hydrogen embrittlement resistance performance described in the present invention is prepared based on the preparation method of the metal material with high hydrogen embrittlement resistance performance. The preparation method of the metal material with high hydrogen embrittlement resistance performance includes the following steps: 1) Pretreat the surface of the metal sample; 2) Place the metal sample in a tube furnace and purge the surface of the metal sample; 3) Heat the metal sample to 500 - 1000 °C through the tube furnace; 4) After the temperature in the tube furnace reaches the target temperature, introduce a mixed gas of oxygen and argon into the tube furnace, then keep it warm for 0.5 - 48 h while keeping the air pressure in the furnace stable; 5) Cool the metal sample to room temperature to obtain a metal material with high hydrogen embrittlement resistance performance.

[0046] The preparation method of the metal material with high hydrogen embrittlement resistance performance described in the present invention includes the following steps:

[0047] 1) Pretreat the surface of the metal sample;

[0048] Use sandpaper to polish the surface of the metal sample until a smooth metal surface is exposed, then ultrasonically clean it in an alcohol solution, and then suspend it in a quartz crucible using a bracket so that the surface of the metal sample is evenly in contact with the gas flow;

[0049] 2) Purge the surface of the metal sample;

[0050] Put the crucible into the tube furnace chamber, turn on the mechanical pump to pump out the air in the tube furnace chamber, and introduce high-purity argon (Ar);

[0051] 3) Heat the tube furnace to 500 - 1000 °C at a heating rate of 10 °C / min;

[0052] 4) Gradient oxygen infiltration: After the temperature in the tube furnace reaches the target temperature, introduce a mixed gas of oxygen and argon into the tube furnace, then keep it warm for 0.5 - 48 h while keeping the air pressure in the furnace stable by adjusting the mechanical pump;

[0053] 5) Cool the metal sample to room temperature by air cooling or water quenching to obtain a metal material with high hydrogen embrittlement resistance performance.

[0054] In this embodiment, the holding temperature for the gradient oxygen infiltration treatment in step 4) is 500 - 1000 °C, and the holding time is 0.5 - 48 h.

[0055] In this embodiment, in step 4), introduce a mixed gas of 5 vol.% oxygen and argon into the tube furnace and control the air pressure in the furnace to be 400 Pa.

[0056] In this embodiment, the material of the metal sample is titanium, titanium alloy, zirconium or zirconium alloy.

[0057] An oxide film with a thickness of 0.5 - 30 μm is formed on the surface of the metal material with high hydrogen embrittlement resistance, and the component of the oxide film is crystalline oxide.

[0058] An oxygen permeation zone with a depth of 1 - 200 μm is formed inside the metal material with high hydrogen embrittlement resistance.

[0059] Example 1

[0060] The metal material selected in this example is high-purity zirconium, and the length, width, and height of the sample are 10 mm, 10 mm, and 3.5 mm respectively. Refer to Figure 1 , and the equipment required for the preparation process of oxygen permeation on the sample surface includes a tube furnace equipped with a mechanical pump, a flow meter, an Ar gas cylinder, and an O2 / Ar gas cylinder. The specific operation process is as follows:

[0061] 1) Grind the surface of the pure zirconium block sample with sandpapers of 80, 220, 600, 800, 1500, and 3000 meshes respectively, and electro-polish it at liquid nitrogen temperature until a smooth, flat, and stress-free metal surface is exposed. After ultrasonic cleaning in an alcohol solution for 5 min, use a zirconium-niobium alloy bracket to suspend the sample in a quartz crucible so that the metal sample surface uniformly contacts the gas flow;

[0062] 2) Put the crucible into the tube furnace chamber, turn on the mechanical pump to pump out the air in the furnace, and introduce high-purity Ar;

[0063] 3) Heat the tube furnace to 1000 °C at a heating rate of 10 °C / min;

[0064] 4) After the temperature in the tube furnace reaches the preset temperature of 1000 °C, introduce a 5 vol.% O2 / Ar mixed gas into the furnace body, keep it warm for 1 h, and at the same time adjust the mechanical pump to make the air pressure in the furnace stable at 400 Pa;

[0065] 5) After the oxygen permeation treatment is completed, cool the sample to room temperature by water quenching.

[0066] Prepare cross-section samples by wire cutting, and corrode the cross-section of the samples by electrochemical polishing to observe the cross-section microstructure after oxygen permeation treatment. As Figure 2a shown, an oxide film with a thickness of about 20 μm is formed on the surface of the pure zirconium sample, and an oxygen permeation layer with a depth of about 100 μm is formed in the subsurface area inside it.

[0067] Hydrogen charging treatment is carried out on the oxygen-permeated pure zirconium by electrochemical hydrogen charging. The electrolyte is a 0.5 mol / L dilute sulfuric acid solution, and the hydrogen charging time is 24 h. As Figure 2b shown, the oxide film on the surface of the pure zirconium sample has a significant hindering effect on the absorption and diffusion of hydrogen atoms, and no brittle hydride phase is formed inside the sample after hydrogen charging.

[0068] Example 2

[0069] The metal material selected in this example is a zirconium-niobium alloy sample (Zr-2.5Nb), and the length, width, and height of the sample are 10 mm, 7 mm, and 3 mm respectively. Refer to Figure 1 , and the equipment required for the preparation process of surface oxygen permeation of the sample includes a tube furnace equipped with a mechanical pump, a flow meter, and Ar gas cylinders and O2 / Ar gas cylinders. The specific operation process is as follows:

[0070] 1) Grind the surface of the Zr-2.5Nb bulk sample with sandpapers of 80, 220, 600, 800, 1500, and 3000 meshes respectively, and electro-polish it at liquid nitrogen temperature until a smooth, flat, and stress-free metal surface is exposed. After ultrasonic cleaning in an alcohol solution for 5 min, use a zirconium-niobium alloy bracket to suspend the sample in a quartz crucible so that the metal sample surface uniformly contacts the gas flow;

[0071] 2) Place the crucible into the tube furnace chamber, turn on the mechanical pump to pump out the air in the tube furnace, and introduce high-purity Ar;

[0072] 3) Heat the tube furnace to 1000 °C at a heating rate of 10 °C / min;

[0073] 4) After the temperature in the tube furnace reaches the preset temperature of 1000 °C, introduce a 5 vol.% O2 / Ar mixed gas into the furnace body, keep it warm for 10 min, and at the same time adjust the mechanical pump to make the furnace pressure stable at 400 Pa;

[0074] 5) After the oxygen permeation treatment is completed, cool the sample to room temperature by water quenching.

[0075] Prepare cross-section samples by wire cutting, and corrode the cross-section of the samples by electrochemical polishing to observe the cross-section microstructure after oxygen permeation treatment. As Figure 3a shown, an oxide film with a thickness of about 20 μm is formed on the surface of the Zr-2.5Nb alloy sample, and an oxygen permeation layer with a depth of about 200 μm is formed in the subsurface layer region inside it.

[0076] Perform hydrogen charging treatment on the oxygen-permeated Zr-2.5Nb by electrochemical hydrogen charging. The electrolyte is a 0.5 mol / L dilute sulfuric acid solution, and the hydrogen charging time is 24 h. As Figure 3b shown, the oxide film on the surface of the Zr-2.5Nb sample has a significant hindering effect on the absorption and diffusion of hydrogen atoms, and no brittle hydride phase is formed inside the sample after hydrogen charging.

[0077] Subsequently, grind off the surface oxide film of the oxygen-permeated Zr-2.5Nb sample, only retain the oxygen permeation layer in the subsurface layer, and perform the same electrochemical hydrogen charging treatment on this sample. The hydrogen charging time is 24 h. As Figure 3cAs shown, the oxygen penetration layer inside the Zr-2.5Nb sample also has an inhibitory effect on the absorption and diffusion of hydrogen atoms.

[0078] Example 3

[0079] The metal material selected in this example is a high-purity titanium sample, with the length, width, and height of the sample being 10 mm, 10 mm, and 3 mm respectively. Refer to Figure 1 , and the equipment required for the surface oxygen penetration preparation process of the sample includes a tube furnace equipped with a mechanical pump, a flow meter, and Ar gas cylinders and O2 / Ar gas cylinders. The specific operation process is as follows:

[0080] 1) Polish the surface of the pure titanium block sample with sandpapers of 80, 220, 600, 800, 1500, and 3000 meshes respectively, and electro-polish it at liquid nitrogen temperature until a smooth, flat, and stress-free metal surface is exposed. After ultrasonic cleaning in an alcohol solution for 5 min, use a zirconium niobium alloy bracket to suspend the sample in a quartz crucible so that the metal sample surface is evenly in contact with the gas flow;

[0081] 2) Send the crucible into the tube furnace chamber, turn on the mechanical pump to pump out the air in the furnace, and introduce high-purity Ar;

[0082] 3) Heat the tube furnace to 600 °C at a heating rate of 10 °C / min;

[0083] 4) After the temperature in the tube furnace reaches the preset temperature of 600 °C, introduce a 5 vol.% O2 / Ar mixed gas into the furnace body, keep it warm for 48 h, and at the same time stabilize the furnace pressure at 400 Pa by adjusting the mechanical pump;

[0084] 5) After the oxygen penetration treatment is completed, cool the sample to room temperature by air cooling.

[0085] Prepare a cross-section sample by wire cutting, and corrode the sample cross-section by electrochemical polishing to observe the cross-section structure after oxygen penetration treatment. As Figure 4a shown, an oxide film with a thickness of about 0.9 μm is formed on the surface of the pure titanium sample, and an oxygen penetration layer with a depth of about 3.4 μm is formed in the subsurface region inside it.

[0086] Hydrogenate the oxygen-penetrated pure titanium by electrochemical hydrogen charging. The electrolyte is a 0.5 mol / L dilute sulfuric acid solution, and the hydrogen charging time is 24 h. As Figure 4b shown, the oxide film on the surface of the pure titanium sample has a significant inhibitory effect on the absorption and diffusion of hydrogen atoms, and no brittle hydride phase is formed inside the sample after hydrogen charging.

[0087] Thus, it can be seen that forming a gradient structure of an oxide film + an oxygen penetration layer on the metal surface and inside through a high-temperature oxygen penetration process is an effective method to inhibit the hydrogen absorption of materials and improve their hydrogen embrittlement resistance.

[0088] Other embodiments of the present invention will be readily contemplated by those skilled in the art in view of the specification and the disclosure of the invention. This application is intended to cover any variations, uses, or adaptations of the present invention, which follow the general principles of the present invention and include known common general knowledge or conventional technical means in the technical field not disclosed in the present invention. The specification and the embodiments are only regarded as exemplary, and the true scope and spirit of the present invention are pointed out by the following claims.

[0089] It should be understood that the present invention is not limited to the exact structures already described and shown in the drawings, and various modifications and changes can be made without departing from its scope. The scope of the present invention is only limited by the appended claims.

[0090] The above are only the preferred embodiments of the present invention, and do not impose any limitation on the present invention. Any simple modifications, changes, and equivalent structural changes made to the above embodiments according to the technical essence of the present invention still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for preparing a metal material with high hydrogen embrittlement resistance, characterized in that: The following steps are involved: 1) Pre-treat the surface of the metal sample; 2) placing the metal sample in a tube furnace and washing the surface of the metal sample; 3) heating the metal sample to 500-1000°C in a tube furnace; 4) After the temperature in the tube furnace reaches the target temperature, a mixed gas of oxygen and argon is introduced into the tube furnace, and the temperature is maintained for another 0.5 to 48 hours, while the gas pressure in the furnace is kept stable; 5) Cooling the metal sample to room temperature to obtain a metal material with high resistance to hydrogen embrittlement.

2. The method for preparing a metal material having high hydrogen embrittlement resistance according to claim 1, characterized in that: The operation process of step 1) is: The surface of the metal sample is polished with sandpaper until a smooth metal surface is exposed, and then ultrasonically cleaned in an alcohol solution, and then suspended in the crucible using a bracket to allow the surface of the metal sample to evenly contact the airflow.

3. The method for preparing a metal material having high hydrogen embrittlement resistance according to claim 2, characterized in that: The operation process of step 2) is: Put the crucible into the tubular furnace, turn on the mechanical pump to extract the air in the tubular furnace, and introduce argon gas.

4. The method for preparing a metal material having high hydrogen embrittlement resistance according to claim 2, characterized in that: The operation process of step 5) is: The metal sample is cooled to room temperature by air cooling or water quenching to obtain a metal material with high resistance to hydrogen embrittlement.

5. The method for preparing a metal material having high hydrogen embrittlement resistance according to claim 2, characterized in that: The holding temperature in step 4) is 500-1000°C.

6. The method for preparing a metal material with high hydrogen embrittlement resistance according to claim 2, characterized in that: In step 4), a 5 vol.% mixed gas of oxygen and argon is introduced into the tubular furnace, and the gas pressure in the furnace is controlled to be 400 Pa.

7. The method for preparing a metal material with high hydrogen embrittlement resistance according to claim 2, characterized in that: The material of the metal sample is titanium, titanium alloy, zirconium or zirconium alloy.

8. A metal material with high hydrogen embrittlement resistance, characterized in that: The metal material is prepared based on the preparation method of any one of claims 1 to 7 having high hydrogen embrittlement resistance.

9. The metal material with high hydrogen embrittlement resistance according to claim 8, characterized in that: An oxide film with a thickness of 0.5 to 30 μm is formed on the surface of the metal material with high hydrogen embrittlement resistance.

10. The metal material with high hydrogen embrittlement resistance according to claim 8, characterized in that: An oxygen permeation zone with a depth of 1 to 200 μm is formed inside the metal material with high hydrogen embrittlement resistance.

Images