High-pressure-resistant hydrogen embrittlement-resistant metal-rubber composite sealing material and preparation method thereof

Abstract

The application belongs to the field of sealing materials, and discloses a high-pressure-resistant hydrogen embrittlement-resistant metal-rubber composite sealing material and a preparation method thereof. The high-pressure-resistant hydrogen embrittlement-resistant metal-rubber composite sealing material comprises, from bottom to top, a titanium alloy base material, a titanium oxide layer generated in situ on the surface of the titanium alloy base material, and a rubber layer bonded to the surface of the titanium oxide layer through hot pressing treatment. The application also discloses a preparation method of the high-pressure-resistant hydrogen embrittlement-resistant metal-rubber composite sealing material. By constructing a hydrogen-inhibiting oxidation layer and combining surface roughening, laser irradiation treatment and hot pressing treatment, a metal-rubber composite sealing material that can maintain stable deformation and is resistant to hydrogen embrittlement in a high-pressure environment is obtained. After the high-pressure-resistant hydrogen embrittlement-resistant metal-rubber sealing material is kept in a 100MPa high-pressure hydrogen environment for 1000 hours, the tensile strength retention rate is greater than or equal to 88%, the elongation retention rate after breaking is greater than or equal to 80%, and the deformation amount is less than or equal to 0.5%.

Description

Technical Field

[0001] This invention belongs to the field of sealing material technology, and particularly relates to a high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material and its preparation method. Background Technology

[0002] With the continuous development of sealing technology under high pressure, the combination of metal and rubber materials has become an important way to solve sealing problems. Metal materials, due to their excellent mechanical strength and high-temperature resistance, are widely used in high-pressure environments; for example, titanium alloys and aluminum alloys play an important role in various pressure seals. While metal materials can withstand high pressures, they are prone to hydrogen embrittlement in harsh environments such as hydrogen permeation, leading to a decrease in mechanical strength and affecting sealing performance. Therefore, to address the problems of metal materials in high-pressure hydrogen environments, researchers have gradually introduced rubber materials. Rubber materials possess good sealing properties, flexibility, and corrosion resistance, effectively filling gaps between metals and ensuring the integrity of the seal. Materials such as hydrogenated nitrile rubber and fluororubber remain stable under high temperature and pressure conditions and are widely used in various seals. To compensate for the shortcomings of both metals and rubber, metal-rubber composites have emerged. These composites combine the advantages of both metals and rubber, maintaining good sealing performance under high pressure. Oxidation treatment enhances the hydrogen embrittlement resistance of the metal layer, improving the durability of the composite material in extreme environments. Although composite materials have strong resistance to high pressure and permeation, existing technologies have not yet fully solved the challenges of high-pressure hydrogen environments.

[0003] The core deficiency of existing metal-rubber composite sealing materials lies in their insufficient ability to suppress hydrogen embrittlement. While oxidation treatment of the metal surface can improve its resistance to hydrogen embrittlement to some extent, current oxide layer treatment technologies cannot completely solve the problem of hydrogen permeation. Under high temperature and pressure environments, the stability and durability of the oxide layer are difficult to maintain long-term. This means that even under prolonged high-pressure hydrogen environments, the metal layer may still experience hydrogen embrittlement, affecting the overall performance and sealing effect of the material. Hydrogen embrittlement reduces the toughness and strength of the metal layer, leading to seal failure and, in severe cases, potential safety hazards to equipment. Therefore, current technologies have failed to effectively suppress hydrogen embrittlement, and the stability and reliability of metal-rubber composite sealing materials in extreme high-pressure hydrogen environments remain significantly inadequate. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies and defects mentioned in the background art above, and to provide a high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material and its preparation method. By constructing an anti-hydrogen hydroxide layer and combining surface roughening, laser irradiation treatment and hot pressing treatment, a metal-rubber composite sealing material that can maintain stable deformation and resist hydrogen embrittlement in a high-pressure environment is obtained.

[0005] To solve the above-mentioned technical problems, the technical solution proposed by this invention is as follows:

[0006] A high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material, comprising layers stacked sequentially from bottom to top:

[0007] Titanium alloy substrate;

[0008] A titanium oxide layer is formed in situ on the surface of the titanium alloy substrate;

[0009] The rubber layer is bonded to the surface of the titanium oxide layer by hot pressing.

[0010] In the aforementioned high-pressure resistant and hydrogen-embrittlement-resistant metal-rubber composite sealing material, preferably, the thickness of the titanium alloy substrate is 0.1mm-5mm, the thickness of the titanium oxide layer is 0.1μm-2μm, and the thickness of the rubber layer is 0.05mm-2mm. The titanium oxide layer can inhibit hydrogen permeation and remain stable under high temperature and high pressure environments.

[0011] In the aforementioned high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material, preferably, the titanium alloy substrate comprises, by mass percentage: 5%-7% aluminum, 3%-5% vanadium, with the balance being titanium and unavoidable impurities, and the total content of unavoidable impurities being ≤0.5%; the rubber layer is made of hydrogenated nitrile rubber.

[0012] Preferably, the high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material described above, after being kept in a 100MPa high-pressure hydrogen environment for 1000h, has a tensile strength retention rate of ≥88%, an elongation at break retention rate of ≥80%, and a deformation of ≤0.5%.

[0013] As a general inventive concept, the present invention also provides a method for preparing the high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material as described above, comprising the following steps:

[0014] (1) Provide a titanium alloy sheet as a substrate and perform surface treatment on the surface of the titanium alloy sheet;

[0015] (2) The titanium alloy plate after step (1) is subjected to chemical oxidation treatment to form a titanium oxide layer on its surface in situ;

[0016] (3) Cover the surface of the titanium oxide layer formed in step (2) with uncured rubber sheet, and then perform pre-curing and hot pressing treatment in sequence to firmly bond the rubber sheet to the titanium oxide layer, thereby obtaining the high pressure resistant and hydrogen embrittlement resistant metal rubber composite sealing material.

[0017] In the above preparation method, preferably, in step (1), the surface treatment includes cleaning, roughening and laser irradiation. The roughening is achieved by sandblasting. The alumina abrasive used in the sandblasting has a particle size of 120 mesh. The surface roughness Ra of the titanium alloy plate after roughening is 1.5μm-2.5μm. The power of the laser irradiation is 50W-200W and the wavelength is 1064nm.

[0018] In the above preparation method, preferably, in step (2), the chemical oxidation treatment specifically includes: immersing the titanium alloy plate in a hydrogen peroxide solution at a temperature of 50℃-70℃ for 20min-60min, and the concentration of the hydrogen peroxide solution is 5wt%-10wt%.

[0019] The chemical equation for the chemical oxidation treatment is:

[0020] .

[0021] In the above preparation method, preferably, in step (2), the pre-curing conditions include: temperature of 150℃-250℃, pressure of 0.15MPa-0.3MPa, and processing time of 24h.

[0022] In the above preparation method, preferably, in step (3), the hot pressing conditions include a temperature of 180℃-220℃, a pressure of 10MPa-20MPa, and a holding time of 30min-60min.

[0023] In the above preparation method, preferably, in step (3), the rubber sheet is hydrogenated nitrile rubber.

[0024] This invention selects titanium alloy as the base material, which has excellent resistance to hydrogen embrittlement. It can prevent material embrittlement in high-hydrogen environments, thereby extending service life and improving the reliability of the sealing material. The in-situ generated titanium oxide layer not only effectively isolates hydrogen permeation and prevents hydrogen from corroding the metal layer, but also maintains structural stability under high temperature and high pressure environments, ensuring long-term stable operation of the material. Hot-pressing bonding of the rubber layer to the base material gives the material excellent deformation resistance under high pressure, maintaining good sealing performance at 100 MPa, meeting high-pressure sealing requirements. Simultaneously, the rubber layer uses hydrogenated nitrile rubber, which has excellent temperature resistance, ensuring no softening or performance degradation at high temperatures. Heat treatment improves the stability of the composite material, ensuring that the material performance does not change significantly under prolonged high pressure environments, further enhancing the service life of the sealing material.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0026] (1) This invention effectively blocks the penetration and diffusion of hydrogen atoms into the metal interior in a high-pressure hydrogen environment by constructing a dense and stable titanium oxide layer (0.1μm-2μm thick) on the surface of a titanium alloy substrate, thus fundamentally inhibiting the occurrence of hydrogen embrittlement. The oxide layer works synergistically with the optimized titanium alloy substrate (containing 5%~7% aluminum and 3%~5% vanadium) to significantly improve the stability of the material in an extreme high-pressure hydrogen environment, extend its service life, and effectively improve the sealing effect, enabling the composite material to withstand more than 1000 hours of continuous high-pressure load without experiencing sealing failure caused by hydrogen embrittlement.

[0027] (2) Through pre-curing and hot pressing, the present invention forms a high-strength, defect-free interface bond between the substrate and the hydrogenated nitrile rubber layer. After the composite material is kept in a 1000MPa high-pressure hydrogen environment for 1000h, the tensile strength retention rate is ≥88%, the elongation after fracture retention rate is ≥80%, and it exhibits extremely low deformation (≤0.5%), ensuring the tightness of the sealing interface and the long-term stability of the sealing performance under long-term dynamic or static high-pressure conditions, and eliminating the risk of leakage caused by material deformation.

[0028] (3) The present invention employs a comprehensive surface treatment technology, including laser irradiation, to clean, activate and micro-roughen the surface of the titanium oxide layer. Without compromising its resistance to hydrogen permeation, it greatly improves the bonding strength and interface integrity between the rubber and the titanium alloy substrate. Attached Figure Description

[0029] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0030] Figure 1 This is a schematic diagram of the preparation process of the metal-rubber composite sealing material of the present invention. Detailed Implementation

[0031] To facilitate understanding of the present invention, the present invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of protection of the present invention is not limited to the following specific embodiments.

[0032] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0033] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.

[0034] Example 1:

[0035] A high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material of the present invention comprises, from bottom to top, the following layers stacked sequentially: a titanium alloy substrate; a titanium oxide layer formed in situ on the surface of the titanium alloy substrate; and a rubber layer bonded to the surface of the titanium oxide layer by hot pressing. The titanium alloy substrate has a thickness of 5 mm, the titanium oxide layer has a thickness of 2 μm, and the rubber layer has a thickness of 2 mm. The titanium alloy substrate comprises, by mass percentage: 7% aluminum, 5% vanadium, with the balance being titanium and unavoidable impurities, and the total content of unavoidable impurities ≤ 0.5%. The rubber layer is made of hydrogenated nitrile rubber, with a temperature resistance range ≥ 200℃ and a tensile strength ≥ 15 MPa.

[0036] The process flow diagram of the preparation method of the high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material in this embodiment is as follows: Figure 1 As shown, it includes the following steps:

[0037] (1) Provide a titanium alloy plate with a thickness of 5 mm (in terms of mass percentage, it includes: 7% aluminum, 5% vanadium, and the balance is titanium and unavoidable impurities, and the total content of unavoidable impurities is ≤0.5%) as the substrate, and perform surface treatment on the titanium alloy plate. The surface treatment includes cleaning, roughening and laser irradiation. The roughening is done by sandblasting. The alumina abrasive used in sandblasting has a particle size of 120 mesh, and the surface roughness Ra of the roughened surface is 2.5 μm. The power of the laser irradiation is 200 W and the wavelength is 1064 nm.

[0038] (2) The titanium alloy plate after step (1) is subjected to chemical oxidation treatment to form a titanium oxide layer with a thickness of 2 μm on its surface. The specific chemical oxidation treatment includes: immersing the titanium alloy plate in hydrogen peroxide solution at a temperature of 70°C for 60 min, and the concentration of hydrogen peroxide solution is 10 wt%.

[0039] (3) Cover the surface of the titanium oxide layer formed in step (2) with uncured hydrogenated nitrile rubber sheet and pre-cur it. The pre-curing conditions are 250°C, 0.3MPa, and 24h.

[0040] (4) The pre-cured rubber sheet after step (3) is firmly bonded to the titanium oxide layer by hot pressing to obtain a high-pressure resistant and hydrogen embrittlement resistant metal rubber composite sealing material. The hot pressing temperature is 220℃, the pressure is 20MPa, and the holding time is 60min.

[0041] This embodiment utilizes a composite material consisting of a 7% aluminum and 5% vanadium metal substrate layer, a 2µm thick titanium oxide layer, and a 2mm thick rubber layer to prepare a high-pressure resistant and hydrogen-embrittlement-resistant metal-rubber composite sealing material. This material exhibits excellent resistance to hydrogen embrittlement and high-temperature performance. After being exposed to 1000 hours of 100MPa high-pressure hydrogen gas, the tensile strength retention rate was 92%, and the elongation at break retention rate was 85%. Under these conditions, the high-pressure resistant and hydrogen-embrittlement-resistant metal-rubber composite sealing material did not fail and maintained good sealing performance. Specific test data are as follows: the initial tensile strength was 25MPa; after 1000 hours of high-pressure hydrogen exposure, the strength retained was 23MPa, with a tensile strength retention rate of 92%. The initial elongation at break was 150%, and after 1000 hours of high-pressure hydrogen exposure, the elongation at break retained was 127.5%, with an elongation at break retention rate of 85%. This demonstrates that the material exhibits excellent sealing performance under prolonged high-pressure conditions, making it suitable for sealing applications in high-temperature and high-pressure hydrogen environments, effectively extending equipment lifespan and improving equipment safety and stability.

[0042] Example 2:

[0043] A high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material of the present invention comprises, from bottom to top, the following layers stacked sequentially: a titanium alloy substrate; a titanium oxide layer formed in situ on the surface of the titanium alloy substrate; and a rubber layer bonded to the surface of the titanium oxide layer by hot pressing. The titanium alloy substrate has a thickness of 0.1 mm, the titanium oxide layer has a thickness of 0.1 μm, and the rubber layer has a thickness of 0.05 mm. The titanium alloy substrate comprises, by mass percentage: 5% aluminum, 3% vanadium, with the balance being titanium and unavoidable impurities, and the total content of unavoidable impurities ≤ 0.5%. The rubber layer is made of hydrogenated nitrile rubber, with a temperature resistance range ≥ 200℃ and a tensile strength ≥ 15 MPa.

[0044] The process flow diagram of the preparation method of the high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material in this embodiment is as follows: Figure 1 As shown, it includes the following steps:

[0045] (1) Provide a titanium alloy plate with a thickness of 0.1 mm (in terms of mass percentage, it includes: 5% aluminum, 3% vanadium, and the balance is titanium and unavoidable impurities, and the total content of unavoidable impurities is ≤0.5%) as the substrate, and perform surface treatment on the titanium alloy plate. The surface treatment includes cleaning, roughening and laser irradiation. The roughening is done by sandblasting. The alumina abrasive used in sandblasting has a particle size of 120 mesh, and the surface roughness Ra of the roughened surface is 1.5 μm. The power of the laser irradiation is 50 W and the wavelength is 1064 nm.

[0046] (2) The titanium alloy plate after step (1) is subjected to chemical oxidation treatment to form a titanium oxide layer with a thickness of 0.1 μm on its surface. The specific chemical oxidation treatment includes: immersing the titanium alloy plate in hydrogen peroxide solution at a temperature of 50°C for 20 min, and the concentration of hydrogen peroxide solution is 5 wt%.

[0047] (3) Cover the surface of the titanium oxide layer formed in step (2) with uncured hydrogenated nitrile rubber sheet and pre-cur it. The pre-curing conditions are: temperature 150°C, pressure 0.15 MPa, and treatment time 24 h.

[0048] (4) The pre-cured rubber sheet after step (3) is firmly bonded to the titanium oxide layer by hot pressing to obtain a high-pressure resistant and hydrogen embrittlement resistant metal rubber composite sealing material. The hot pressing conditions are 180℃, 10MPa, and 30min.

[0049] Example 3:

[0050] A high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material of the present invention comprises, from bottom to top, the following layers stacked sequentially: a titanium alloy substrate; a titanium oxide layer formed in situ on the surface of the titanium alloy substrate; and a rubber layer bonded to the surface of the titanium oxide layer by hot pressing. The titanium alloy substrate has a thickness of 2.55 mm, the titanium oxide layer has a thickness of 1.05 μm, and the rubber layer has a thickness of 1.025 mm. The titanium alloy substrate comprises, by mass percentage: 6% aluminum, 4% vanadium, with the balance being titanium and unavoidable impurities, and the total content of unavoidable impurities ≤ 0.5%. The rubber layer is made of hydrogenated nitrile rubber, with a temperature resistance range ≥ 200℃ and a tensile strength ≥ 15 MPa.

[0051] The process flow diagram of the preparation method of the high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material in this embodiment is as follows: Figure 1 As shown, it includes the following steps:

[0052] (1) Provide a titanium alloy plate with a thickness of 2.55mm (in terms of mass percentage, it includes: 6% aluminum, 4% vanadium, and the balance is titanium and unavoidable impurities, and the total content of unavoidable impurities is ≤0.5%) as the substrate, and perform surface treatment on the titanium alloy plate. The surface treatment includes cleaning, roughening and laser irradiation. The roughening is done by sandblasting. The alumina abrasive used in sandblasting has a particle size of 120 mesh, and the surface roughness Ra of the roughened surface is 2.0μm. The power of the laser irradiation is 125W and the wavelength is 1064nm.

[0053] (2) The titanium alloy plate after step (1) is subjected to chemical oxidation treatment to form a titanium oxide layer with a thickness of 1.05 μm on its surface. The specific chemical oxidation treatment includes: immersing the titanium alloy plate in hydrogen peroxide solution at a temperature of 60°C for 40 min, and the concentration of hydrogen peroxide solution is 7 wt%.

[0054] (3) Cover the surface of the titanium oxide layer formed in step (2) with uncured hydrogenated nitrile rubber sheet and pre-cur it. The pre-curing conditions are 200°C, 0.225MPa, and 24h.

[0055] (4) The pre-cured rubber sheet from step (3) is firmly bonded to the titanium oxide layer by hot pressing to obtain a high-pressure resistant and hydrogen embrittlement resistant metal-rubber composite sealing material. The hot pressing conditions are 200℃, 15MPa, and 45min.

[0056] Comparative Example 1:

[0057] Compared with Example 1, this comparative example does not introduce a titanium oxide layer. Instead, it directly uses a titanium alloy substrate and a hydrogenated nitrile rubber layer for hot pressing and bonding, without undergoing the chemical oxidation treatment in step (2). Other processes and parameters are the same as in Example 1.

[0058] Comparative Example 2:

[0059] Compared with Example 1, the surface treatment method of this comparative example does not use laser irradiation treatment, but other processes and parameters are the same as those of Example 1.

[0060] Comparative Example 3:

[0061] Compared with Example 1, this comparative example omits the laser irradiation treatment in step (1) and the chemical oxidation treatment in step (2). Uncured hydrogenated nitrile rubber sheet is directly applied to the surface of the titanium alloy plate after sandblasting roughening and cleaning, and then the same pre-curing and hot pressing treatment as in Example 1 is performed.

[0062] Table 1: Comparison of Performance of High-Pressure Resistant and Hydrogen Embrittlement Resistant Metal-Rubber Composite Sealing Materials

[0063]

[0064] The performance indicators expressed as percentages in Table 1 are all results converted from the original test values ​​obtained based on the corresponding standards. The specific testing and conversion process is as follows:

[0065] 1. Tensile strength retention rate (%): The tensile strength σ0 before exposure and the tensile strength σ1 after exposure (unit: MPa) were measured according to GB / T528-2009, and calculated according to formula (1):

[0066] Equation (1) Tensile strength retention rate (%) = (σ1 / σ0) × 100%.

[0067] 2. Elongation retention rate after fracture (%): The elongation before fracture ε0 and the elongation after fracture ε1 after exposure were measured according to GB / T528-2009 (unit: %), and calculated according to formula (2):

[0068] Equation (2) Elongation retention rate after fracture (%) = (ε1 / ε0) × 100%.

[0069] 3. Deformation (%): Measured according to ASTM D395-14 and expressed as compressive permanent deformation rate. Using the constant deformation method, the initial thickness t0 of the specimen, the final thickness ti after the specified recovery time after the test, and the thickness tn of the limiting shim or spacer (units consistent) are calculated according to formula (3):

[0070] Formula (3) Compression permanent deformation rate CB (%) = [(t0) ti) / (t0 tn)]×100%.

[0071] 4. Hydrogen permeability resistance (%): The hydrogen permeability parameter (denoted as GTR, with unit) is determined according to ISO 15105-1. Under the same sample thickness, temperature and pressure difference conditions, the permeability GTRref of the control sample and the permeability GTRs of the test sample are converted into hydrogen permeability resistance according to formula (4):

[0072] Formula (4) Hydrogen permeability resistance (%) = [1 (GTRs / GTRref)]×100%.

[0073] 5. Hardness: Measured according to ASTM D2240-05 and expressed directly as Shore hardness value, without conversion.

[0074] 6. Pressure resistance test (MPa@h): The pressure resistance result is expressed as the pressure level corresponding to the sample meeting the integrity criteria after being continuously pressurized in a high-pressure hydrogen environment for a specified time (e.g., 1000h).

[0075] As can be seen from the experimental data in Table 1, Example 1 exhibits excellent performance in terms of tensile strength retention (92%) and elongation at break retention (85%), with a deformation of only 0.4%, demonstrating the material's stability in a high-pressure hydrogen environment. Compared to Comparative Example 3, which lacks a titanium oxide layer, the performance of Comparative Example 3 is significantly reduced, with both tensile strength retention and elongation at break retention decreasing to 60%. This indicates that the titanium oxide layer formation technology effectively enhances the material's resistance to hydrogen embrittlement and high pressure, improving its sealing effect and resistance to hydrogen permeation.

[0076] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material, characterized in that, The high-pressure resistant and hydrogen-embrittlement-resistant metal-rubber composite sealing material, after being kept in a 100MPa high-pressure hydrogen environment for 1000 hours, exhibits a tensile strength retention rate ≥88%, an elongation at break retention rate ≥80%, and a deformation ≤0.5%; the high-pressure resistant and hydrogen-embrittlement-resistant metal-rubber composite sealing material comprises layers stacked sequentially from bottom to top: The titanium alloy substrate comprises, by weight percentage: 5%-7% aluminum, 3%-5% vanadium, with the balance being titanium and unavoidable impurities, and the total content of unavoidable impurities being ≤0.5%. A titanium oxide layer is formed in situ on the surface of the titanium alloy substrate; the titanium oxide layer is formed in situ by immersing the titanium alloy substrate in a hydrogen peroxide solution at 50-70°C for 20-60 minutes. A rubber layer is bonded to the surface of the titanium oxide layer by hot pressing; the material of the rubber layer is hydrogenated nitrile rubber. Before the rubber layer is hot-pressed, pre-curing and hot-pressing are performed sequentially. The pre-curing is carried out at a temperature of 150℃-250℃ and a pressure of 0.15MPa-0.3MPa for 24 hours.

2. The high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material as described in claim 1, characterized in that, The thickness of the titanium alloy substrate is 0.1mm-5mm, the thickness of the titanium oxide layer is 0.1μm-2μm, and the thickness of the rubber layer is 0.05mm-2mm.

3. A method for preparing a high-pressure resistant and hydrogen embrittlement-resistant metal-rubber composite sealing material as described in any one of claims 1 to 2, characterized in that, Includes the following steps: (1) Provide a titanium alloy sheet as a titanium alloy substrate, and perform surface treatment on the surface of the titanium alloy sheet; (2) The titanium alloy plate after step (1) is subjected to chemical oxidation treatment to form a titanium oxide layer on its surface in situ; (3) Cover the surface of the titanium oxide layer formed in step (2) with uncured rubber sheet, and then perform pre-curing and hot pressing treatment in sequence to obtain the high pressure resistant and hydrogen embrittlement resistant metal rubber composite sealing material.

4. The preparation method according to claim 3, characterized in that, In step (1), the surface treatment includes cleaning, roughening and laser irradiation. The roughening is achieved by sandblasting. The alumina abrasive used in the sandblasting has a particle size of 120 mesh. The surface roughness Ra of the titanium alloy plate after roughening is 1.5μm-2.5μm. The laser irradiation has a power of 50W-200W and a wavelength of 1064nm.

5. The preparation method according to claim 3, characterized in that, In step (2), the chemical oxidation treatment specifically includes: immersing the titanium alloy plate in a hydrogen peroxide solution at a temperature of 50℃-70℃ for 20min-60min, wherein the concentration of the hydrogen peroxide solution is 5wt%-10wt%.

6. The preparation method according to claim 3, characterized in that, In step (3), the conditions for hot pressing include a temperature of 180℃-220℃, a pressure of 10MPa-20MPa, and a holding time of 30min-60min.

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