Hydrogen permeation prevention coating for improving service life of titanium alloy and preparation method thereof
By preparing an Al2O3 and TiO2 hydrogen permeation barrier protective layer on the surface of titanium alloy, the problem of hydrogen permeation in a hydrogen environment of titanium alloy was solved, the fatigue life was improved and the hydrogen resistance was enhanced, and a highly efficient protective effect was achieved.
Patent Information
- Application Number
- CN202411946012.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2044-12-27
AI Technical Summary
Titanium alloys are prone to hydrogen permeation in hydrogen environments, which leads to a decrease in strength, plasticity and fatigue properties, affecting service reliability.
A hydrogen permeation-resistant protective layer was prepared on the surface of a titanium alloy. The outer layer was Al2O3 and the inner layer was TiO2. The layer was formed in situ by vacuum oxygen permeation, which utilized the structural properties of aluminum oxide and titanium dioxide to hinder hydrogen diffusion.
It improves the fatigue life of titanium alloys, prevents hydrogen permeation, enhances the hydrogen resistance of materials, and is low in cost, highly efficient in production, and has a uniform protective layer distribution.
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Figure CN119824360B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of metal material surface protection, and particularly relates to a hydrogen permeation resistance protective layer for improving the service life of titanium alloy and a preparation method thereof. BACKGROUND
[0002] Titanium alloy has a density of about 60% of steel and a high specific strength, and is suitable for manufacturing parts with high strength and good rigidity. However, hydrogen atoms have a small radius and a high diffusion rate in a crystal lattice, and are particularly prone to gathering along a crystal dislocation and an interface to generate a brittle hydride, thereby suddenly reducing the strength, plasticity, toughness and fatigue performance of the titanium alloy and endangering the service reliability of a structure prepared therefrom.
[0003] The vacancy hydrogen trap, micro-nano pores and water and aluminum oxide compounds generated by hydrogen reaction in the Al2O3 structure hinder the movement of hydrogen molecules and effectively hinder the diffusion of hydrogen and slow down the hydrogen permeation speed. Meanwhile, hydrogen atoms are prone to occupying the octahedral interstitial position of TiO2 oxygen atoms and forming an OH bond with the nearest oxygen atoms. Therefore, the surface oxide layer with the outer layer of Al2O3 and the inner layer of TiO2 can effectively hinder hydrogen from permeating into the matrix, and the Ti atoms doped into the aluminum oxide at the interface can hinder the diffusion and gathering of hydrogen by forming insoluble stable hydride TiH, thereby improving the hydrogen permeation resistance of the material. SUMMARY
[0004] The application aims to provide a hydrogen permeation resistance protective layer for improving the service life of titanium alloy and a preparation method thereof, which can improve the fatigue life of the titanium alloy under a hydrogen environment.
[0005] In order to achieve the above-mentioned purpose, the application adopts the following technical scheme:
[0006] A preparation method of a hydrogen permeation resistance protective layer for improving the service life of titanium alloy, specifically comprising the following steps:
[0007] Step 1, mixed gas: open the gas source, and let the oxygen and argon pass through the mixing device according to the set ratio to realize accurate mixing, and use a sensor to monitor the concentration of the mixed gas, wherein the argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%;
[0008] Step 2, titanium alloy selection: the titanium alloy matrix needs to contain aluminum elements, and a metastable beta type titanium alloy with a nominal composition of Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy is less than 5ppm;
[0009] Step 3, hydrogen barrier layer preparation: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace, argon is first introduced, the vacuum pump is used to vacuumize to 8 Pa, then the temperature of the vacuum furnace is increased to the oxygenation temperature, the vacuum pump is closed after 1.5 h, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace, the pressure in the vacuum furnace is 0.023 MPa, at this time the pressure in the vacuum furnace is lower than the standard atmospheric pressure, the oxygenation process is carried out, the oxygenation temperature is 300-600 DEG C, the oxygenation process is 1-24 h, and the hydrogen barrier layer is prepared on the surface of the titanium alloy, the outer layer of the hydrogen barrier layer is Al2O3, the inner layer is TiO2, and the Ti and Al elements in the hydrogen barrier layer come from the inside of the titanium alloy, and the O element comes from the oxygen and argon mixed gas in the vacuum furnace.
[0010] Further, in step 1, the content of oxygen and argon is: argon is 80-95%, and oxygen is 5-20%.
[0011] Compared with the prior art, the present application has the following beneficial effects:
[0012] The preparation method of the hydrogen barrier layer for improving the service life of the titanium alloy provided by the present application uses different mixed oxygen and argon as the oxygenation condition, in-situ diffusion forms the hydrogen barrier layer on the titanium alloy substrate, does not need to add titanium and aluminum alloy elements, has low cost, high product production efficiency, the prepared hydrogen barrier layer is uniformly distributed, has good plasticity, satisfies that the alloy bending fatigue behavior does not break, and has the effect of hindering hydrogen diffusion and penetration. BRIEF DESCRIPTION OF DRAWINGS
[0013] Figure 1 is the morphology diagram of the hydrogen barrier layer and the titanium alloy substrate prepared in embodiment 1 of the present application;
[0014] Figure 2 is the morphology diagram of the hydrogen barrier layer oxide prepared in embodiment 4 of the present application. DETAILED DESCRIPTION
[0015] The present application will be described in detail below in combination with the drawings and specific embodiments.
[0016] The preparation method of the hydrogen barrier layer for improving the service life of the titanium alloy, specifically includes the following steps:
[0017] Step 1, mixed gas: the gas source is opened, and oxygen and argon are mixed according to the set ratio through the mixing device to realize accurate mixing, the content of oxygen and argon is: argon is 80-95%, and oxygen is 5-20%, the concentration of the mixed gas is monitored by using a sensor, the argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%;
[0018] Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum elements, and a metastable β-type titanium alloy with nominal composition Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy is less than 5 ppm;
[0019] Step 3, preparation of hydrogen permeation prevention layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace. In order to effectively reduce the content of oxygen and water vapor in the furnace, argon is first introduced, the vacuum pump is vacuumed to 8 Pa, then the temperature of the vacuum furnace is raised to the oxygenation temperature of 300-600°C, after 1.5 h, the vacuum pump is turned off, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately displays the pressure value in the system as 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure, and the oxygenation process is carried out for 1-24 h to prepare a hydrogen permeation prevention layer on the surface of the titanium alloy.
[0020] The hydrogen permeation prevention layer prepared according to the above-mentioned method for preparing a hydrogen permeation prevention layer for improving the service life of a titanium alloy has an outer layer of Al2O3 and an inner layer of TiO2. The Ti and Al elements in the hydrogen permeation prevention layer come from the inside of the titanium alloy, and the O element comes from the oxygen and argon mixed gas in the vacuum furnace.
[0021] The reasons for selecting the two oxide layers in the hydrogen permeation prevention layer and their functions are as follows:
[0022] 1. The vacancy hydrogen trap, micro-nano pores and hydrogen reaction generated water and aluminum oxide compounds in the aluminum oxide structure hinder the movement of hydrogen molecules, effectively hinder the diffusion of hydrogen, and slow down the permeation speed of hydrogen to meet the needs of different applications.
[0023] 2. Hydrogen atoms are easily located in the octahedral interstitial sites of TiO2 oxygen atoms and form OH bonds with the nearest oxygen atoms.
[0024] 3. Ti atoms doped into aluminum oxide at the interface can hinder the diffusion and aggregation of hydrogen by forming insoluble stable hydride TiH, thereby improving the hydrogen resistance of the material.
[0025] Example 1
[0026] A method for preparing a hydrogen permeation prevention layer for improving the service life of a titanium alloy, the specific steps are as follows:
[0027] Step 1, mixed gas: open the gas source and let the oxygen and argon pass through the mixing device according to the set ratio to achieve accurate mixing. The content of oxygen and argon is: argon is 80%, oxygen is 20%, and the concentration of the mixed gas is monitored by a sensor. The argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%.
[0028] Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum elements, and a metastable β-type titanium alloy with nominal composition of Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy before oxidation is less than 5 ppm.
[0029] Step 3, preparation of hydrogen permeation prevention layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace. In order to effectively reduce the content of oxygen and water vapor in the furnace, argon is first introduced, the vacuum pump is evacuated to 8 Pa, then the temperature of the vacuum furnace is raised to the oxygenation temperature of 350℃, after 1.5h, the vacuum pump is turned off, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately displays the pressure value in the system as 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure, and the oxygenation process is carried out for 6h to prepare the hydrogen permeation prevention layer on the surface of the titanium alloy.
[0030] An electrochemical workstation is used to carry out hydrogen permeation experiment on the titanium alloy with hydrogen permeation prevention layer prepared in this embodiment. The hydrogen permeation time is 7 days, all the electrolytic solutions are 3.5% NaCl aqueous solution, the negative electrode is the titanium alloy with hydrogen permeation prevention layer, the positive electrode is pure zinc, and the temperature is room temperature.
[0031] A self-made bending fatigue testing machine is used to carry out experiment on the titanium alloy with hydrogen permeation prevention layer prepared in this embodiment, and the life before fracture under room temperature condition is obtained. The 45° bending fatigue test is carried out on the QJWQ-6 numerical control bending testing machine at a rate of 60 times per minute until the sample is broken, and the bending fatigue life is obtained.
[0032] The microstructure morphology of the hydrogen permeation prevention layer for improving the life of titanium alloy prepared by in-situ oxidation method in Example 1 is shown in Figure 1 The hydrogen permeation prevention layer and the titanium alloy substrate are well combined, and there is no crack between the hydrogen permeation prevention layers. After the bending fatigue experiment, the bending life before fracture is 1.2 x 10 4 , which is 1.79 times the fatigue life of titanium alloy without hydrogen permeation prevention layer (the initial titanium alloy without hydrogen permeation prevention layer is 6704 times).
[0033] Example 2
[0034] A preparation method of a hydrogen permeation prevention layer for improving the life of titanium alloy, the specific steps are as follows:
[0035] Step 1, mixed gas: open the gas source, and let the oxygen and argon pass through the mixing device according to the set proportion to realize accurate mixing. The content of oxygen and argon is: argon is 85%, oxygen is 15%, and the concentration of the mixed gas is monitored by a sensor. The argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%.
[0036] Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum elements, and a metastable β-type titanium alloy with nominal composition of Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy before oxidation is less than 5ppm.
[0037] Step 3, preparation of hydrogen permeation prevention layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace. In order to effectively reduce the content of oxygen and water vapor in the furnace, argon is first introduced, the vacuum pump is evacuated to 8Pa, then the temperature of the vacuum furnace is raised to the oxygenation temperature of 350℃, after 1.5h, the vacuum pump is closed, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately displays the pressure value in the system as 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure, and the oxygenation process is carried out for 12h to prepare the hydrogen permeation prevention layer on the surface of the titanium alloy.
[0038] An electrochemical workstation is used to carry out hydrogen permeation experiment on the titanium alloy with hydrogen permeation prevention layer prepared in this embodiment. The hydrogen permeation time is 7 days, all the electrolytic solutions are 3.5% NaCl aqueous solution, the negative electrode is the titanium alloy with hydrogen permeation prevention layer, the positive electrode is pure zinc, and the temperature is room temperature.
[0039] A self-made bending fatigue testing machine is used to carry out experiment on the titanium alloy with hydrogen permeation prevention layer prepared in this embodiment, and the life before fracture under room temperature condition is obtained. The 45° bending fatigue test is carried out on the QJWQ-6 numerical control bending testing machine at a rate of 60 times per minute until the sample is broken, and the bending fatigue life is obtained.
[0040] The hydrogen permeation prevention layer for improving the life of titanium alloy prepared by in-situ oxidation method in Example 2 is subjected to bending fatigue experiment, and the bending life before fracture is 3.0 × 104 times. 4 , which is 4.47 times (initial titanium alloy without hydrogen permeation prevention layer is 6704 times) of the fatigue life of titanium alloy without hydrogen permeation prevention layer.
[0041] Example 3
[0042] A preparation method of a hydrogen permeation prevention layer for improving the life of titanium alloy, the specific steps are as follows:
[0043] Step 1, mixed gas: open the gas source, and let the oxygen and argon pass through the mixing device according to the set proportion to realize accurate mixing. The content of oxygen and argon is: argon is 95%, and oxygen is 5%. A sensor is used to monitor the concentration of the mixed gas. The argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%.
[0044] Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum elements, and a metastable β-type titanium alloy with nominal composition of Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy before oxidation is less than 5ppm.
[0045] Step 3, Preparation of the hydrogen permeation barrier layer: After ultrasonic cleaning, the titanium alloy selected in Step 2 is placed in a vacuum furnace. To effectively reduce the oxygen and water vapor content in the furnace, argon gas is first introduced, and the vacuum pump is used to evacuate to 8 Pa. Then, the temperature of the vacuum furnace is raised to the oxygen permeation temperature of 300℃. After 1.5 hours, the vacuum pump is turned off. Finally, the gas mixed in Step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately shows that the internal pressure of the system is 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure. The oxygen permeation process is carried out for 18 hours, and a hydrogen permeation barrier layer is prepared on the surface of the titanium alloy.
[0046] Hydrogen permeation experiments were conducted on the titanium alloy with a hydrogen permeation barrier layer prepared in this embodiment using an electrochemical workstation. The hydrogen permeation time was 7 days. All electrolyte solutions were 3.5% NaCl aqueous solutions. The negative electrode was the titanium alloy with the hydrogen permeation barrier layer, and the positive electrode was pure zinc. The temperature was room temperature.
[0047] The titanium alloy with a hydrogen permeation-resistant protective layer prepared in this embodiment was tested using a self-made bending fatigue testing machine to obtain the life before fracture at room temperature. A 45° bending fatigue test was performed on a QJWQ-6 CNC bending testing machine at a rate of 60 times per minute until the specimen fractured, thus obtaining the bending fatigue life.
[0048] In Example 3, the hydrogen permeation barrier layer for improving the lifespan of titanium alloys, prepared by in-situ oxidation, exhibited a bending fatigue life of 2.6 x 10 before fracture after bending fatigue testing. 4 It has 3.88 times the fatigue life of titanium alloys without hydrogen permeation barrier coating (the initial fatigue life of titanium alloys without hydrogen permeation barrier coating is 6704 cycles).
[0049] Example 4
[0050] A method for preparing a hydrogen permeation-resistant protective layer to improve the service life of titanium alloys, comprising the following specific steps:
[0051] Step 1, Gas Mixing: Turn on the gas source and let oxygen and argon pass through the mixing device in the set ratio to achieve precise mixing. The oxygen and argon content is: argon 80% and oxygen 20%. Use a sensor to monitor the gas concentration after mixing. Before mixing, the argon concentration is 99.999% and the oxygen concentration is 99.5%.
[0052] Step 2, Titanium alloy selection: The titanium alloy matrix needs to contain aluminum. A metastable β-type titanium alloy is selected, with a nominal composition of Ti3Al15V3Cr3Sn. Before oxidation, the hydrogen content of the titanium alloy is less than 5ppm.
[0053] Step 3, Preparation of the hydrogen permeation barrier layer: The titanium alloy selected in Step 2 was ultrasonically cleaned and then placed in a vacuum furnace. In order to effectively reduce the oxygen and water vapor content in the furnace, argon gas was first introduced, and the vacuum pump was used to evacuate to 8 Pa. Then the temperature of the vacuum furnace was raised to the oxygen permeation temperature of 450℃. After 1.5 h, the vacuum pump was turned off. Finally, the gas mixed in Step 1 was introduced into the vacuum furnace. The vacuum pressure gauge accurately showed that the internal pressure of the system was 0.023 MPa. At this time, the pressure in the vacuum furnace was lower than the standard atmospheric pressure. The oxygen permeation process was carried out for 12 h, and a hydrogen permeation barrier layer was prepared on the surface of the titanium alloy.
[0054] Hydrogen permeation experiments were conducted on the titanium alloy with a hydrogen permeation barrier layer prepared in this embodiment using an electrochemical workstation. The hydrogen permeation time was 7 days. All electrolyte solutions were 3.5% NaCl aqueous solutions. The negative electrode was the titanium alloy with the hydrogen permeation barrier layer, and the positive electrode was pure zinc. The temperature was room temperature.
[0055] The titanium alloy with a hydrogen permeation-resistant protective layer prepared in this embodiment was tested using a self-made bending fatigue testing machine to obtain the life before fracture at room temperature. A 45° bending fatigue test was performed on a QJWQ-6 CNC bending testing machine at a rate of 60 times per minute until the specimen fractured, thus obtaining the bending fatigue life.
[0056] Example 4 describes a hydrogen permeation barrier layer for improving the lifespan of titanium alloys, prepared using an in-situ oxidation method. Figure 2 As shown, the hydrogen permeation barrier layer consists of a surface alumina layer and an internal titanium dioxide layer, with a clear interface between the two oxide layers and the titanium alloy substrate. After bending fatigue testing, the bending life before fracture was 3.6 x 10⁻¹⁰. 4 It has a fatigue life 5.37 times that of titanium alloys without a hydrogen permeation barrier (the initial fatigue life of titanium alloys without a hydrogen permeation barrier was 6704 cycles).
[0057] Example 5
[0058] A method for preparing a hydrogen permeation-resistant protective layer to improve the service life of titanium alloys, comprising the following specific steps:
[0059] Step 1, Gas Mixing: Turn on the gas source and let oxygen and argon pass through the mixing device in the set ratio to achieve precise mixing. The oxygen and argon content is: argon 85% and oxygen 15%. Use a sensor to monitor the gas concentration after mixing. Before mixing, the argon concentration is 99.999% and the oxygen concentration is 99.5%.
[0060] Step 2, Titanium alloy selection: The titanium alloy matrix needs to contain aluminum. A metastable β-type titanium alloy is selected, with a nominal composition of Ti3Al15V3Cr3Sn. Before oxidation, the hydrogen content of the titanium alloy is less than 5ppm.
[0061] Step 3, preparation of hydrogen permeation barrier layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace. In order to effectively reduce the content of oxygen and water vapor in the furnace, argon is first introduced, the vacuum pump is used to vacuum to 8 Pa, then the temperature of the vacuum furnace is increased to the oxygenation temperature of 450℃, after 1.5h, the vacuum pump is turned off, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately displays the pressure value in the system as 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure, and the oxygenation process is carried out for 24h to prepare the hydrogen permeation barrier layer on the surface of the titanium alloy.
[0062] The titanium alloy with hydrogen permeation barrier layer prepared in this embodiment is subjected to hydrogen permeation experiment by using an electrochemical workstation. The hydrogen permeation time is 7 days, all the electrolytic solutions are 3.5% NaCl aqueous solution, the negative electrode is the titanium alloy with hydrogen permeation barrier layer, the positive electrode is pure zinc, and the temperature is room temperature.
[0063] The titanium alloy with hydrogen permeation barrier layer prepared in this embodiment is subjected to experiment by using a self-made bending fatigue testing machine, and the life before fracture under room temperature condition is obtained. The 45° bending fatigue test is carried out on the QJWQ-6 numerical control bending testing machine at a rate of 60 times per minute until the sample is broken, and the bending fatigue life is obtained.
[0064] The hydrogen permeation barrier layer for improving the life of titanium alloy prepared by in-situ oxidation method in Example 5 is subjected to bending fatigue experiment, and the bending life before fracture is 1.2 x 10 4 , which is 1.79 times the fatigue life of titanium alloy without hydrogen permeation barrier layer (6704 times for titanium alloy without hydrogen permeation barrier layer initially).
[0065] Example 6
[0066] A method for preparing a hydrogen permeation barrier layer for improving the life of titanium alloy, the specific steps are as follows:
[0067] Step 1, mixed gas: open the gas source, and let the oxygen and argon pass through the mixing device according to the set ratio to realize accurate mixing. The content of oxygen and argon is: argon is 95%, and oxygen is 5%. A sensor is used to monitor the concentration of the mixed gas. The argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%.
[0068] Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum element, and a metastable β type titanium alloy with nominal composition of Ti3Al15V3Cr3Sn is selected. The hydrogen content of the titanium alloy before oxidation is less than 5ppm.
[0069] Step 3, preparation of hydrogen permeation barrier layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace. In order to effectively reduce the content of oxygen and water vapor in the furnace, argon is first introduced, the vacuum pump is used to vacuumize to 8 Pa, then the temperature of the vacuum furnace is increased to the oxygenation temperature of 600℃, after 1.5 h, the vacuum pump is closed, and finally the mixed gas prepared in step 1 is introduced into the vacuum furnace. The vacuum pressure gauge accurately displays the pressure value in the system as 0.023 MPa. At this time, the pressure in the vacuum furnace is lower than the standard atmospheric pressure, and the oxygenation process is carried out for 1 h to prepare a hydrogen permeation barrier layer on the surface of the titanium alloy.
[0070] The titanium alloy with the hydrogen permeation barrier layer prepared in this embodiment is subjected to hydrogen permeation experiment by using an electrochemical workstation. The hydrogen permeation time is 7 days, all the electrolytic solutions are 3.5% NaCl aqueous solution, the negative electrode is the titanium alloy with the hydrogen permeation barrier layer, the positive electrode is pure zinc, and the temperature is room temperature.
[0071] The titanium alloy with the hydrogen permeation barrier layer prepared in this embodiment is subjected to experiment by using a self-made bending fatigue testing machine, and the life before fracture under room temperature condition is obtained. The 45° bending fatigue test is carried out on the QJWQ-6 numerical control bending testing machine at a rate of 60 times per minute until the sample is broken, and the bending fatigue life is obtained.
[0072] The hydrogen permeation barrier layer for improving the life of the titanium alloy prepared by the in-situ oxidation method in embodiment 6 is subjected to bending fatigue experiment, and the bending life before fracture is 2.7×10 4 , which is 4.02 times the fatigue life of the titanium alloy without the hydrogen permeation barrier layer (6704 times for the titanium alloy without the hydrogen permeation barrier layer).
[0073] The above description of the present application is only part of the embodiments, but the present application is not limited to the above examples. The above embodiments are illustrative and not restrictive. Any specific expansion using the materials and methods of the present application without departing from the purpose of the present application and the scope protected by the claims is within the protection scope of the present application.
Claims
1. A method for producing a hydrogen permeation barrier for improving the life of a titanium alloy, characterized by, Specifically comprising the following steps: Step 1, mixed gas: open the gas source, let the oxygen and argon pass through the mixing device according to the set ratio, realize accurate mixing, use a sensor to monitor the concentration of the mixed gas, the argon concentration before mixing is 99.999%, and the oxygen concentration is 99.5%; Step 2, titanium alloy selection: the titanium alloy substrate needs to contain aluminum elements, a metastable β type titanium alloy with nominal composition Ti3Al15V3Cr3Sn is selected, and the hydrogen content of the titanium alloy is less than 5ppm; Step 3, preparation of hydrogen permeation prevention layer: the titanium alloy selected in step 2 is cleaned by ultrasonic cleaning and then loaded into a vacuum furnace, argon is first introduced, the vacuum pump is vacuumed to 8Pa, then the temperature of the vacuum furnace is raised to the oxygen permeation temperature, after 1.5h, the vacuum pump is closed, finally the mixed gas prepared in step 1 is introduced into the vacuum furnace, the pressure in the vacuum furnace is 0.023 MPa, at this time the pressure in the vacuum furnace is lower than the standard atmospheric pressure, the oxygen permeation process is carried out, the oxygen permeation temperature is 300-600℃, the oxygen permeation process is 1-24h, the hydrogen permeation prevention layer is prepared on the surface of the titanium alloy, the outer layer of the hydrogen permeation prevention layer is Al2O3, the inner layer is TiO2, the Ti and Al elements in the hydrogen permeation prevention layer come from the inside of the titanium alloy, and the O element comes from the oxygen and argon mixed gas in the vacuum furnace.
2. The method of claim 1, wherein the method is characterized by: In step 1, the content of oxygen and argon is: argon is 80-95%, and oxygen is 5%-20%.
Citation Information
Patent Citations
High-bonding-strength in-situ oxidation coating on surface of titanium product and preparation method
CN118792713A
Method for depositing hard coatings on titanium or titanium alloys
US4902535A