A method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel

By preparing a FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel, the corrosion problem of lead-bismuth alloys on structural materials was solved, and the corrosion resistance and mechanical properties of the material were improved, making it suitable for lead-based reactor structural materials.

CN119411086BActive Publication Date: 2025-11-14TECHN PHYSICS INST HEILONGJIANG ACADOF SCI
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Patent Information

Application Number
CN202411582759.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-07
Publication Date
2025-11-14
Estimated Expiration
2044-11-07

AI Technical Summary

Technical Problem

Lead-bismuth alloys, when used as coolants, can severely corrode structural materials, especially in the high-temperature liquid lead-bismuth eutectic environment. This can lead to dissolution corrosion and oxidation corrosion of structural materials, affecting their corrosion resistance.

Method used

A FeCrAlTi-yttrium oxide coating was prepared on the surface of austenitic 316L steel by magnetron sputtering. A composite target was prepared by powder metallurgy, and Y2O3 nano-oxide was introduced. The coating was deposited under specific conditions using DC magnetron sputtering technology, and the coating thickness was 5μm to 7μm.

Benefits of technology

The mechanical properties and resistance to lead-bismuth eutectic corrosion of 316L austenitic steel are improved. The coating has good adhesion and uniform distribution, making it suitable for radiation/corrosion protection of lead-based reactor structural materials under extreme conditions.

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Abstract

A method for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel is disclosed. This invention addresses the problem of severe corrosion of structural materials by existing lead-bismuth alloys used as coolants. The method comprises: 1. Target mounting and sputtering pretreatment; 2. Magnetron sputtering. This invention is used for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel.
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Description

Technical Field

[0001] This invention relates to a method for applying a magnetron sputtering coating to a steel surface. Background Technology

[0002] Energy is a vital material foundation for human survival and a driving force for the development of human society. Nuclear energy, characterized by its high efficiency, cleanliness, and safety, is internationally recognized as a new energy source suitable for large-scale application. In the early 21st century, to minimize nuclear waste and improve the nuclear fuel cycle, the fourth generation of reactors was creatively proposed, which includes six reactor types. Lead-based reactors are an advanced nuclear energy system, including lead-cooled fast reactor systems (LFR) and accelerator-driven subcritical systems (ADS). Lead-cooled fast reactors are considered one of the most promising nuclear reactors for the future.

[0003] Lead-cooled fast reactors in the fourth-generation nuclear energy system are named for their coolant, which is pure lead or lead-bismuth alloy. They have the following advantages: (1) high safety performance; (2) sustainable supply of nuclear fuel; and (3) good economic benefits. Stainless steel structural materials are often used as structural materials for LFR and ADS due to their good resistance to high-temperature oxidation, resistance to neutron radiation, good thermal conductivity and cold workability. At present, the international choice for the main vessel of lead-based fast reactors is mainly 316L austenitic stainless steel. However, using lead-bismuth alloy as a coolant also has some disadvantages for structural materials, such as severe corrosion: in the high-temperature liquid lead-bismuth eutectic (LBE) environment, structural materials are prone to dissolution corrosion and oxidation corrosion. With the change of corrosion temperature and dissolved oxygen concentration in liquid lead-bismuth alloy, these two corrosion behaviors will jointly affect the corrosion resistance of the material. Summary of the Invention

[0004] This invention aims to solve the problem of severe corrosion of structural materials by existing lead-bismuth alloys as coolants, and provides a method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel.

[0005] A method for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel, comprising the following steps:

[0006] I. Target installation and sputtering pretreatment:

[0007] The 53Fe18Cr13Al8Ti-8Y2O3 composite target was installed on the target position of the DC magnetron sputtering device. The austenitic 316L steel substrate was placed on the sample stage of the DC magnetron sputtering device. The distance between the sample and the target head was adjusted. After closing the chamber door, the vacuum was drawn and argon gas was introduced. The negative bias voltage power supply was turned on, and then the austenitic 316L steel substrate was pre-sputtered.

[0008] II. Magnetron Sputtering:

[0009] After pre-sputtering, the sample stage speed is adjusted, and magnetron sputtering is performed under the following conditions: working gas pressure in the chamber is 0.4 Pa to 0.7 Pa, chamber temperature is 60 °C to 150 °C, current is 0.2 A to 0.4 A, and negative bias voltage is 0 V to 200 V. Then, the chamber vacuum is maintained and cooled to room temperature. Finally, the sample is removed, thus completing the method of magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel.

[0010] The beneficial effects of this invention are:

[0011] 1. This invention prepares a composite target material by powder metallurgy, wherein Y2O3 nano-oxide can be dispersed into FeCrAlTi alloy, wherein the target material purity is ≥99.9%, and the target material can be reused multiple times. It can effectively overcome the complex process conditions such as dual-target sputtering required by traditional Y2O3 sputtering, and can use DC magnetron sputtering to prepare coating materials, and its sputtering rate is faster than that of radio frequency magnetron sputtering.

[0012] 2. This invention introduces dispersed Y2O3 nanoparticles. These fine and dispersed Y2O3 particles are key to improving the mechanical properties and resistance to LBE corrosion. The process of this invention is highly controllable and easy to implement. It can be applied to the surface of lead-based fast reactor structural materials, achieving a coating thickness of 5μm to 7μm. This coating can improve the mechanical properties and resistance to lead-bismuth eutectic (LBE) corrosion of 316L austenitic steel to a certain extent. It can also be used as a radiation / corrosion resistant coating material for lead-based reactor structural materials under extreme operating conditions. The resulting coating film has no undesirable porosity, good adhesion, and a uniform distribution without obvious defects.

[0013] Instruction manual illustrations

[0014] Figure 1 The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating prepared by surface magnetron sputtering in Example 1 on austenitic 316L steel. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image.

[0015] Figure 2 The GIXRD pattern of the austenitic 316L steel intermediate coating with FeCrAlTi-Y2O3 surface magnetron sputtering prepared in Example 1;

[0016] Figure 3The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating on austenitic 316L steel prepared by surface magnetron sputtering in Example 2. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image.

[0017] Figure 4 The GIXRD pattern of the austenitic 316L steel intermediate coating prepared by surface magnetron sputtering FeCrAlTi-Y2O3 coating in Example 2;

[0018] Figure 5 The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating on austenitic 316L steel prepared by surface magnetron sputtering in Example 3. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image.

[0019] Figure 6 The GIXRD pattern of the austenitic 316L steel intermediate coating with FeCrAlTi-Y2O3 surface magnetron sputtering prepared in Example 3;

[0020] Figure 7 XPS image of the coating in austenitic 316L steel prepared by surface magnetron sputtering FeCrAlTi-Y2O3 coating in Example 2;

[0021] Figure 8 The following are schematic diagrams of nanoindentation on austenitic 316L steel with FeCrAlTi-Y2O3 surface magnetron sputtered coating prepared in Examples 1 to 3: (a) is the nanoindentation displacement-load curve, and (b) is the indentation hardness H and reduced elastic modulus E.

[0022] Figure 9 The image shows the SEM images of the austenitic 316L steel intermediate coating with FeCrAlTi-Y2O3 surface magnetron sputtering prepared in Example 1 after LBE corrosion at 550℃ for 100h. (a) is on a scale of 10μm, and (b) is on a scale of 5μm.

[0023] Figure 10 The images show SEM and EDS images of the austenitic 316L steel with a FeCrAlTi-Y2O3 surface magnetron sputtering coating prepared in Example 2, after being irradiated with γ-rays at a total dose of 1 MGy and then subjected to LBE corrosion at 650℃ for 500 h. (a) is the SEM image, and (b) is the EDS image. Detailed Implementation

[0024] Specific Implementation Method 1: This implementation method is a method for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel, which is carried out according to the following steps:

[0025] I. Target installation and sputtering pretreatment:

[0026] The 53Fe18Cr13Al8Ti-8Y2O3 composite target was installed on the target position of the DC magnetron sputtering device. The austenitic 316L steel substrate was placed on the sample stage of the DC magnetron sputtering device. The distance between the sample and the target head was adjusted. After closing the chamber door, the vacuum was drawn and argon gas was introduced. The negative bias voltage power supply was turned on, and then the austenitic 316L steel substrate was pre-sputtered.

[0027] II. Magnetron Sputtering:

[0028] After pre-sputtering, the sample stage speed is adjusted, and magnetron sputtering is performed under the following conditions: working gas pressure in the chamber is 0.4 Pa to 0.7 Pa, chamber temperature is 60 °C to 150 °C, current is 0.2 A to 0.4 A, and negative bias voltage is 0 V to 200 V. Then, the chamber vacuum is maintained and cooled to room temperature. Finally, the sample is removed, thus completing the method of magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel.

[0029] In this specific embodiment, after the coating preparation is completed, the target baffle, heating device, DC power supply and sample stage rotation are turned off in sequence, and the vacuum chamber is kept to slowly cool to room temperature. This cooling method can effectively reduce the internal stress generated in the coating during the cooling process. Then the sample is taken out and placed in the film box.

[0030] The beneficial effects of this implementation are:

[0031] 1. This embodiment prepares a composite target material by powder metallurgy, wherein Y2O3 nano-oxide can be dispersed into FeCrAlTi alloy, wherein the purity of the target material is ≥99.9%, and the target material can be reused multiple times. It can effectively overcome the complex process conditions such as dual-target sputtering required by traditional Y2O3 sputtering, and DC magnetron sputtering can be used to prepare coating materials, and its sputtering rate is faster than that of radio frequency magnetron sputtering.

[0032] 2. This embodiment introduces dispersed Y2O3 nanoparticles. The fine and dispersed Y2O3 particles are key to improving its mechanical properties and resistance to LBE corrosion. This embodiment has strong process controllability and is easy to implement. It can be used on the surface of lead-based fast reactor structural materials, and the resulting coating thickness can reach 5μm to 7μm. It can improve the mechanical properties and resistance to lead-bismuth eutectic (LBE) corrosion of 316L austenitic steel to a certain extent. It can also be used as a radiation / corrosion resistant coating material for lead-based reactor structural materials under extreme operating conditions. The resulting coating film has no undesirable pores, good adhesion, uniform coating distribution, and no obvious defects.

[0033] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the 53Fe18Cr13Al8Ti-8Y2O3 composite target material described in step one is prepared according to the following steps: Fe powder, Cr powder, Al powder, Ti powder, and Y2O3 ceramic oxide powder are mixed in an atomic ratio of 53:18:13:8:8 to obtain an alloyed mixed powder. Under Ar atmosphere, pressure of 260MPa~300MPa, and sintering temperature of 900℃~1000℃, the alloyed mixed powder is sintered under pressure for 5min~10min to obtain the FeCrAlTi-Y2O3 composite target material. Everything else is the same as in Specific Implementation Method One.

[0034] Specific Implementation Method Three: This implementation method differs from Specific Implementation Method One or Two in that the austenitic 316L steel substrate mentioned in step one is obtained after pretreatment. The pretreatment is specifically carried out according to the following steps: the surface of the austenitic 316L steel substrate is successively polished with 400#, 800#, 1200#, 2000# and 3000# sandpaper, and then polished successively with polishing liquids with particle sizes of 1.5μm, 1.0μm and 0.5μm until there are no obvious scratches on the surface. Then, it is ultrasonically cleaned with acetone, anhydrous ethanol and deionized water for 10 min to 15 min in sequence. Finally, it is taken out and dried. The rest is the same as in Specific Implementation Method One or Two.

[0035] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that the distance between the sample and the target head is adjusted to 4cm to 6cm in step one. Everything else is the same as in Specific Implementation Methods One to Three.

[0036] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that: the vacuuming and argon gas introduction in step one is specifically carried out as follows: a mechanical pump and a molecular pump are used to evacuate to a vacuum level of 1.5 × 10⁻⁶. -3 Pa ~ 1.5 × 10 -4Pa, then Ar gas is introduced and the Ar gas flow rate is adjusted so that the working gas pressure in the chamber is 0.4 Pa to 0.7 Pa. The rest is the same as in specific embodiments one to four.

[0037] Specific Implementation Method Six: This implementation method differs from Specific Implementation Methods One to Five in that the Ar gas flow rate is adjusted to 90 sccm / min to 120 sccm / min. Everything else is the same as Specific Implementation Methods One to Five.

[0038] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Methods One to Six in that the pre-sputtering described in step one is carried out under the following conditions: a working gas pressure of 0.4 Pa to 0.7 Pa, a chamber temperature of 60°C to 150°C, a DC current of 0.2 A to 0.4 A, and a negative bias voltage of 300 V to 500 V, for 5 to 10 minutes of pre-sputtering. Everything else is the same as in Specific Implementation Methods One to Six.

[0039] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Methods One to Seven in that the thickness of the magnetron sputtering coating in step two is 5μm to 7μm. Everything else is the same as in Specific Implementation Methods One to Seven.

[0040] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Methods One to Eight in that the magnetron sputtering deposition in step two takes 2 to 4 hours. Everything else is the same as in Specific Implementation Methods One to Eight.

[0041] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in that the sample stage rotation speed is adjusted to 10 r / min to 15 r / min in step two. Everything else is the same as in Specific Implementation Methods One to Nine.

[0042] The beneficial effects of the present invention are verified using the following embodiments:

[0043] Example 1:

[0044] A method for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel, comprising the following steps:

[0045] I. Target installation and sputtering pretreatment:

[0046] The 53Fe18Cr13Al8Ti-8Y2O3 composite target was installed on the target position of the DC magnetron sputtering device. The austenitic 316L steel substrate was placed on the sample stage of the DC magnetron sputtering device. The distance between the sample and the target head was adjusted to 4cm. After closing the chamber door, the vacuum was evacuated and argon gas was introduced. The negative bias voltage power supply was turned on. Then, the austenitic 316L steel substrate was pre-sputtered for 10min under the conditions of working gas pressure of 0.6Pa, chamber temperature of 150℃, DC current of 0.3A and negative bias voltage of 500V.

[0047] II. Magnetron Sputtering:

[0048] After pre-sputtering, the sample stage speed was adjusted. Magnetron sputtering was performed for 4 hours under the following conditions: sample stage speed of 10 r / min, working gas pressure in the chamber of 0.6 Pa, temperature in the chamber of 150 °C, current of 0.3 A, and negative bias voltage of 0 V. Then, the chamber vacuum was maintained and cooled to room temperature. Finally, the sample was removed, and austenitic 316L steel with FeCrAlTi-Y2O3 coating on the surface was obtained.

[0049] The 53Fe18Cr13Al8Ti-8Y2O3 composite target material mentioned in step one is prepared according to the following steps: Fe powder, Cr powder, Al powder, Ti powder and Y2O3 ceramic oxide powder are mixed in an atomic ratio of 53:18:13:8:8 to obtain an alloyed mixed powder. Under Ar atmosphere, pressure of 300MPa and sintering temperature of 1000℃, the alloyed mixed powder is sintered under pressure for 5min to obtain the FeCrAlTi-Y2O3 composite target material; the purity of the target material is ≥99.9%.

[0050] The austenitic 316L steel substrate mentioned in step one is obtained after pretreatment; the pretreatment is specifically carried out according to the following steps: the surface of the austenitic 316L steel substrate is polished with 400#, 800#, 1200#, 2000# and 3000# sandpaper in sequence, and then polished with polishing liquids with particle sizes of 1.5μm, 1.0μm and 0.5μm in sequence until there are no obvious scratches on the surface. Then, it is ultrasonically cleaned with acetone, anhydrous ethanol and deionized water in sequence for 10 minutes, and finally taken out and dried.

[0051] Step one, which involves evacuating the vacuum and introducing argon gas, is specifically performed as follows: The vacuum is evacuated to 1.5 × 10⁻⁶ using both a mechanical pump and a molecular pump. -4 Pa, then Ar gas is introduced and the Ar gas flow rate is adjusted to 120 sccm / min, so that the working gas pressure in the chamber is 0.6 Pa.

[0052] In step two, the thickness of the magnetron sputtering coating is 6.88 μm.

[0053] Example 2: This example differs from Example 1 in that the negative bias voltage in step 2 is 100V; and the thickness of the magnetron sputtering film in step 2 is 6.70μm. Everything else is the same as in Example 1.

[0054] Example 3: This example differs from Example 1 in that the negative bias voltage in step 2 is 200V; and the thickness of the magnetron sputtering film in step 2 is 5.73μm. Everything else is the same as in Example 1.

[0055] Figure 1 The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating prepared in Example 1 on austenitic 316L steel. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image. As shown in the figures, the thickness of the prepared FeCrAlTi-Y2O3 coating is approximately 6.88 μm. There is a clear interface between the alloy coating and the substrate material. There are no undesirable pores on the surface of the alloy coating and the 316L steel substrate material, indicating that there is good film-substrate adhesion between the two. The cross-sectional EDS image shows that the elements in the deposited coating are evenly distributed, and no obvious element aggregation or segregation was observed. Ti and Y elements are enriched on the surface of the alloy coating.

[0056] Figure 2 The image shows the GIXRD pattern of the FeCrAlTi-Y2O3 coating on austenitic 316L steel prepared by surface magnetron sputtering in Example 1. As can be seen from the image, the prepared FeCrAlTi-Y2O3 coating material exhibits a clear amorphous structure with two broad peaks at 2θ = 33° and 2θ = 45°. The coating has no obvious defects, and no diffraction peaks of the 316L steel substrate were detected.

[0057] Figure 3 The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating prepared in Example 2 on austenitic 316L steel. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image. As can be seen from the figures, the thickness of the prepared FeCrAlTi-Y2O3 coating is approximately 6.70 μm, which also indicates that there is a clear interface between the alloy coating and the substrate material. There are no undesirable pores on the surface of the alloy coating and the substrate material, austenitic 316L steel, indicating that there is good film-substrate adhesion between the two.

[0058] Figure 4The image shows the GIXRD pattern of the FeCrAlTi-Y2O3 coating on austenitic 316L steel prepared by surface magnetron sputtering in Example 2. As can be seen from the image, the prepared FeCrAlTi-Y2O3 coating material exhibits a distinct amorphous structure, with enhanced diffraction peaks of the Fe-Cr phase.

[0059] Figure 5 The images show SEM and EDS diagrams of the cross-section of the FeCrAlTi-Y2O3 coating prepared by surface magnetron sputtering in Example 3 on austenitic 316L steel. (a) is an SEM image with a scale of 100 μm, (b) is an SEM image with a scale of 10 μm, (c) is an SEM image with a scale of 5 μm, and (d) is an EDS image. As can be seen from the figures, the thickness of the prepared FeCrAlTi-Y2O3 coating is about 5.73 μm. There is a clear interface between the coating and the substrate. The EDS image shows that the coating was successfully prepared. The elements in the coating are uniformly distributed, and no obvious element aggregation or segregation was observed. Ti and Y elements are enriched on the surface of the alloy coating.

[0060] The comparison revealed that the coating thickness decreased with increasing bias voltage, indicating that the coating deposition rate decreased to some extent with increasing bias voltage. The increase in bias voltage reduced the atomic deposition rate on the coating surface. The larger ion flux promoted the migration and filling of deposited atoms on the substrate surface, improved the surface density of the coating, and thus caused the coating deposition rate to decrease with increasing bias voltage.

[0061] Figure 6 The image shows the GIXRD pattern of the FeCrAlTi-Y2O3 surface magnetron sputtered coating on austenitic 316L steel prepared in Example 3. As can be seen from the image, the coating exhibits an amorphous structure, which is beneficial for improving the material's oxidation resistance.

[0062] Figure 7 The XPS spectra of the FeCrAlTi-Y2O3 surface-sputtered FeCrAlTi-Y2O3 coating on austenitic 316L steel prepared in Example 2 are shown. As can be seen from the figure, 157.5 eV and 159.5 eV correspond to Y3d... 5 / 2 and Y 3d 3 / 2 The electron binding energy indicates that Y exists in the alloy coating in multiple forms, including Y₂O₃. No metallic Y 3d peak was found at 155.6 eV, indicating that the content of metallic Y in the film is small or absent. XPS data demonstrate that the successful preparation of the FeCrAlTi-Y₂O₃ alloy coating and the successful incorporation of Y₂O₃ dispersed metal oxides play a crucial role in improving the coating material's resistance to high-temperature oxidation and radiation corrosion.

[0063] Figure 8The figures show the nanoindentation diagrams of the FeCrAlTi-Y2O3 surface magnetron sputtered FeCrAlTi-Y2O3 coatings prepared in Examples 1 to 3 on austenitic 316L steel. (a) shows the nanoindentation displacement-load curve, and (b) shows the indentation hardness H and reduced elastic modulus E. The maximum load is set to 20 mN. As can be seen from the figures, the nanohardness of the coating in Example 3 can reach up to 11.52 GPa, while the nanohardness of the 316L steel substrate is only 5.49 GPa. The coating increases the nanohardness by more than 100%. Under the same maximum load pressure, the indentation depth of the 316L steel substrate is about 450 nm, while the indentation depth of the sample prepared in Example 3 is only 300 nm.

[0064] Figure 9 The image shows a SEM image of the austenitic 316L steel coating with a FeCrAlTi-Y2O3 surface magnetron sputtering coating prepared in Example 1 after LBE corrosion at 550℃ for 100 h. (a) shows the scale bar at 10 μm, and (b) shows the scale bar at 5 μm. The LBE contains 44.5 at.% Pb and 55.5 at.% Bi. As shown in the image, a large amount of oxides are generated on the surface of the alloy coating in Example 1 after LBE corrosion. The generated oxides can effectively inhibit further penetration of LBE. The surface contains 1.38 at.% Pb, and the contents of Ti and Y elements are 2.21 at.% and 4.72 at.%, respectively.

[0065] In Example 2, after LBE etching at 550℃ for 100 hours, only 0.16 at.% Bi remained on the surface, with Ti and Y content at 2.18 at.% and 4.69 at.%, respectively. In Example 3, after LBE etching at 550℃ for 100 hours, a certain amount of lead-bismuth alloy remained on the surface, containing 0.5 at.% Pb and 0.16 at.% Bi, with Ti and Y content at 1.74 at.% and 4.28 at.%, respectively, indicating the formation of a certain amount of Pb oxide. However, the coatings prepared in Examples 1 to 3 remained intact after LBE etching at 550℃ for 100 hours. Under certain conditions, the preparation of a dense FeCrAlTi-Y2O3 alloy coating can improve the corrosion resistance of the substrate.

[0066] Figure 10The images show cross-sectional SEM and EDS images of the austenitic 316L steel with a FeCrAlTi-Y2O3 surface magnetron sputtered coating prepared in Example 2, after irradiation with a total dose of 1 mgy of gamma rays and LBE corrosion at 650°C for 500 h. (a) is the SEM image, and (b) is the EDS image. The LBE contains 44.5 at.% Pb and 55.5 at.% Bi. As shown in the figures, the entire oxide layer can be divided into an outer oxide layer and an inner oxide layer. The outer oxide layer is mainly composed of Fe composite oxides with a thickness of approximately 15 μm, while the inner oxide layer is mainly composed of Cr composite oxides with a thickness of approximately 20 μm. The LBE alloy is confined to the coating surface, and the FeCrAlTi-Y2O3 coating can effectively inhibit further penetration of LBE, thereby improving the radiation / corrosion resistance of the substrate under extreme corrosive environments.

Claims

1. A method for magnetron sputtering a FeCrAlTi-yttrium oxide coating onto the surface of austenitic 316L steel, characterized in that... It is done in the following steps: I. Target installation and sputtering pretreatment: The 53Fe18Cr13Al8Ti-8Y2O3 composite target was installed on the target position of the DC magnetron sputtering device. The austenitic 316L steel substrate was placed on the sample stage of the DC magnetron sputtering device. The distance between the sample and the target head was adjusted. After closing the chamber door, the vacuum was drawn and argon gas was introduced. The negative bias voltage power supply was turned on, and then the austenitic 316L steel substrate was pre-sputtered. The 53Fe18Cr13Al8Ti-8Y2O3 composite target is prepared according to the following steps: Fe powder, Cr powder, Al powder, Ti powder and Y2O3 ceramic oxide powder are mixed in an atomic ratio of 53:18:13:8:8 to obtain an alloyed mixed powder. Under Ar atmosphere, pressure of 260MPa~300MPa and sintering temperature of 900℃~1000℃, the alloyed mixed powder is sintered under pressure for 5min~10min to obtain the FeCrAlTi-Y2O3 composite target. II. Magnetron Sputtering: After pre-sputtering, the sample stage speed is adjusted to 10 r / min to 15 r / min. Magnetron sputtering is performed under the following conditions: working gas pressure in the chamber is 0.4 Pa to 0.7 Pa, chamber temperature is 60 °C to 150 °C, current is 0.2 A to 0.4 A, and negative bias voltage is 0 V to 200 V. Then, the chamber vacuum is maintained and cooled to room temperature. Finally, the sample is removed, thus completing the method of magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel.

2. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 1, characterized in that... The austenitic 316L steel substrate mentioned in step one is obtained after pretreatment; the pretreatment is specifically carried out according to the following steps: the surface of the austenitic 316L steel substrate is polished with 400#, 800#, 1200#, 2000# and 3000# sandpaper in sequence, and then polished with polishing liquids with particle sizes of 1.5μm, 1.0μm and 0.5μm in sequence until there are no obvious scratches on the surface. Then, it is ultrasonically cleaned with acetone, anhydrous ethanol and deionized water in sequence for 10min~15min. Finally, it is taken out and dried.

3. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 1, characterized in that... In step one, adjust the distance between the sample and the target to 4cm~6cm.

4. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 1, characterized in that... Step one, which involves evacuating the vacuum and introducing argon gas, is specifically performed as follows: The vacuum is evacuated to 1.5 × 10⁻⁶ using both a mechanical pump and a molecular pump. -3 Pa ~ 1.5 × 10 -4 Pa, then introduce Ar gas and adjust the Ar gas flow rate to make the working gas pressure in the chamber 0.4Pa~0.7Pa.

5. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 4, characterized in that... Adjust the Ar flow rate to 90 sccm / min to 120 sccm / min.

6. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 1, characterized in that... The pre-sputtering described in step one is specifically carried out under the following conditions: working gas pressure in the chamber is 0.4 Pa to 0.7 Pa, chamber temperature is 60°C to 150°C, DC current is 0.2 A to 0.4 A, and negative bias voltage is 300 V to 500 V, for 5 min to 10 min.

7. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 1, characterized in that... In step two, the thickness of the magnetron sputtering coating is 5μm~7μm.

8. The method for magnetron sputtering FeCrAlTi-yttrium oxide coating on the surface of austenitic 316L steel according to claim 7, characterized in that... In step two, the magnetron sputtering coating process takes 2 to 4 hours.

Citation Information

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