A method for preparing FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology

Abstract

The present invention mainly proposes a method for preparing a FeCrAlY wear-resistant and corrosion-resistant coating based on HiPIMS and ion implantation technology, including: step 1, pickling, cleaning, rinsing and dehydrating and drying the workpiece in sequence; step 2, placing the treated workpiece in the vacuum chamber of the ion implantation equipment for ion implantation treatment; step 3, placing the workpiece in the vacuum chamber of the magnetron sputtering for arc-enhanced plasma etching and cleaning treatment; step 4, depositing Al as a base layer; step 5, turning on the magnetron FeCrAlY target source for coating plating; step 6, turning off the vacuum system; step 7, taking out the workpiece for ultrasonic alcohol cleaning, and placing it in a vacuum bag after drying. The present invention forms a FeCrAlY coating on the workpiece through HiPIMS and ion implantation technology, which has the effects of high temperature resistance, wear resistance and corrosion resistance. The pre-injected and deposited Al element can diffuse outward when the coating is damaged to play a self-repairing role and extend the service life.

Description

Technical Field

[0001] The invention belongs to the technical field of coating preparation and surface treatment, and specifically relates to a method for preparing a FeCrAlY wear-resistant and corrosion-resistant coating based on HiPIMS and ion implantation technology. Background Art

[0002] In the current high-end industrial field, especially in the face of extreme operating conditions, such as the nuclear energy environment of lead-cooled fast reactors and high-temperature, high-pressure, and highly corrosive application scenarios such as turbine engine blades, traditional materials are often unable to simultaneously meet the stringent requirements of high temperature resistance, corrosion resistance, and wear resistance, resulting in rapid degradation of material properties, limiting the depth and breadth of technology applications.

[0003] High-power pulsed magnetron sputtering (HiPIMS) technology has unique pulse energy characteristics and can generate high-density, high-energy plasma in a short time, thereby achieving efficient and uniform deposition of high-quality, high-performance coatings on the substrate. Through HiPIMS technology, dense and strongly bonded coatings can be formed on the substrate. These coatings not only have excellent high-temperature resistance and can resist thermal stress damage in high-temperature environments, but also show excellent corrosion resistance and effectively resist erosion by corrosive media. At the same time, HiPIMS technology can also further optimize the microstructure and performance of the coating by adjusting process parameters to meet specific needs in different application scenarios. Summary of the invention

[0004] Based on the above problems, the present invention proposes a method for preparing a FeCrAlY wear-resistant and corrosion-resistant coating based on HiPIMS and ion implantation technology. The FeCrAlY coating is selected because of its high temperature resistance, wear resistance and corrosion resistance and has been used as a thermal barrier coating in engine and other application scenarios for a long time. The coating mainly plays a protective role by quickly generating a stable alumina protective film, wherein the Fe element is the common main element of the coating and various types of steel, which is conducive to ensuring the bonding strength of such coating on the steel; the Cr element itself can form a protective chromium oxide film, and can also promote the Al element to quickly form a dense oxide film. Increasing its content within a certain range can enable the coating to exert sufficient protection capabilities with a lower Al content; the Al element is the main element of the alumina protective film, and its content is too high will increase the brittleness of the coating. Such coatings are not suitable for being directly made into bulk structural materials because such bulk materials with high Al content should be too brittle and have poor processing performance; the Y element is doped as a rare earth element to refine the grains and promote the rapid formation of the alumina protective film, and can delay its thickening after its formation. At the same time, the Al element is pre-embedded in the surface of the substrate by the method of ion implantation, which will not increase the Al content of the coating to damage the mechanical properties, but can diffuse outward to form a protective oxide film again when the coating is damaged due to friction and other reasons, so as to play the role of self-repair of the coating and prolong its service life.

[0005] The technical solution of the present invention is a method for preparing a FeCrAlY wear-resistant and corrosion-resistant coating based on HiPIMS and ion implantation technology, comprising the following steps:

[0006] Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, dehydration and drying of the workpiece in sequence;

[0007] Step 2, placing the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, installing the Al target, adjusting the background vacuum degree of the vacuum chamber of the ion implantation equipment and heating it, turning on the ion implantation source, adjusting the ion implantation energy, ion beam intensity and ion implantation metering, opening the baffle, and when the ion implantation metering reaches a preset value, closing the baffle, turning off the ion source, and waiting for the workpiece temperature to drop below 100° C., and then turning off the vacuum system;

[0008] Step 3: Place the workpiece processed in step 2 into a magnetron sputtering vacuum chamber, adjust the background vacuum of the magnetron sputtering vacuum chamber and heat it, turn on the ion implantation source, turn on the Al arc target source and anode source of the physical vapor deposition equipment, shield the arc source, introduce argon gas to the working pressure, perform arc enhanced plasma etching and cleaning, further activate the structural material substrate after ion implantation and promote the uniform diffusion of the implanted particles;

[0009] Step 4: turn off the Al arc target source and the anode source, turn on the magnetron Al target source and the bias power supply, adjust the power supply parameters, adjust the argon gas flux and the working gas pressure in the vacuum chamber, and deposit the Al base layer;

[0010] Step 5: Based on the operation in step 4, start the magnetron FeCrAlY target source and adjust the power supply parameters to perform coating plating;

[0011] Step 6: After the predetermined time in step 5, turn off all power supplies and argon gas, wait until the temperature of the magnetron sputtering vacuum chamber drops below 100° C., and then turn off the vacuum system;

[0012] Step 7: Take out the treated 304 stainless steel substrate and clean it with ultrasonic alcohol, then put it into a vacuum bag after drying.

[0013] Preferably, the pickling in step one mainly uses acetic acid, and the three washing times of ultrasonic pickling, ultrasonic alcohol cleaning, and ultrasonic deionized water rinsing are not less than 20 minutes, 30 minutes, and 30 minutes respectively; the workpiece in step one is selected from one of various types of ferrite, martensitic steel, austenitic steel, zirconium alloy and titanium alloy.

[0014] Preferably, in step 2, the background vacuum degree of the vacuum chamber of the ion implantation equipment is 1×10 -5 ~1×10 -4Pa, and the heating temperature is 300-500°C. Preferably, in step 2, the ion implantation energy is adjusted to 100-1000 KeV, the ion beam current is adjusted to 1-100 mA, and the ion implantation dosage is 1.0×1016-1.0×1018 atoms / cm 2 .

[0015] Preferably, in step 3, the background vacuum degree of the vacuum chamber of the magnetron sputtering equipment should be less than 1×10 -4 Pa~1×10 - 3 Pa, heated to 100~300℃.

[0016] Preferably, in step three, the Al arc target power supply uses a DC 40-60A, the anode power supply uses a DC 20-30A, the working gas pressure is 1.0-1.5Pa, and the power-on time is not less than 30min.

[0017] Preferably, in step 4, the Al magnetron target power supply is a HiPIMS power supply, and the constant voltage mode is set to 600-800 V, the pulse width is 50-100 μs, and the pulse frequency is 400-600 Hz.

[0018] Preferably, in step 4, the bias power supply is a DC pulse power supply, whose pulse properties are synchronized with the HiPIMS power supply, the bias voltage is set to 100~300V, the working gas pressure should be 1.0~1.5Pa, and the Al base layer thickness is 100~300nm.

[0019] Preferably, in step 5, the FeCrAlY magnetron target power supply is a HiPIMS power supply, and the constant voltage mode is set to 600-800V, the pulse width is 50-100μs, and the pulse frequency is 400-600Hz.

[0020] Preferably, the composition ratio of FeCrAlY is as follows: Fe: 60~70ωt%; Cr: 10~20ωt%; Al: 5~15ωt%; Y: 0.3~0.5ωt%.

[0021] Preferably, the total thickness of the FeCrAlY coating should be 10-15 μm. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a cross-sectional microstructure image of a FeCrAlY protective coating obtained on a 304 stainless steel surface in Example 1 of the present invention.

[0023] Figure 2 This is a surface microstructure image of a FeCrAlY protective coating obtained on a 304 stainless steel surface in Example 1 of the present invention.

[0024] Figure 3This is a diagram of the ion implantation SRIM simulation results of Example 1 of the present invention. DETAILED DESCRIPTION

[0025] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0026] Example 1

[0027] This embodiment includes the following steps:

[0028] Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying are performed on the 304 stainless steel substrate in sequence, and the three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively;

[0029] Step 2: Place the cleaned 304 stainless steel substrate in the vacuum chamber of the ion implantation equipment, install the Al target, and adjust the background vacuum degree of the vacuum chamber of the ion implantation equipment to 8×10 -5 Pa and heated to 400 °C, turned on the ion implantation source, adjusted the ion implantation energy to 500 KeV, adjusted the ion beam intensity to 50 mA, and the ion implantation metering to 1.0 × 1017 atoms / cm 2 , open the baffle, when the ion injection metering reaches the preset value, close the baffle, turn off the ion source, wait until the temperature of the 304 stainless steel substrate drops below 100°C, and then turn off the vacuum system;

[0030] Step 3: Place the 304 stainless steel substrate obtained in step 2 into the magnetron sputtering vacuum chamber and adjust the background vacuum of the magnetron sputtering vacuum chamber to 5×10 -4 Pa and heated to 200 ° C, turned on the ion implantation source, turned on the Al arc target source and anode source of the physical vapor deposition equipment, the Al arc target power supply used a DC 50A, the anode power supply used a DC 25A, shielded the arc source, introduced argon gas to a working pressure of 1.2Pa, and performed arc enhanced plasma etching cleaning for 40 minutes to further activate the 304 stainless steel substrate after ion implantation;

[0031] Step 4: Turn off the Al arc target source and anode source, turn on the magnetron Al magnetron target source and bias power supply, and adjust the power supply parameters as follows: the Al magnetron power supply is a HiPIMS power supply, set the constant voltage mode to 700V, the pulse width to 75μs, and the pulse frequency to 500Hz; the bias power supply is a DC pulse power supply, and its pulse properties should be synchronized with the HiPIMS power supply, and the bias size is set to 200V. Adjust the argon gas flux and the working gas pressure in the vacuum chamber to 1.2Pa, deposit the Al base layer, power on for 10 minutes, and the thickness is 100nm;

[0032] Step 5. Turn off the Al magnetron target and turn on the magnetron FeCrAlY magnetron target power supply. The composition ratio of the FeCrAlY magnetron target is Fe:Cr:Al:Y=67:24:8.5:0.5ωt%. The FeCrAlY magnetron target power supply should be a HiPIMS power supply. Set the constant voltage mode to 700V, the pulse width to 75μs, the pulse frequency to 500Hz, for a total of 250min, and the total thickness of the FeCrAlY coating is 10μm;

[0033] Step 6: After running for 250 minutes in step 5, turn off all power supplies and argon gas, wait until the temperature of the magnetron sputtering vacuum chamber drops below 100°C, and then turn off the vacuum system;

[0034] Step 7: Take out the treated 304 stainless steel substrate and perform ultrasonic alcohol cleaning for 30 minutes. After drying, put it into a vacuum bag and store it properly.

[0035] Example 2

[0036] This embodiment includes the following steps:

[0037] Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying are performed on the 304 stainless steel substrate in sequence, and the three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively;

[0038] Step 2: Place the cleaned 304 stainless steel substrate in the vacuum chamber of the ion implantation equipment, install the Al target, and adjust the background vacuum of the vacuum chamber to 8×10 -5 Pa and heated to 400 °C, turned on the ion implantation source, adjusted the ion implantation energy to 300 KeV, adjusted the ion beam intensity to 50 mA, and the ion implantation metering to 1.0 × 10 18 atoms / cm 2 , open the baffle, when the ion injection metering reaches the preset value, close the baffle, turn off the ion source, wait for the sample temperature to drop below 100℃, and then turn off the vacuum system;

[0039] Step 3: Place the activated 304 stainless steel substrate obtained in step 2 into the magnetron sputtering vacuum chamber and adjust the background vacuum of the magnetron sputtering vacuum chamber to 5×10 -4 Pa and heated to 200 ° C, turned on the ion implantation source, turned on the Al arc target source and anode source of the physical vapor deposition equipment, the Al arc target power supply used a DC 45A, the anode power supply used a DC 30A, shielded the arc source, introduced argon gas to a working pressure of 1.5Pa, and performed arc enhanced plasma etching cleaning for 30 minutes to further activate the 304 stainless steel substrate after ion implantation;

[0040] Step 4: Turn off the Al arc target source and anode source, turn on the magnetron Al magnetron target source and bias power supply, and adjust the power supply parameters as follows: the Al magnetron power supply should be a HiPIMS power supply, set the constant voltage mode to 800V, the pulse width to 80μs, and the pulse frequency to 400Hz; the bias power supply should be a DC pulse power supply, and its pulse properties should be synchronized with the HiPIMS power supply, and the bias size should be set to 100V. Adjust the argon gas flux and the working gas pressure in the vacuum chamber to 1.5Pa, deposit the Al base layer, power on for 10 minutes, and the thickness is 200nm;

[0041] Step 5. Turn off the Al magnetron target and turn on the magnetron FeCrAlY magnetron target power supply. The composition ratio of the FeCrAlY magnetron target is Fe:Cr:Al:Y=63:24:12.5:0.5ωt%. The FeCrAlY magnetron target power supply should be a HiPIMS power supply. Set the constant voltage mode to 800V, the pulse width to 80μs, the pulse frequency to 400Hz, for a total of 250min, and the total thickness of the FeCrAlY coating is 12μm;

[0042] Step 6: After running for 250 minutes in step 5, turn off all power supplies and argon gas, wait until the temperature of the magnetron sputtering vacuum chamber drops below 100°C, and then turn off the vacuum system;

[0043] Step 7: Take out the treated 304 stainless steel substrate and perform ultrasonic alcohol cleaning for 30 minutes. After drying, put it into a vacuum bag and store it properly.

[0044] Example 3

[0045] This embodiment includes the following steps:

[0046] Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying are performed on the 304 stainless steel substrate in sequence, and the three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively;

[0047] Step 2: Place the cleaned substrate in the vacuum chamber of the ion implantation equipment, install the Al target, and adjust the background vacuum of the vacuum chamber to 8×10 -5 Pa and heated to 400 °C, turned on the ion implantation source, adjusted the ion implantation energy to 800 KeV, adjusted the ion beam intensity to 50 mA, and the ion implantation metering to 1.0 × 10 16 atoms / cm 2 , open the baffle, when the ion injection metering reaches the preset value, close the baffle, turn off the ion source, wait for the sample temperature to drop below 100℃, and then turn off the vacuum system;

[0048] Step 3: Place the 304 stainless steel substrate obtained in step 2 into the magnetron sputtering vacuum chamber and adjust the background vacuum of the magnetron sputtering vacuum chamber to 5×10 -4Pa and heated to 200 ° C, turned on the ion implantation source, turned on the Al arc target source and anode source of the physical vapor deposition equipment, the Al arc target power supply used a DC 60A, the anode power supply used a DC 40A, shielded the arc source, introduced argon gas to a working pressure of 1.0Pa, and performed plasma enhanced etching cleaning for 40 minutes to further activate the 304 stainless steel substrate after ion implantation;

[0049] Step 4: Turn off the Al arc target source and anode source, turn on the magnetron Al magnetron target source and bias power supply, and adjust the power supply parameters as follows: the Al magnetron power supply should be a HiPIMS power supply, set the constant voltage mode to 600V, pulse width to 70μs, and pulse frequency to 600Hz; the bias power supply should be a DC pulse power supply, and its pulse properties should be synchronized with the HiPIMS power supply, and the bias voltage should be set to 200V. Adjust the argon gas flux and the working gas pressure in the vacuum chamber to 1.0Pa, deposit the Al base layer, power on for 15min, and the thickness is 100nm;

[0050] Step 5. Turn off the Al magnetron target and turn on the magnetron FeCrAlY magnetron target power supply. The composition ratio of the FeCrAlY magnetron target is Fe:Cr:Al:Y=67:28:4.5:0.5ωt%. The FeCrAlY magnetron target power supply should be a HiPIMS power supply. Set the constant voltage mode to 600V, the pulse width to 70μs, the pulse frequency to 600Hz, for a total of 280min, and the total thickness of the FeCrAlY coating is 10μm.

[0051] Step 6: After step 5 has been running for 280 minutes, turn off all power supplies and argon gas, wait until the temperature of the magnetron sputtering vacuum chamber drops below 100°C, and then turn off the vacuum system;

[0052] Step 7: Take out the treated 304 stainless steel substrate and perform ultrasonic alcohol cleaning for 30 minutes. After drying, put it into a vacuum bag and store it properly.

[0053] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology, characterized in that: The following steps are involved: Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, dehydration and drying of the workpiece in sequence; Step 2: Place the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, install an Al target, adjust the background vacuum degree of the vacuum chamber of the ion implantation equipment and heat it, turn on the ion implantation source, adjust the ion implantation energy, ion beam current intensity and ion implantation metering, open the baffle, and when the ion implantation metering reaches a preset value, close the baffle, turn off the ion source, wait until the temperature of the workpiece drops to less than 100° C., and turn off the vacuum system; wherein, the ion implantation energy is adjusted to 100-1000 KeV, the ion beam current intensity is adjusted to 1-100 mA, and the ion implantation metering is 1.0×10 16 ~1.0×10 18 atoms / cm 2 ; Step 3, placing the workpiece processed in step 2 into a magnetron sputtering vacuum chamber, adjusting the background vacuum degree of the magnetron sputtering vacuum chamber and heating it, turning on the ion implantation source, turning on the Al arc target source and anode source of the physical vapor deposition equipment, shielding the arc source, introducing argon gas to the working pressure, and performing arc enhanced plasma etching cleaning; Step 4: turn off the Al arc target source and the anode source, turn on the magnetron Al target source and the bias power supply, adjust the power supply parameters, adjust the argon gas flux and the working gas pressure in the vacuum chamber, and deposit the Al base layer; Step 5: based on the operation of step 4, start the magnetron FeCrAlY target source and adjust the power supply parameters to perform coating plating; Step 6: After the step 5 is executed for a predetermined time, the power supplies and the argon gas are turned off, and the vacuum system is turned off when the temperature of the magnetron sputtering vacuum chamber drops below 100° C.; Step 7, taking out the treated workpiece, performing ultrasonic alcohol cleaning, and placing it in a vacuum bag after drying; The pickling in step one mainly uses acetic acid, and the three washing times of ultrasonic pickling, ultrasonic alcohol cleaning, and ultrasonic deionized water rinsing are not less than 20 minutes, 30 minutes, and 30 minutes respectively; the workpiece in step one is selected from one of various types of ferrite, martensitic steel, austenitic steel, zirconium alloy and titanium alloy.

2. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step 2, the background vacuum degree of the vacuum chamber of the ion implantation equipment is 1×10 -5 ~1×10 - 4 Pa, heating temperature is 300~500℃.

3. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In step 3, the background vacuum degree of the vacuum chamber of the magnetron sputtering equipment should be less than 1×10 -4 ~1×10 -3 Pa, heated to 100~300℃.

4. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step three, the Al arc target power supply uses a DC 40-60A, the anode power supply uses a DC 20-30A, the working gas pressure is 1.0-1.5Pa, and the power-on time is not less than 30min.

5. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step 4, the Al magnetron target power supply is a HiPIMS power supply, and the constant voltage mode is set to 600-800V, the pulse width is 50-100μs, and the pulse frequency is 400-600Hz.

6. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step 4, the bias power supply is a DC pulse power supply, and its pulse properties are synchronized with the HiPIMS power supply. The bias voltage is set to 100-300V, the working gas pressure should be 1.0-1.5Pa, and the thickness of the Al base layer is 100-300nm.

7. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step 5, the power supply of the FeCrAlY magnetron target is a HiPIMS power supply, and the constant voltage mode is set to 600-800V, the pulse width is 50-100μs, and the pulse frequency is 400-600Hz.

8. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: The composition ratio of FeCrAlY is as follows: Fe: 60~70wt%; Cr: 10~20wt%; Al: 5~15wt%; Y: 0.3~0.5wt%.

9. The method for preparing a FeCrAlY wear-corrosion resistant coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: The total thickness of the FeCrAlY coating should be 10~15μm.

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