A Mo-Ni coating preparation method based on HiPIMS and ion implantation technology

Abstract

The present invention mainly proposes a method for preparing a Mo-Ni coating based on HiPIMS and ion implantation technology, including cleaning a workpiece with a DLC film on its surface and then dehydrating and drying it; placing the workpiece in a vacuum chamber of an ion implantation device for ion implantation; placing the workpiece after the treatment in step 2 in a magnetron sputtering vacuum chamber, evacuating the chamber and performing arc-enhanced plasma etching cleaning; depositing a Mo / Ni diffusion-proof layer; turning on a magnetron Ni / Mo target source to plate a coating; shutting down the machine for sampling; taking out the workpiece for ultrasonic alcohol cleaning, and storing it in a vacuum bag after drying. The present invention combines HiPIMS and ion implantation technology, uses ion implantation to improve the lattice and expansion coefficient matching between the substrate and the coating to reduce the internal stress between the film and the substrate, uses HiPIMS technology to prepare a protective Mo-Ni coating with high bonding strength on the DLC film, and at the same time relieves the internal stress of the DLC film, significantly improving the service life of the workpiece.

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 Mo-Ni coating with high bonding strength on a DLC film surface based on HiPIMS and ion implantation technology. Background Art

[0002] DLC film, or Diamond-like Carbon films, is a thin film material that has emerged in recent years. It has attracted much attention because of its excellent properties of both diamond and graphite. DLC film has excellent thermal conductivity and electrical conductivity, and is often used in electronic devices, solar energy and other fields. It is also used in the medical field because of its chemical inertness and is considered to have good biological compatibility. Although it has high hardness and lubrication and wear resistance, it is thin, with the thickest being only a few microns. It needs to be plated with a protective coating to extend its service life when used in wear environments such as mechanical and windy sand. In addition, DLC and the metal substrate have large stress due to lattice mismatch, and the manufacturing process itself will also introduce a lot of stress, making it very easy to peel off, reducing its engineering life. Summary of the invention

[0003] Based on the above problems, the present invention proposes a preparation method for forming a Mo-Ni coating on the surface of a DLC film based on HiPIMS and ion implantation technology. HiPIMS, i.e. High Power Impulse Magnetron Sputtering, is an emerging PVD coating technology, and has a large number of successful application cases in the field of hard wear-resistant coatings. The present invention utilizes the excellent wear resistance and high temperature stability of the Mo-Ni alloy coating, and then uses the HiPIMS preparation process to make the Mo-Ni coating have excellent film-based bonding. Metal particles are implanted into the DLC film through ion implantation technology to generate reverse stress to relieve its internal stress, and at the same time form a structure that matches the metal crystal structure to enhance its bonding. The present invention combines HiPIMS and ion implantation technology to prepare a protective Mo-Ni coating with high bonding strength on the DLC film, while alleviating the internal stress of the DLC film, significantly improving the service life of related devices.

[0004] The technical solution of the present invention is: a method for preparing a Mo-Ni coating based on HiPIMS and ion implantation technology, comprising the following steps:

[0005] Step 1: ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying are performed on the workpiece with the DLC film on the surface in sequence;

[0006] Step 2, placing the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, installing the Mo / Ni 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;

[0007] Step 3, placing the workpiece processed in step 2 into a magnetron sputtering vacuum chamber, adjusting the background vacuum of the magnetron sputtering vacuum chamber and heating it, turning on the ion implantation source, turning on the Mo 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 and cleaning to further activate the DLC film after ion implantation and promote the uniform diffusion of the implanted particles;

[0008] Step 4: turn off the Mo / Ni arc target source and the anode source, turn on the magnetron Mo / Ni target source and the bias power supply, adjust the power supply parameters, adjust the argon gas flux and the working gas pressure in the magnetron sputtering vacuum chamber, and deposit the Mo / Ni anti-diffusion layer;

[0009] Step 5: start the magnetron Ni / Mo target source based on the operation in step 4, and gradually increase the power of the Ni / Mo target power supply;

[0010] 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;

[0011] Step 7: After taking out the workpiece, perform ultrasonic alcohol cleaning, dry it and put it into a vacuum bag.

[0012] Preferably, the pickling in step one is performed using acetic acid, wherein the three washing times of ultrasonic pickling, ultrasonic alcohol cleaning, and ultrasonic deionized water rinsing are not less than 20 min, 30 min, and 30 min, respectively.

[0013] Preferably, the background vacuum degree of the vacuum chamber of the ion implantation equipment should be less than 1×10 -4 Pa, heating temperature is 300~500℃.

[0014] Preferably, in step 2, the ion implantation energy is adjusted to 1-3 MeV, 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 .

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

[0016] Preferably, in step three, the Mo / Ni 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 Mo / Ni 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 is 1.0~1.5Pa, and the thickness of the anti-diffusion Mo layer is 300~500nm.

[0019] Preferably, in step five, the Ni / Mo target power supply is a HiPIMS power supply, and the constant voltage mode is set to gradually increase from 300 V to 800 V, with the number of changes being no less than 50 times, and the time interval for each change being consistent, the pulse width is set to remain unchanged at 50~100 μs, and the pulse frequency is set to remain unchanged at 400~600 Hz.

[0020] Preferably, the total thickness of the Mo-Ni coating is 8-10 μm.

[0021] Compared with the prior art, the present invention has the following advantages:

[0022] 1. In order to solve the problem that the DLC film of common DLC film-related devices is prone to peeling due to excessive stress during use, and the bonding strength of the protective coating plated on its surface is not high, ion implantation of Mo / Ni ions with the same lattice as the substrate and the protective coating can effectively improve the stress environment and enhance the bonding strength of the DLC film itself and its protective coating.

[0023] 2. Solve the difficulties encountered in the application environment of DLC film-related devices such as mechanical wear and wind and sand erosion. By selecting Mo-Ni protective coating with excellent wear resistance and high temperature stability, the stability and service life of DLC film-related devices can be significantly improved, broadening its application prospects in more demanding application environments.

[0024] 3. To solve the problems of large environmental pollution, poor coating adhesion, and uneven coating that may be encountered by commonly used coating methods such as electroplating and DC magnetron sputtering, the present invention uses HiPIMS coating technology to coat Mo-Ni protective coatings, and increases plasma density and energy through megawatt-level instantaneous power, thereby improving the coating film-base adhesion. At the same time, by increasing the sputtering particle energy, two different crystal structure elements of Mo and Ni can be mixed to form a single crystal structure, significantly improving the coating performance and stability. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a cross-sectional microstructure image of a Mo-Ni gradient protective coating obtained on the surface of a DLC film in Example 1 of the present invention;

[0026] Figure 2 This is a surface microstructure image of a Mo-Ni gradient protective coating obtained on the surface of a DLC film in Example 1 of the present invention;

[0027] Figure 3 This is a diagram of the ion implantation SRIM simulation results of Example 1 of the present invention. DETAILED DESCRIPTION

[0028] 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.

[0029] Example 1

[0030] This embodiment includes the following steps:

[0031] Step 1: The workpiece with the DLC film on the surface is subjected to ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying in sequence. The three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively.

[0032] Step 2: Place the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, install the Mo 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 3 MeV, adjusted the ion beam current to 50 mA, and the ion implantation metering to 1.0 × 10 17 atoms / cm 2 , open the baffle, when the ion injection dosage reaches the preset value, close the baffle, turn off the ion source, wait until the workpiece temperature drops below 100℃, and then turn off the vacuum system.

[0033] Step 3: Place the workpiece processed in step 2 into the magnetron sputtering vacuum chamber and adjust the background vacuum degree 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 Mo arc target source and anode source of the physical vapor deposition equipment, the Mo arc target power supply uses a DC 50A, the anode power supply uses a DC 25A, shielded the arc source, introduced argon gas to a working pressure of 1.2Pa, and performed plasma enhanced etching and cleaning for 40 minutes to further activate the DLC film after ion implantation and promote the uniform diffusion of the injected particles.

[0034] Step 4: Turn off the Mo arc target source and anode source, turn on the magnetron Mo target source and bias power supply, and adjust the power supply parameters as follows: the Mo target 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 voltage is set to 200V. Adjust the argon gas flux and the working gas pressure in the magnetron sputtering vacuum chamber to 1.2Pa, deposit the Mo resistance diffusion layer, power on for 10min, and the thickness is 400nm.

[0035] Step 5: Based on the operation in step 4, start the magnetron Ni target source and gradually increase the Ni target power supply. The adjustment parameters are as follows: the Ni target power supply is the HiPIMS power supply. Set the constant voltage mode to gradually increase from 300V to 800V, increase by 10V each time, change the time interval for 5min each time, set the pulse width to 75μs unchanged, set the pulse frequency to 500Hz unchanged, for a total of 250min, and the total thickness of the Mo-Ni coating is 10μm.

[0036] 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.

[0037] Step 7. After taking out the workpiece, perform ultrasonic alcohol cleaning for 30 minutes, and then put it into a vacuum bag for proper storage after drying.

[0038] Example 2

[0039] This embodiment includes the following steps:

[0040] Step 1: The workpiece with the DLC film on the surface is subjected to ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying in sequence. The three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively.

[0041] Step 2: Place the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, install the Ni 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 3 MeV, adjusted the ion beam current to 50 mA, and the ion implantation metering to 1.0 × 10 17 atoms / cm 2 , open the baffle, when the ion injection dosage reaches the preset value, close the baffle, turn off the ion source, wait until the workpiece temperature drops below 100℃, and then turn off the vacuum system.

[0042] Step 3: Place the workpiece processed in step 2 into the magnetron sputtering vacuum chamber and adjust the background vacuum degree of the magnetron sputtering vacuum chamber to 5×10 -4Pa and heated to 200°C, turned on the ion implantation source, turned on the Ni arc target source and anode source of the physical vapor deposition equipment, used a DC 50A for the Ni arc target power supply and a DC 25A for the anode power supply, shielded the arc source, introduced argon gas to a working pressure of 1.2Pa, and performed plasma enhanced etching and cleaning for 40min to further activate the DLC film after ion implantation and promote the uniform diffusion of the injected particles.

[0043] Step 4: Turn off the Ni arc target source and anode source, turn on the magnetron Ni target source and bias power supply, and adjust the power supply parameters as follows: the Ni target 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 magnetron sputtering vacuum chamber to 1.2Pa, deposit the Ni resistance diffusion base layer, power on for 10min, and the thickness is 400nm.

[0044] Step 5: Based on the operation in step 4, start the magnetron Mo target source and gradually increase the power of the Mo target power supply. The adjustment parameters are as follows: the Mo target power supply is a HiPIMS power supply. Set the constant voltage mode to gradually increase from 300V to 800V, increase by 10V each time, change the time interval for 5min each time, set the pulse width to 75μs unchanged, set the pulse frequency to 500Hz unchanged, for a total of 250min, and the total thickness of the Mo-Ni coating is 10μm.

[0045] 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.

[0046] Step 7. After taking out the workpiece, perform ultrasonic alcohol cleaning for 30 minutes, and then put it into a vacuum bag for proper storage after drying.

[0047] Example 3

[0048] This embodiment includes the following steps:

[0049] Step 1: The workpiece with the DLC film on the surface is subjected to ultrasonic pickling, ultrasonic alcohol cleaning, ultrasonic deionized water rinsing, and dehydration and drying in sequence. The three cleaning steps are performed for 30 minutes, 40 minutes, and 40 minutes respectively.

[0050] Step 2: Place the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, install the Mo / Ni 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 2 MeV, adjusted the ion beam intensity to 100 mA, and the ion implantation metering to 1.0 × 10 18atoms / cm 2 , open the baffle, when the ion injection dosage reaches the preset value, close the baffle, turn off the ion source, wait for the workpiece temperature to drop below 100℃, and then turn off the vacuum system.

[0051] Step 3: Place the processed workpiece into the magnetron sputtering vacuum chamber and adjust the background vacuum degree 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 Mo arc target source and anode source of the physical vapor deposition equipment, the Mo arc target power supply uses a DC 60A, the anode power supply uses a DC 30A, shielded the arc source, introduced argon gas to a working gas pressure of 1.5Pa, and performed plasma enhanced etching and cleaning for 40 minutes to further activate the DLC film after ion implantation and promote the uniform diffusion of the injected particles.

[0052] Step 4: Turn off the Mo arc target source and anode source, turn on the magnetron Mo target source and bias power supply, and adjust the power supply parameters as follows: the Mo target power supply is a HiPIMS power supply, set the constant voltage mode to 800V, the pulse width to 100μs, and the pulse frequency to 600Hz; 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 magnetron sputtering vacuum chamber to 1.5Pa, deposit the Mo resistance diffusion base layer, power on for 10min, and the thickness is 600nm.

[0053] Step 5: Based on the operation in step 4, start the magnetron Ni target source and gradually increase the Ni target power supply. The adjustment parameters are as follows: the Ni target power supply is the HiPIMS power supply. Set the constant voltage mode to gradually increase from 300V to 800V, increase by 10V each time, change the time interval for 5min each time, set the pulse width to 100μs unchanged, set the pulse frequency to 600Hz unchanged, for a total of 230min, and the total thickness of the Mo-Ni coating is 10μm.

[0054] Step 6: After running for 230 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.

[0055] Step 7. After taking out the workpiece, perform ultrasonic alcohol cleaning for 30 minutes, and then put it into a vacuum bag for proper storage after drying.

[0056] 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 Mo-Ni 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, and dehydration and drying are performed on the workpiece with the DLC film on the surface in sequence; Step 2: Place the workpiece processed in step 1 in the vacuum chamber of the ion implantation equipment, install the Mo / Ni 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 the 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; in step 2, adjust the ion implantation energy to 1~3MeV, adjust the ion beam current intensity to 1~100mA, and the ion implantation metering 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 of the magnetron sputtering vacuum chamber and heating it, turning on the ion implantation source, turning on the Mo / Ni arc target source and anode source of the physical vapor deposition equipment, shielding the arc source, introducing argon gas to the working pressure, performing arc enhanced plasma etching and cleaning, further activating the DLC film after ion implantation and promoting uniform diffusion of the implanted particles; in step 3, the Mo / Ni arc target power supply uses a DC 40-60A, the anode power supply uses a DC 20~30A, the working pressure is 1.0~1.5Pa, and the power-on time is not less than 30min; Step 4: turn off the Mo / Ni arc target source and the anode source, turn on the magnetron Mo / Ni target source and the bias power supply, adjust the power supply parameters, adjust the argon flux and the working pressure in the magnetron sputtering vacuum chamber, and deposit the Mo / Ni anti-diffusion layer; in the step 4, the bias power supply is a DC pulse power supply, the pulse property of which is synchronized with the HiPIMS power supply, the bias voltage is set to 100~300V, the working pressure is 1.0~1.5Pa, and the thickness of the anti-diffusion Mo layer is 300~500nm; Step 5, based on the operation of step 4, the magnetron Ni / Mo target source is turned on, and the power of the Ni / Mo target power supply is gradually increased; in step 5, the Ni / Mo target power supply is a HiPIMS power supply, and the constant voltage mode is set to gradually increase from 300V to 800V, the number of changes is not less than 50 times, and the time interval for each change is consistent, the pulse width is set to 50~100μs unchanged, and the pulse frequency is set to 400~600Hz unchanged; 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; Step 7: After taking out the workpiece, perform ultrasonic alcohol cleaning, dry it, and put it into a vacuum bag.

2. The method for preparing a Mo-Ni coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: The pickling in step 1 is performed using acetic acid, wherein 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.

3. The method for preparing a Mo-Ni 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 should be less than 1×10 -4 Pa, heating temperature is 300~500℃.

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

5. The method for preparing a Mo-Ni coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: In the step 4, the Mo / Ni 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 Mo-Ni coating based on HiPIMS and ion implantation technology according to claim 1, characterized in that: The total thickness of the Mo-Ni coating is 8-10 μm.

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