CN115612998B - Magnesium alloy surface lubricating wear-resistant composite film and preparation method thereof - Google Patents
Magnesium alloy surface lubricating wear-resistant composite film and preparation method thereof Download PDFInfo
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- CN115612998B CN115612998B CN202211593975.0A CN202211593975A CN115612998B CN 115612998 B CN115612998 B CN 115612998B CN 202211593975 A CN202211593975 A CN 202211593975A CN 115612998 B CN115612998 B CN 115612998B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention discloses a magnesium alloy surface lubricating wear-resistant composite film and a preparation method thereof, and relates to the technical field of magnesium alloy surface treatment. The preparation method of the magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps: after the surface of the magnesium alloy is pretreated, an Al layer and Al are sequentially sputtered by adopting a magnetron sputtering method 2 O 3 Layer, moS 2 Layer of Al/Al 2 O 3 /MoS 2 And (5) compounding the film layer. The thickness of the Al layer in the magnesium alloy surface lubricating wear-resistant composite film layer is 7 to 9um 2 O 3 The layer thickness is 3 to 5um 2 The thickness of the layer is 2 to 3um, the surface of the film layer is distributed with near-circular nano-scale particle substances, under the action of the composite film layer, the magnesium alloy not only has good corrosion resistance, but also has excellent comprehensive friction performance, and meets the requirements of certain corrosion resistance and good tribology performance when the magnesium alloy is used as a moving part.
Description
Technical Field
The invention relates to the technical field of magnesium alloy surface treatment, in particular to a magnesium alloy surface lubricating wear-resistant composite film and a preparation method thereof.
Background
Magnesium alloy is the lightest metal material with an engineering structure, has the characteristics of low density, low strength, reproducibility and the like, is more and more widely applied to the fields of machinery, automobiles, aerospace, communication and the like, however, compared with the aluminum alloy with the same light weight, although the density of the magnesium alloy is reduced by one third, the magnesium has more active chemical properties and is more likely to react with oxygen in the air and the like in the using process so as to corrode, so the corrosion resistance of the magnesium alloy is usually improved by adopting a surface modification treatment process.
The common surface treatment methods of magnesium alloy include chemical treatment, electroplating, anodic oxidation, micro-arc oxidation and the like, wherein micro-arc oxidation technology (MAO) is used as a newer surface treatment process, so that a ceramic film layer is generated on the surface of the magnesium alloy in situ, and the corrosion resistance of the magnesium alloy can be improved.
However, when the magnesium alloy is used as a moving part, the magnesium alloy is required to have not only good corrosion resistance but also better comprehensive friction performance including better wear resistance, lubricating antifriction performance and the like on the surface, and oxides such as MgO and the like in a film layer formed by the magnesium alloy in the micro-arc oxidation process have high hardness and good wear resistance, but the friction coefficient is higher, the lubricating antifriction performance is poor, meanwhile, the wear resistance life is shorter, and the comprehensive friction performance is obviously poor.
Therefore, a magnesium alloy surface treatment film layer is needed, so that the magnesium alloy surface has good corrosion resistance and excellent comprehensive friction performance.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a magnesium alloy surface lubricating wear-resistant composite film layer and a preparation method thereof. Specifically, the invention adopts a magnetron sputtering method to sequentially sputter an Al layer and Al on the surface of the magnesium alloy 2 O 3 Layer and MoS 2 Layer of Al/Al 2 O 3 /MoS 2 The magnesium alloy surface lubricating wear-resistant composite film layer not only has good corrosion resistance, but also has excellent wear resistance and antifriction performance, and can meet the performance requirements when the magnesium alloy is used as a moving part.
In order to realize the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer, which comprises the following steps:
(1) Performing surface pretreatment on a magnesium alloy sample;
(2) Sputtering an Al film on the magnesium alloy sample subjected to surface pretreatment in the step (1) by adopting an Al target material;
(3) Changing the target material to Al 2 O 3 A target formed by sputtering Al on the magnesium alloy sample having the Al film adhered to the surface thereof in the step (2) 2 O 3 A film;
(4) Changing target material to MoS 2 Target, al film and Al are adhered on the surface of the step (3) 2 O 3 Sputtering of MoS on magnesium alloy samples of films 2 And (5) taking out the magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film layer.
Preferably, in the step (1), the magnesium alloy is one of AZ91D magnesium alloy, AZ31B magnesium alloy, AM60 magnesium alloy or WE43 magnesium alloy.
Preferably, in the step (1), the method for pretreating the surface of the magnesium alloy sample comprises the following steps: and (3) sequentially polishing the magnesium alloy sample by using abrasive paper of SiC of 150#, 400#, 1000#, and 2000#, putting the magnesium alloy sample into an acetone solution and deionized water for ultrasonic cleaning for 5-10 min after polishing, taking out the magnesium alloy sample, and drying the magnesium alloy sample.
Preferably, in the step (2), the method for magnetron sputtering of the Al film comprises: and (2) placing the magnesium alloy sample subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target and the magnesium alloy sample to be 90mm, closing the vacuum chamber for vacuumizing, introducing argon, carrying out sputtering cleaning on the target, then adjusting the flow rate of the argon and the air pressure of the vacuum chamber, and sputtering a layer of Al film on the surface of the magnesium alloy sample.
Further preferably, the purity of the Al target is more than or equal to 99.99%, and the sputtering and cleaning parameters of the target are as follows: degree of vacuum of 2X 10 -4 ~7×10 -4 Pa, argon flow of 150-250sccm, and sputtering cleaning time of 5-20min; the parameters of the sputtered Al film are as follows: argon flow is 40 to 60sccm, vacuum chamber pressure is 1.0 to 2.0Pa, sputtering time is 0.5 to 10h, sputtering power is 50 to 300W, and sputtering temperature is 100 to 180 ℃.
Preferably, in step (3), al 2 O 3 The target purity is more than or equal to 99.99 percent, and the sputtering and cleaning parameters of the target are as follows: degree of vacuum of 2X 10 -4 ~7×10 -4 Pa, argon flow of 150-250sccm, and sputtering cleaning time of 5-20min; sputtering of Al 2 O 3 The parameters of the membrane were: argon flow of 40 to 60sccm, vacuum chamber pressure of 1.0 to 2.0Pa, sputtering time of 0.5 to 5h, sputtering power of 100 to 380W and sputtering temperature of room temperature。
Preferably, in step (4), moS 2 The target purity is more than or equal to 99.99 percent, and the sputtering and cleaning parameters of the target are as follows: degree of vacuum of 2X 10 -4 ~7×10 -4 Pa, argon flow of 150-250sccm, and sputtering cleaning time of 5-20min; sputtering of MoS 2 The parameters of the membrane were: argon flow is 40 to 60sccm, vacuum chamber pressure is 1.0 to 2.0Pa, sputtering time is 0.5 to 7h, sputtering power is 100 to 300W, and sputtering temperature is room temperature.
The invention provides a magnesium alloy surface lubricating wear-resistant composite film layer, which is formed by sequentially arranging an Al layer and an Al layer from inside to outside on a magnesium alloy substrate 2 O 3 Layer and MoS 2 Layer of Al/Al 2 O 3 /MoS 2 And (5) compounding a film layer.
Preferably, the thickness of the Al layer is 7 to 9um 2 O 3 The layer thickness is 3 to 5um 2 The layer thickness is 2 to 3um.
The invention has the beneficial effects that:
1. the invention adopts a magnetron sputtering method to form a layer of Al/Al on the surface of the magnesium alloy 2 O 3 / MoS 2 The composite film layer adopts the Al film as the bottommost layer of the composite film to be connected with the magnesium alloy, and is close to the atomic structure of the magnesium alloy substrate, so that the mutual solubility of the Al film and the magnesium alloy substrate is good, and the bonding force of the composite film layer and the magnesium alloy substrate can be greatly improved.
2. In the magnesium alloy surface lubricating wear-resistant composite film layer, al is selected 2 O 3 The film being an intermediate layer of a composite film layer, al 2 O 3 The film has good compactness, strong capability of isolating corrosive media, high hardness and good wear resistance, and is easy to combine with Al, so that the layer can be used as an intermediate layer to further improve the combination of the composite film layer and a matrix, and can greatly improve the corrosion resistance and wear resistance of the whole magnesium alloy surface lubricating wear-resistant composite film layer.
3. In the invention, al film and Al are coated 2 O 3 Film and MoS 2 The film is attached to the surface of the magnesium alloy in sequence, thereby ensuring that the surface of the magnesium alloy is ensuredThe lubricating wear-resistant composite film layer is tightly combined with the magnesium alloy matrix, and can give full play to the Al film and the Al 2 O 3 The film has better corrosion resistance and wear resistance, and simultaneously gives full play to MoS 2 The lubricating and antifriction properties are excellent, and the friction life is obviously prolonged, so that the corrosion resistance and the comprehensive friction performance of the magnesium alloy matrix are ensured.
Drawings
FIG. 1: (a) A scanning electron microscope image of the surface appearance of the magnesium alloy surface lubricating wear-resistant composite film obtained in the example 1, (b) a scanning electron microscope image of the cross-sectional appearance of the magnesium alloy surface lubricating wear-resistant composite film obtained in the example 1;
FIG. 2: the Tafel polarization test curve of the magnesium alloy surface lubricating wear-resistant composite film prepared in the embodiment 2, the magnesium alloy matrix in the comparative example 1, the micro-arc oxidation film in the comparative example 2 and the magnesium alloy magnetron sputtering single film in the comparative example 3~5 is obtained;
FIG. 3: the tribology curve of the magnesium alloy surface lubricating wear-resistant composite film prepared in the embodiment 2, the magnesium alloy matrix in the comparative example 1, the micro-arc oxidation film in the comparative example 2 and the magnesium alloy magnetron sputtering single film in the comparative example 3~5 is provided.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background art, because the chemical property of magnesium is very active, the corrosion resistance of magnesium alloy is poor, and when the magnesium alloy is used for manufacturing moving parts, the magnesium alloy is required to have excellent comprehensive friction performance, so that the invention provides a method for preparing Al/Al on the surface of the magnesium alloy by adopting a magnetron sputtering method 2 O 3 / MoS 2 The method for compounding the film and the prepared composite film ensure that the magnesium alloy has good corrosion resistance and friction performance.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Grinding an AZ31B magnesium alloy sample by using SiC sand paper of 150#, 400#, 1000#, 2000# in sequence, polishing, putting into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99% and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing to the vacuum degree of 5 multiplied by 10 - 4 Introducing argon gas with the flow rate of 200sccm, carrying out sputtering cleaning on the Al target material for 10min, then regulating the flow rate of the argon gas to be 45sccm and the air pressure of a vacuum chamber to be 1.1Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 130 ℃, the sputtering power is 200W, and the sputtering time is 5h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Target, closing vacuum chamber and vacuumizing to 5X 10 degree of vacuum - 4 Pa, introducing argon gas with the flow rate of 200sccm for Al 2 O 3 Sputtering and cleaning the target material for 10min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.2Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 150W, and the sputtering time is 2h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Target, closing vacuum chamber and vacuumizing to 5X 10 degree of vacuum - 4 Pa, argon gas is introduced, the flow rate of the argon gas is 200sccm, for MoS 2 Sputtering and cleaning the target for 10min, then adjusting the argon flow to 40sccm and the vacuum chamber pressure to 1.2Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Magnesium alloy of filmSputtering of MoS on a sample 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 200W, and the sputtering time is 2 h.
Example 2
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Sequentially grinding an AZ31B magnesium alloy sample by using 150#, 400#, 1000#, and 2000# SiC abrasive paper, polishing, putting into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99% and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing until the vacuum degree is 5 multiplied by 10 - 4 Introducing argon gas with the flow rate of 200sccm, carrying out sputtering cleaning on the Al target material for 10min, then regulating the flow rate of the argon gas to be 45sccm and the air pressure of a vacuum chamber to be 1.1Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 130 ℃, the sputtering power is 180W, and the sputtering time is 4h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Closing the vacuum chamber, vacuumizing to 5 × 10 - 4 Pa, introducing argon gas with the flow rate of 200sccm for Al 2 O 3 Sputtering and cleaning the target material for 10min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.2Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 160W, and the sputtering time is 2h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Target, closing vacuum chamber and vacuumizing to 5X 10 degree of vacuum - 4 Pa, introducing argon gas with a flow rate of 200sccm for MoS 2 Sputtering and cleaning the target for 10min, then adjusting the argon flow to 40sccm and the vacuum chamber pressure to 1.2Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Magnesium alloy of filmSputtering MoS on gold sample 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 180W, and the sputtering time is 2 h.
Example 3
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Grinding an AZ31B magnesium alloy sample by using sand paper of SiC of 150#, 400#, 1000#, 2000#, polishing, putting into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99% and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing until the vacuum degree is 5 multiplied by 10 - 4 Introducing argon gas with the flow rate of 200sccm, carrying out sputtering cleaning on the Al target material for 10min, then regulating the flow rate of the argon gas to be 45sccm and the air pressure of a vacuum chamber to be 1.1Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 140 ℃, the sputtering power is 200W, and the sputtering time is 6h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Target, closing vacuum chamber and vacuumizing to 5X 10 degree of vacuum - 4 Pa, introducing argon gas with a flow rate of 200sccm for Al 2 O 3 Sputtering and cleaning the target material for 10min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.2Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 150W, and the sputtering time is 2.5h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Target, closing vacuum chamber and vacuumizing to 5X 10 degree of vacuum - 4 Pa, introducing argon gas with a flow rate of 200sccm for MoS 2 Sputtering and cleaning the target for 10min, then adjusting the argon flow to 40sccm and the vacuum chamber pressure to 1.2Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Of membranesSputtering MoS on magnesium alloy sample 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 210W, and the sputtering time is 1.5 h.
Example 4
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Sequentially grinding an AZ91D magnesium alloy sample by using 150#, 400#, 1000#, 2000# SiC abrasive paper, polishing, putting into an acetone solution and deionized water, performing ultrasonic cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99 percent and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing until the vacuum degree is 2 multiplied by 10 - 4 Pa, introducing argon gas with the flow of 150sccm, carrying out sputtering cleaning on the Al target for 5min, then regulating the flow of the argon gas to be 40sccm and the air pressure of a vacuum chamber to be 1.0Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 100 ℃, the sputtering power is 50W, and the sputtering time is 0.5h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Target, closing vacuum chamber and vacuumizing to 2X 10 degree of vacuum - 4 Pa, argon gas with a flow rate of 150sccm for Al 2 O 3 Sputtering and cleaning the target material for 5min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.0Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 100W, and the sputtering time is 0.5h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Target, closing vacuum chamber and vacuumizing to 2X 10 degree of vacuum - 4 Pa, introducing argon gas with flow rate of 150sccm for MoS 2 Sputtering and cleaning the target material for 5min, then adjusting the argon flow to be 40sccm and the vacuum chamber pressure to be 1.0Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Sputtering of MoS on magnesium alloy samples of films 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 100W, and the sputtering time is 0.5 h.
Example 5
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Sequentially grinding an AM60 magnesium alloy sample by using SiC sand paper of 150#, 400#, 1000#, and 2000#, polishing, placing into an acetone solution and deionized water, ultrasonically cleaning for 10min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99% and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing until the vacuum degree is 7 multiplied by 10 - 4 Introducing argon gas with the flow rate of 250sccm, carrying out sputtering cleaning on the Al target material for 20min, then regulating the flow rate of the argon gas to be 60sccm and the air pressure of a vacuum chamber to be 2.0Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 180 ℃, the sputtering power is 300W, and the sputtering time is 10h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Target, closing vacuum chamber and vacuumizing to 7X 10 degree of vacuum - 4 Pa, introducing argon gas with the flow rate of 250sccm for Al 2 O 3 Sputtering and cleaning the target for 20min, then adjusting the argon flow to be 60sccm and the vacuum chamber pressure to be 2.0Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 380W, and the sputtering time is 5h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Closing the vacuum chamber, vacuumizing to 7 × 10 - 4 Pa, introducing argon gas with the flow rate of 250sccm for MoS 2 Sputtering and cleaning the target for 20min, then adjusting the argon flow to 60sccm and the vacuum chamber pressure to 2.0Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Sputtering of MoS on magnesium alloy samples of films 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 300W, and the sputtering time is 7 h.
Example 6
A preparation method of a magnesium alloy surface lubricating wear-resistant composite film layer comprises the following steps:
(1) Sequentially grinding a WE43 magnesium alloy sample by using sand paper of SiC of 150#, 400#, 1000#, 2000#, polishing, putting into an acetone solution and deionized water, ultrasonically cleaning for 8min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99% and a magnesium alloy sample to be 90mm, closing the vacuum chamber, and vacuumizing until the vacuum degree is 4.5 multiplied by 10 - 4 Pa, introducing argon gas with the flow of 200sccm, carrying out sputtering cleaning on the Al target for 13min, then regulating the flow of the argon gas to be 50sccm and the air pressure of a vacuum chamber to be 1.5Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 140 ℃, the sputtering power is 175W, and the sputtering time is 5.5h;
(3) The target material is replaced by Al with the purity of 99.99 percent 2 O 3 Closing the vacuum chamber, vacuumizing to 4.5X 10 - 4 Pa, introducing argon gas with a flow rate of 200sccm for Al 2 O 3 Sputtering and cleaning the target material for 10min, then regulating the argon flow to be 50sccm and the vacuum chamber pressure to be 1.5Pa, and sputtering Al on the magnesium alloy sample with the Al film attached to the surface in the step (2) 2 O 3 The film is prepared by the following steps of (1) forming a film, wherein the sputtering temperature is room temperature, the sputtering power is 240W, and the sputtering time is 5.5h;
(4) The target material is replaced by MoS with the purity of 99.99 percent 2 Target, close the vacuum chamber and vacuumize to 4.5X 10 - 4 Pa, argon gas is introduced, the flow rate of the argon gas is 200sccm, for MoS 2 Sputtering and cleaning the target for 10min, then adjusting the argon flow to 50sccm and the vacuum chamber pressure to 1.5Pa, and attaching an Al film and Al on the surface in the step (3) 2 O 3 Sputtering of MoS on magnesium alloy samples of films 2 And (3) taking out a magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film, wherein the sputtering temperature is room temperature, the sputtering power is 200W, and the sputtering time is 5.5 h.
Comparative example 1
And grinding the AZ31B magnesium alloy sample by using 150#, 400#, 1000#, 2000# SiC abrasive paper in sequence, polishing, putting the sample into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying.
Comparative example 2
The method comprises the following steps of (1) carrying out micro-arc oxidation treatment on an AZ31B magnesium alloy sample:
(1) Performing surface pretreatment on an AZ31B magnesium alloy sample, sequentially grinding with 150#, 400#, 1000#, and 2000# SiC abrasive paper, then performing polishing treatment, respectively putting into an acetone solution and deionized water, performing ultrasonic cleaning for 5min, taking out, and drying;
(2) Connecting the magnesium alloy test sample obtained in the step (1) by using an aluminum wire, then immersing the magnesium alloy test sample into a treatment tank of silicate system electrolyte, connecting the other end of the aluminum wire with the positive electrode of a pulse power supply,
wherein, the silicate system electrolyte consists of 17g/L sodium silicate, 12g/L potassium fluoride, 3g/L sodium hydroxide and 10mL/L glycerol;
(3) And (3) carrying out micro-arc oxidation treatment on the magnesium alloy sample in the step (2), wherein the pulse frequency is 600Hz, the duty ratio is 20%, the voltage is 400V, and the treatment time is 30min.
Comparative example 3
A preparation method of a single Al film layer on the surface of a magnesium alloy comprises the following steps:
(1) Sequentially grinding an AZ31B magnesium alloy sample by using 150#, 400#, 1000#, and 2000# SiC abrasive paper, polishing, putting into an acetone solution and deionized water, performing ultrasonic cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target material with the purity of 99.99 percent and a magnesium alloy sample to be 90mm, and closingVacuum pumping is carried out in the vacuum chamber until the vacuum degree is 5 multiplied by 10 - 4 And Pa, introducing argon gas with the flow rate of 200sccm, carrying out sputtering cleaning on the Al target material for 10min, then regulating the flow rate of the argon gas to be 45sccm and the air pressure of the vacuum chamber to be 1.1Pa, and sputtering a layer of Al film on the surface of the magnesium alloy sample, wherein the sputtering temperature is 130 ℃, the sputtering power is 180W, and the sputtering time is 4h, so as to obtain the single Al film on the surface of the magnesium alloy.
Comparative example 4
Magnesium alloy surface single Al 2 O 3 The preparation method of the film layer comprises the following steps:
(1) Grinding an AZ31B magnesium alloy sample by using SiC sand paper of 150#, 400#, 1000#, 2000# in sequence, polishing, putting into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a turntable of a magnetron sputtering vacuum chamber, and adjusting the purity of Al to 99.99 percent 2 O 3 The distance between the target material and the magnesium alloy sample is 90mm, the vacuum chamber is closed, and the vacuum degree is 5 multiplied by 10 -4 Pa, introducing argon gas with the flow rate of 200sccm for Al 2 O 3 Sputtering and cleaning the target material for 10min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.2Pa, and sputtering Al on the surface of the magnesium alloy sample 2 O 3 The film is formed, wherein the sputtering temperature is room temperature, the sputtering power is 160W, and the sputtering time is 2h, so that the single Al on the surface of the magnesium alloy is obtained 2 O 3 And (3) a membrane.
Comparative example 5
Magnesium alloy surface single MoS 2 The preparation method of the film layer comprises the following steps:
(1) Grinding an AZ31B magnesium alloy sample by using SiC sand paper of 150#, 400#, 1000#, and 2000# in sequence, polishing, putting the sample into an acetone solution and deionized water, ultrasonically cleaning for 5min, taking out the magnesium alloy sample, and drying for later use;
(2) Placing the AZ91D magnesium alloy subjected to surface pretreatment in the step (1) into a turntable of a magnetron sputtering vacuum chamber, and adjusting the purity of MoS to 99.99 percent 2 Target material and magnesium alloyThe distance between the gold samples is 90mm, the vacuum chamber is closed and the vacuum is pumped till the vacuum degree is 5 multiplied by 10 - 4 Pa, argon gas is introduced, the flow rate of the argon gas is 200sccm, for MoS 2 Sputtering and cleaning the target for 10min, then regulating the argon flow to be 40sccm and the vacuum chamber pressure to be 1.2Pa, and sputtering MoS on the surface of the magnesium alloy sample 2 Film, wherein the sputtering temperature is room temperature, the sputtering power is 180W, the sputtering time is 2h, and the magnesium alloy sample is taken out to obtain the single MoS on the surface of the magnesium alloy 2 And (3) a film.
Test example 1
The magnesium alloy surface lubricating wear-resistant composite film layer prepared in example 1 is characterized by a scanning electron microscope, and the result is shown in fig. 1, wherein fig. 1 (a) is a scanning electron microscope photograph of the surface morphology of the obtained magnesium alloy surface lubricating wear-resistant composite film layer, and fig. 1 (b) is a scanning electron microscope photograph of the surface morphology of the magnesium alloy surface lubricating wear-resistant composite film layer obtained in example 1.
As can be seen from fig. 1 (a), the surface of the magnesium alloy surface lubricating wear-resistant composite film is distributed with nearly circular particle substances, most of the particle substances have the size within the range of hundreds of nanometers, no obvious coarse substances and microcracks exist, and the surface quality is good. As clearly seen from FIG. 1 (b), the lubricating and wear-resistant composite film layer on the surface of the magnesium alloy is respectively an Al layer and an Al layer from inside to outside 2 O 3 Layer, moS 2 The thickness of each layer is different, wherein the thickness of the Al layer is the largest and is 7-9um, and the layer is used as a priming layer, so that the characteristics of close atomic structure and good intersolubility with a magnesium matrix are fully exerted, and the bonding capability of the magnesium alloy surface lubricating wear-resistant composite film layer and the matrix can be remarkably improved; second is Al 2 O 3 Layer with a thickness of 3-5um, due to Al 2 O 3 The magnesium alloy surface lubricating wear-resistant composite film has good compactness, strong capability of isolating corrosive media, high hardness and good wear resistance, and is easy to combine with Al, so that the layer serving as an intermediate layer can further improve the combination of the magnesium alloy surface lubricating wear-resistant composite film and a matrix on one hand, and can greatly improve the corrosion resistance and wear resistance of the whole magnesium alloy surface lubricating wear-resistant composite film on the other hand; and the outermost MoS 2 Layer, thickness2-3um, the MoS can be fully exerted 2 The lubricating antifriction performance is excellent, thereby obviously improving the comprehensive friction performance of the lubricating wear-resistant composite film layer on the surface of the magnesium alloy.
Test example 2
The Tafel polarization test curve is carried out on the magnesium alloy surface lubricating wear-resistant composite film layer prepared in the embodiment 2 of the invention, the magnesium alloy substrate in the comparative example 1, the micro-arc oxidation film layer in the comparative example 2 and the magnesium alloy magnetron sputtering single film layer in the comparative example 3~5, and the result is shown in FIG. 2.
The specific test method comprises the steps of adopting a three-electrode system for testing, wherein a test solution is a sodium chloride aqueous solution with the mass fraction of 3.5%, a reference electrode is a saturated calomel electrode, the potential scanning rate is 0.001V/s, fitting is carried out on each polarization curve by adopting a linear extrapolation method, and the fitting result is shown in table 1.
TABLE 1 Tafel polarization curve fitting results for example 2 and comparative example 1~5 film layers
According to the theory related to corrosion electrochemistry, the corrosion potential is more positive, the corrosion current density is smaller, the polarization resistance is larger, the possibility of corrosion is lower, and the corrosion resistance of the material is better. As can be seen from FIG. 2 and Table 1, the magnesium alloy substrate of comparative example 1, the micro-arc oxidation film layer of comparative example 2, and the single Al film of comparative examples 3 to 5 were formed by magnetron sputtering 2 O 3 Membrane, unitary MoS 2 Compared with the film, the magnesium alloy surface lubricating wear-resistant composite film layer obtained by the invention has the advantages that the corrosion potential is obviously shifted forwards, the corrosion current density is respectively reduced by 1-3 orders of magnitude, and the corresponding polarization resistance is respectively improved by 1-3 orders of magnitude, so that the magnesium alloy surface lubricating wear-resistant composite film layer obviously improves the corrosion resistance of a magnesium alloy matrix, and the corrosion resistance of the magnesium alloy surface lubricating wear-resistant composite film layer is superior to that of a micro-arc oxidation film layer and a magnetron sputtering single film layer.
Test example 3
The magnesium alloy surface lubricating wear-resistant composite film prepared in the embodiment 2 of the invention, the magnesium alloy substrate in the comparative example 1, the micro-arc oxidation film in the comparative example 2 and the magnetron sputtering single film in the comparative example 3~5 are subjected to tribology tests, and the results are shown in fig. 3 and table 2.
The test is carried out in an atmospheric environment (the relative humidity is about 30%), a ball-disc type friction abrasion tester is adopted, the friction dual ball is a GCr15 steel ball, the diameter is about 5mm, the rotating speed of the ball relative to the disc is 1000r/min, and the normal load is 10N.
As can be seen from FIG. 3, compared with the magnesium alloy substrate of comparative example 1 and the micro-arc oxidation film layer of comparative example 2, the surface friction coefficient of the magnesium alloy surface lubricating and wear-resistant composite film prepared by the invention is obviously smaller, and the value is in the range of 0.1-0.15; meanwhile, the surface friction coefficient of the composite film layer is obviously smaller than that of the single Al film of comparative example 3 and that of the single Al film of comparative example 4 2 O 3 Film, and MoS Single comparative example 5 2 The films are essentially identical, from which it can be seen that it is due to the surface layer MoS 2 The friction coefficient of the surface of the magnesium alloy surface lubricating wear-resistant composite film is obviously reduced.
As can be seen from Table 2, compared with comparative examples 1-5, the friction life of the magnesium alloy surface lubricating wear-resistant composite film layer obtained by the invention is obviously longer and reaches 52.3 multiplied by 10 4 r is even higher than the sum of the friction lives of all the comparative example film layers, so that the magnesium alloy surface lubricating wear-resistant composite film layer remarkably improves the friction life of the magnesium alloy surface lubricating wear-resistant composite film layer by fully exerting the synergistic action of all the layers.
TABLE 2 Friction Life of example 3 and comparative example 1~5 film layers
Therefore, compared with a micro-arc oxidation film layer, the magnesium alloy surface lubricating wear-resistant composite film layer prepared by the invention has excellent corrosion resistance, more importantly, has good comprehensive friction performance, better lubricating friction-reducing performance and longer wear-resistant and friction service life, and can completely meet the requirements of magnesium alloy on the tribological performance when being used as a moving part.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (6)
1. The preparation method of the magnesium alloy surface lubricating wear-resistant composite film layer is characterized by comprising the following steps:
(1) Performing surface pretreatment on a magnesium alloy sample;
(2) Sputtering an Al film on the magnesium alloy sample subjected to the surface pretreatment in the step (1) by adopting an Al target material;
(3) Changing the target material to Al 2 O 3 A target formed by sputtering Al on the magnesium alloy sample having the Al film adhered to the surface thereof in the step (2) 2 O 3 A film;
(4) Changing the target material to MoS 2 Target, al film and Al are adhered on the surface of the step (3) 2 O 3 Sputtering of MoS on magnesium alloy samples of films 2 Film, taking out the magnesium alloy sample to obtain the magnesium alloy surface lubricating wear-resistant composite film layer;
in the step (2), the method for sputtering the Al film comprises the following steps: putting the magnesium alloy sample subjected to surface pretreatment in the step (1) into a rotating disc of a magnetron sputtering vacuum chamber, adjusting the distance between an Al target and the magnesium alloy sample to be 90mm, closing the vacuum chamber for vacuumizing, introducing argon, carrying out sputtering cleaning on the target, then adjusting the flow rate of the argon and the air pressure of the vacuum chamber, and sputtering a layer of Al film on the surface of the magnesium alloy sample;
the purity of the Al target is more than or equal to 99.99 percent, and the sputtering and cleaning parameters of the target are as follows: vacuum degree of 2X 10 -4 ~7×10 -4 Pa, argon flow of 150-250sccm, and sputtering cleaning time of 5-20min;
the parameters of the sputtered Al film are: argon flow is 40 to 60sccm, vacuum chamber pressure is 1.0 to 2.0Pa, sputtering time is 0.5 to 10h, sputtering power is 50 to 300W, and sputtering temperature is 100 to 180 ℃;
in step (3), al 2 O 3 The target purity is more than or equal to 99.99 percent, and the sputtering and cleaning parameters of the target are as follows: degree of vacuum of 2X 10 -4 ~7×10 -4 Pa, argon flow rate is 150 to 250sccm, and sputtering cleaning time is 5 to 20min;
sputtering of Al 2 O 3 The membrane parameters were: argon flow is 40 to 60sccm, the vacuum chamber pressure is 1.0 to 2.0Pa, the sputtering time is 0.5 to 5 hours, the sputtering power is 100 to 380W, and the sputtering temperature is room temperature;
in step (4), moS 2 The target purity is more than or equal to 99.99 percent, and the sputtering and cleaning parameters of the target are as follows: degree of vacuum 2X 10 -4 ~7×10 -4 Pa, argon flow of 150-250sccm, and sputtering cleaning time of 5-20min;
sputtering MoS 2 The parameters of the film were: argon flow is 40 to 60sccm, vacuum chamber pressure is 1.0 to 2.0Pa, sputtering time is 0.5 to 7h, sputtering power is 100 to 300W, and sputtering temperature is room temperature.
2. The method for preparing the magnesium alloy surface lubricating wear-resistant composite film layer according to claim 1, wherein in the step (1), the magnesium alloy is one of AZ91D magnesium alloy, AZ31B magnesium alloy, AM60 magnesium alloy or WE43 magnesium alloy.
3. The method for preparing the magnesium alloy surface lubricating wear-resistant composite film layer according to claim 1, wherein in the step (1), the method for pretreating the surface of the magnesium alloy sample comprises the following steps: and grinding the magnesium alloy sample by using SiC sand paper of 150#, 400#, 1000#, and 2000# in sequence, polishing, putting the magnesium alloy sample into an acetone solution and deionized water, ultrasonically cleaning for 5-10 min, taking out the magnesium alloy sample, and drying by blowing.
4. The magnesium alloy surface lubricating wear-resistant composite film layer prepared by the preparation method of any one of claims 1~3.
5. The magnesium alloy surface lubricating wear-resistant composite film layer as claimed in claim 4, wherein the magnesium alloy surface lubricating wear-resistant composite film layer comprises an Al layer and an Al layer from inside to outside in sequence 2 O 3 Layer, moS 2 And (3) a layer.
6. The method of claim 5The magnesium alloy surface lubricating wear-resistant composite film layer is characterized in that the thickness of the Al layer is 7~9 mu m, and the Al layer is Al 2 O 3 Layer thickness 3~5 μm, moS 2 The layer thickness was 2~3 μm.
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