CN115161608A - Preparation method of ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication - Google Patents
Preparation method of ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication Download PDFInfo
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- 239000006104 solid solution Substances 0.000 title claims abstract description 64
- 238000005461 lubrication Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010408 film Substances 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 239000010409 thin film Substances 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims description 44
- 239000000758 substrate Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000013077 target material Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 20
- 125000001165 hydrophobic group Chemical group 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 230000001050 lubricating effect Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 31
- 239000007789 gas Substances 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- -1 Transition Metal Nitride Chemical class 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A preparation method of a ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication relates to a preparation method of a ZrN nano solid solution film. The invention aims to solve the technical problem that the existing ZrN-based thin film has poor tribological performance and hydrophobic performance. According to the invention, through introducing the rare earth element Y and the soft ductile metal Ag, a tribochemical reaction can be excited to form a friction oxidation product and a self-lubricating phase with a synergistic lubricating effect, and the average friction coefficient of the film is effectively reduced. In addition, the solid solution of Y atoms and Ag atoms can effectively cut the chemical bond state of the film surface and accelerate the formation of Y 2 O 3 And Ag 2 O a hydrophobic group. The invention provides a novel method for constructing a ZrYAgN nano solid solution film integrating high hydrophobicity, self-lubrication, low friction and other properties by utilizing a magnetron sputtering method, and the ZrYAgN nano solid solution film prepared by the method has good development on the surface of an aerospace componentAnd (4) application prospect.
Description
Technical Field
The invention relates to a preparation method of a ZrN-based nano solid solution film.
Background
With the progress and development of the industry, the thin film material has wide application in the aspects of aerospace engine components, mechanical parts, human body orthopedic implants and the like, but the high friction coefficient and poor hydrophobicity still cause the failure of the parts and are the main problems to be overcome. Therefore, high demands are made on the hydrophobicity, self-lubricity, and the like of the film material. Transition Metal Nitride (TMN) films have high hardness and excellent tribological properties and have been widely used in frictional wear parts. ZrN-based thin films are receiving increasing attention due to their good mechanical properties, thermal stability, chemical stability and oxidation resistance. However, with the emergence of harsh conditions such as dry type, high speed, high temperature and the like, especially under more complex working conditions such as aerospace engines and the like, higher requirements are put on the surfaces of components. The ZrN-based thin film has a high friction coefficient, is not wear-resistant, and has poor hydrophobicity, so its application is greatly limited. In recent years, it has been found that the formation of a nano solid-solution film by adding other elements to the film is an effective way to improve its hydrophobic and tribological properties. The prepared intelligent self-lubricating nano composite film with low friction coefficient and high hydrophobicity has certain scientific significance and application value. Ag has a good lubricating effect over a wide temperature range as a soft ductile metal and has been recognized as a soft lubricating phase in films. Therefore, it is an urgent need of current research to prepare a nano solid solution film with self-lubricating and high hydrophobic properties.
Disclosure of Invention
The invention provides a preparation method of a ZrYAgN nano solid solution film with high hydrophobicity and self lubrication, aiming at solving the technical problem that the existing ZrN-based film has poor tribological property and hydrophobic property.
The preparation method of the ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication is carried out according to the following steps:
1. cleaning and drying the substrate in sequence; the substrate is a titanium-based material;
2. putting the substrate cleaned and dried in the step one into a magnetron sputtering deviceIn the vacuum cavity, a Zr target, a Y target and an Ag target are respectively arranged on three target positions of a magnetron sputtering device, the distances between the three targets and a substrate are 12 cm-13 cm, and the cavity is vacuumized until the vacuum degree is 1 multiplied by 10 -4 Pa～1.1×10 -4 Pa；
3. Introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; the Y target adopts direct current, and the sputtering current of the Y target is set to be 0.01A; the Zr target adopts direct current, and the sputtering current of the Zr target is set to be 0.5A; closing the Ag target material window; sputtering the Y target and the Zr target simultaneously, wherein the sputtering thicknesses of the two targets are equal and are both 0.9-1.1 mu m, and obtaining a ZrYN nano solid solution film on the titanium substrate; the flow rate of Ar is 60-65 sccm; said N 2 The flow rate of (2) is 10sccm to 15sccm;
introducing soft metal Ag into the ZrYN nano solid solution film: introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; closing windows of the Y target and the Zr target, opening a window of the Ag target, setting the sputtering current of the Ag target to be 0.01-0.04A by adopting direct current for the Ag target, starting sputtering, and setting the sputtering thickness to be 1-1.2 mu m; the flow rate of Ar is 60 sccm-65 sccm; said N 2 The flow rate of (2) is 10-15 sccm;
4. and after the sputtering is finished, cooling the cavity to room temperature to obtain the ZrYAgN nano solid solution film.
The invention aims to improve the hydrophobicity and the tribological performance of a ZrN-based thin film by introducing a rare earth element Y and a soft ductile metal Ag element.
The invention provides a ZrN based thin film material, which comprises zirconium element and nitrogen element. According to the invention, through introducing the rare earth element Y and the soft ductile metal Ag, a tribochemical reaction can be excited to form a friction oxidation product and a self-lubricating phase with a synergistic lubricating effect, and the average friction coefficient of the film is effectively reduced. In addition, the solid solution of Y atoms and Ag atoms can effectively cut the chemical bond state of the film surface and accelerate the formation of Y 2 O 3 And Ag 2 An O hydrophobic group. Due to Ag 2 Ag cation (Ag) in O + ) Filling shell layer (4 d) for coordination saturation 10 5S 0 ) ElectricitySubstructure, without tendency to interact with water, forms Ag on the surface of the film by autoxidation 2 An O group. Ag for surface hydrophobicity 2 O comes from solute Ag atoms instead of precipitated metal Ag, wherein a proper amount of Ag atoms are added into the sublattice to further improve the hydrophobicity, so that the film presents high hydrophobicity, the tribological behavior of the film in a water friction environment is improved, the hydrophobicity and the tribological performance of the ZrN-based film are improved, and the self-lubrication and high-hydrophobicity characteristics of the ZrYAgN nano solid solution film are realized. The invention provides a novel method for constructing a ZrYAgN nano solid solution film integrating the performances of high hydrophobicity, self-lubrication, low friction and the like by using a magnetron sputtering method, and the ZrYAgN nano solid solution film prepared by the method has good development and application prospects on the surfaces of aerospace components.
Compared with a pure ZrN film, the series of ZrYAgN nano solid solution films prepared by the method have the advantages that a small amount of rare earth element Y and soft metal Ag element are added to greatly influence the tribological performance of the films, the hydrophobicity of the ZrYAgN nano solid solution films is greatly related to the content of Y and Ag, and the solid solution of Y atoms and Ag atoms can effectively cut the chemical bond state on the surfaces of the films and accelerate the formation of Y atoms 2 O 3 And Ag 2 O a hydrophobic group. The surface hydrophobic angle of the pure ZrN film is 92 degrees, and after the rare earth element Y is added, the surface hydrophobic angle of the ZrYN nano solid solution film reaches 110 degrees; after the soft ductile metal Ag is added, the hydrophobic property of the surface of the film is further improved. When the addition content of Ag is 2at.% (namely A2), the ZrYAgN nano solid solution film has the highest hydrophobicity, the surface hydrophobic angle of the film reaches 127 degrees, and the surface hydrophobic angle is 35 degrees higher than that of a pure ZrN film; when the addition content of Ag is 1at percent (namely A1), the hydrophobic angle of the surface of the ZrYAgN nano solid solution film reaches 123 degrees, and the hydrophobic angle of the surface of the ZrYAgN nano solid solution film is reduced by 4 degrees compared with the addition content of Ag of 2at percent, because the content of Ag is lower, the formed Ag is 2 The hydrophobic groups O are fewer, so that the hydrophobic property of the surface is influenced; when the addition content of Ag is 3at.% (namely A3) and 4at.% (namely A4), the hydrophobic angles of the ZrYAgN coating surface are 120 degrees and 116 degrees respectively, and with the increase of the Ag content, the hydrophobic property of the ZrYAgN nano solid solution film surface is on the contraryDecrease due to addition of excess Ag metal resulting in no Ag formation 2 The precipitation of the O hydrophobic group as Ag nanoclusters deteriorates the hydrophobicity. The invention proves that Y is formed by adding proper amount of Y and Ag elements into the film 2 O 3 And Ag 2 The O hydrophobic group improves the hydrophobicity of the surface of the ZrYAgN nano solid solution film, and a new method is provided for realizing the integrated regulation and control of the performances of the ZrYAgN nano solid solution film, such as high hydrophobicity, self-lubrication, excellent tribology and the like.
The invention has the beneficial effects that:
1. the invention adopts the magnetron sputtering deposition technology to prepare the nano solid solution film material, has simple process, low cost and high yield, and can be industrially produced in large scale;
2. the invention provides a novel method for constructing a ZrYAgN nano solid solution film integrating the performances of high hydrophobicity, self-lubrication, excellent tribology and the like by utilizing a magnetron sputtering method.
Drawings
FIG. 1 is an XRD pattern of the product after sputtering;
FIG. 2 is a graph of coefficient of friction data;
FIG. 3 is a hydrophobic angle measurement diagram.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication, which is specifically carried out according to the following steps:
1. cleaning and drying the substrate in sequence; the substrate is a titanium-based material;
2. putting the substrate cleaned and dried in the step one into a vacuum cavity of a magnetron sputtering device, respectively installing a Zr target, a Y target and an Ag target on three target positions of the magnetron sputtering device, wherein the distances between the three targets and the substrate are 12-13 cm, and vacuumizing the cavity until the vacuum degree is 1 multiplied by 10 -4 Pa～1.1×10 -4 Pa；
3. Introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; the Y target adopts direct current, and the sputtering current of the Y target is set to be 0.01A; the Zr target adopts direct current, and the sputtering power of the Zr target is setThe flow was 0.5A; closing the Ag target window; sputtering the Y target and the Zr target simultaneously, wherein the sputtering thicknesses of the two targets are equal and are both 0.9-1.1 mu m, and obtaining a ZrYN nano solid solution film on the titanium substrate; the flow rate of Ar is 60 sccm-65 sccm; said N 2 The flow rate of (2) is 10sccm to 15sccm;
introducing soft metal Ag into the ZrYN nano solid solution film: introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; closing windows of a Y target and a Zr target, opening a window of an Ag target, setting the sputtering current of the Ag target to be 0.01-0.04A by adopting direct current for the Ag target, starting sputtering, and setting the sputtering thickness to be 1-1.2 mu m; the flow rate of Ar is 60 sccm-65 sccm; said N 2 The flow rate of (2) is 10sccm to 15sccm;
4. and after the sputtering is finished, cooling the cavity to room temperature to obtain the ZrYAgN nano solid solution film.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the titanium-based material in the step one is alloy Ti-6Al-4V. The rest is the same as the first embodiment.
The third concrete implementation mode: the first or second difference between the present embodiment and the specific embodiment is: in the first step, the substrate is subjected to ultrasonic cleaning by sequentially selecting absolute ethyl alcohol, acetone and deionized water for 20-25 min, and finally the substrate is placed in a drying box and dried at 60 ℃. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the second step, the vacuum degree of the cavity is pumped to 1 multiplied by 10 by a mechanical pump and a turbo molecular pump -4 Pa. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between the present embodiment and the specific embodiment is that: in the third step, the sputtering current of the Ag target was set to 0.01A. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fifth embodiment is different from the fifth embodiment in that: the flow rate of Ar in the third step is 60sccm; said N 2 The flow rate of (2) is 10sccm. Other and specific embodimentsThe fifth mode is the same.
The invention was verified with the following tests:
test one: the test is a preparation method of a ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication, and the preparation method is specifically carried out according to the following steps:
1. sequentially selecting absolute ethyl alcohol, acetone and deionized water to ultrasonically clean the substrate for 25min, and finally placing the substrate in a drying box to dry at 60 ℃; the substrate is alloy Ti-6Al-4V;
2. putting the substrate cleaned and dried in the step one into a vacuum cavity of a magnetron sputtering device, respectively installing a Zr target, a Y target and an Ag target on three target positions of the magnetron sputtering device, wherein the distances between the three targets and the substrate are 12cm, and pumping the vacuum degree of the cavity to 1 x 10 by a mechanical pump and a turbo molecular pump -4 Pa；
3. Introducing Ar and N into the cavity 2 The mixed gas of (2) is used as sputtering gas (the working pressure in the cavity is 0.8 Pa); the Y target adopts direct current, and the sputtering current of the Y target is set to be 0.01A; the Zr target adopts direct current, and the sputtering current of the Zr target is set to be 0.5A; closing the Ag target window; sputtering the Y target and the Zr target simultaneously, wherein the sputtering thicknesses of the two targets are equal and are both 0.9 mu m, and obtaining a ZrYN nano solid solution film on the titanium substrate; the flow rate of Ar is 60sccm; said N 2 The flow rate of (2) is 10sccm;
introducing soft metal Ag into the ZrYN nano solid solution film: introducing Ar and N into the cavity 2 The mixed gas of (2) is used as sputtering gas (the working pressure in the cavity is 0.8 Pa); closing windows of the Y target and the Zr target, opening a window of the Ag target, setting the sputtering current of the Ag target to be 0.01A by adopting the direct current for the Ag target, starting sputtering, and enabling the sputtering thickness to be 1 mu m; the flow rate of Ar is 60sccm; said N 2 The flow rate of (2) is 10sccm;
4. and after the sputtering is finished, cooling the cavity to room temperature to obtain the ZrYAgN nano solid solution film, which is marked as A1.
Test one the ZrYAgN nano solid solution thin film prepared by the contact angle measuring apparatus has a hydrophobic angle of 123 ° (see fig. 3).
The coefficient of friction of the ZrYAgN nano solid solution film prepared in test one was 0.018 as measured by a ball-and-disk type frictional abrasion meter under water friction conditions (see fig. 2).
And (2) test II: this test differs from the test one in that: in the third step, the current of the Ag target is set to be 0.02A, and the ZrYAgN nano solid solution film obtained in the fourth step is marked as A2. The rest were the same as in test one.
The hydrophobic angle of the ZrYAgN nano solid solution film prepared by the second test is 127 degrees (shown in figure 3) by using a contact angle measuring instrument.
The friction coefficient of the ZrYAgN nano solid solution film prepared in test two was measured to be 0.005 (fig. 2) by a ball-and-disk type frictional wear meter under the water frictional condition.
And (3) test III: this test differs from the test one in that: in the third step, the current of the Ag target is set to be 0.03A, and the ZrYAgN nano solid solution film obtained in the fourth step is marked as A3. The rest is the same as test one.
The hydrophobic angle of the ZrYAgN nano solid solution film prepared in test three was 120 ° (see fig. 3) measured by a contact angle measuring instrument.
The coefficient of friction of the ZrYAgN nano solid solution film prepared in test three was 0.021 (see fig. 2) as measured by a ball-and-disk friction and wear meter under water friction conditions.
And (4) testing: the test is a comparative test, no Ag element is added, and the specific process is different from the first test in that: and step two, no Ag target is installed, and the ZrYN nano solid solution film obtained in step four is marked as A0. The rest were the same as in test one.
The hydrophobic angle of the ZrYN nano solid solution film prepared in the fourth test is 110 degrees (shown in FIG. 3) by using a contact angle measuring instrument.
The friction coefficient of the ZrYN nano solid solution film prepared in the fourth test is 0.055 (shown in figure 2) measured by a ball-disk friction and abrasion instrument under the water friction condition.
And (5) testing five: this test differs from the test one in that: in the third step, the current of the Ag target is set to be 0.04A, and the ZrYAgN nano solid solution film obtained in the fourth step is marked as A4. The rest is the same as test one.
The hydrophobic angle of the ZrYAgN nano solid solution film prepared in test five was 116 ° (see fig. 3) measured by a contact angle measuring instrument.
The friction coefficient of the ZrYAgN nano solid solution film prepared in the fifth test is 0.031 (shown in figure 2) measured by a ball-disk friction and wear meter under the water friction condition.
Fig. 1 is an XRD pattern of the product after sputtering, from which it can be seen that diffraction peaks Ag appear at A2 and A3 due to the introduction of Ag element, and the Ag peak of A2 is stronger than that of A3. The presence of weak diffraction peaks was observed at A1 and A4; there was no significant peak for the pure ZrYN nano solid solution film (test four).
Claims (6)
1. A preparation method of a ZrYAgN nano solid solution film with high hydrophobicity and self lubrication is characterized in that the preparation method of the ZrYAgN nano solid solution film with high hydrophobicity and self lubrication is carried out according to the following steps:
1. cleaning and drying the substrate in sequence; the substrate is a titanium-based material;
2. putting the substrate cleaned and dried in the step one into a vacuum cavity of a magnetron sputtering device, respectively installing a Zr target, a Y target and an Ag target on three target positions of the magnetron sputtering device, wherein the distances between the three targets and the substrate are 12 cm-13 cm, and vacuumizing the cavity until the vacuum degree is 1 multiplied by 10 -4 Pa～1.1×10 -4 Pa；
3. Introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; the Y target adopts direct current, and the sputtering current of the Y target is set to be 0.01A; the Zr target adopts direct current, and the sputtering current of the Zr target is set to be 0.5A; closing the Ag target material window; sputtering the Y target and the Zr target simultaneously, wherein the sputtering thicknesses of the two targets are equal and are both 0.9-1.1 mu m, and obtaining a ZrYN nano solid solution film on the titanium substrate; the flow rate of Ar is 60 sccm-65 sccm; said N 2 The flow rate of (2) is 10sccm to 15sccm;
introducing a soft metal Ag into the ZrYN nano solid solution film: introducing Ar and N into the cavity 2 The mixed gas of (a) is used as a sputtering gas; closing windows of the Y target and the Zr target, opening a window of the Ag target, setting the sputtering current of the Ag target by adopting direct current for the Ag targetStarting sputtering at 0.01-0.04A, wherein the sputtering thickness is 1-1.2 μm; the flow rate of Ar is 60-65 sccm; n is as follows 2 The flow rate of (2) is 10-15 sccm;
4. and after the sputtering is finished, cooling the cavity to room temperature to obtain the ZrYAgN nano solid solution film.
2. The method for preparing ZrYAgN nano solid solution film with high hydrophobicity and self lubrication according to claim 1, wherein the titanium-based material in the step one is alloy Ti-6Al-4V.
3. The method for preparing a ZrYAgN nano solid solution film with high hydrophobicity and self lubrication according to claim 1, wherein in the first step, the substrate is subjected to ultrasonic cleaning by sequentially selecting absolute ethyl alcohol, acetone and deionized water, the cleaning is performed for 20-25 min respectively, and finally the substrate is placed in a drying box and dried at 60 ℃.
4. The method for preparing ZrYAgN nano solid solution film with high hydrophobicity and self lubrication according to claim 1, wherein the vacuum degree of the chamber is pumped to 1 x 10 by the mechanical pump and the turbo molecular pump in the second step -4 Pa。
5. The method for preparing ZrYAgN nano solid solution film with high hydrophobicity and self lubrication according to claim 1, wherein sputtering current of Ag target is set to 0.01A in the third step.
6. The method for preparing ZrYAgN nano solid solution thin film with high hydrophobicity and self lubrication according to claim 1, wherein the flow rate of Ar in the third step is 60sccm; n is as follows 2 The flow rate of (2) is 10sccm.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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