CN114959613A - Method for enhancing corrosion resistance of medium-entropy alloy CoCrNi film - Google Patents
Method for enhancing corrosion resistance of medium-entropy alloy CoCrNi film Download PDFInfo
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- CN114959613A CN114959613A CN202210675791.2A CN202210675791A CN114959613A CN 114959613 A CN114959613 A CN 114959613A CN 202210675791 A CN202210675791 A CN 202210675791A CN 114959613 A CN114959613 A CN 114959613A
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- 239000000956 alloy Substances 0.000 title claims abstract description 40
- 238000005260 corrosion Methods 0.000 title claims abstract description 29
- 230000007797 corrosion Effects 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 17
- 238000004544 sputter deposition Methods 0.000 claims abstract description 87
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 238000010791 quenching Methods 0.000 claims abstract description 14
- 230000000171 quenching effect Effects 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims description 15
- 238000005086 pumping Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 9
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- 239000000243 solution Substances 0.000 claims description 9
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- 239000003344 environmental pollutant Substances 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 229910001018 Cast iron Inorganic materials 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000007888 film coating Substances 0.000 abstract description 2
- 238000009501 film coating Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 44
- 239000000463 material Substances 0.000 description 8
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for enhancing corrosion resistance of a medium entropy alloy CoCrNi film, which comprises the following steps: treating the surface of a component needing film coating; respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine, fixing a component as a base on a sample table, and introducing argon for pre-sputtering when the vacuum degree in a sputtering chamber reaches a preset value; adjusting the air pressure in the sputtering chamber, setting sputtering power and carrying out co-sputtering coating; and heating the coated component to 1200 ℃, preserving heat, and then carrying out quenching treatment. The method co-sputters the CoCrNi and the Ti target to the surface of the component by magnetron sputtering, adjusts the Ti content of the CoCrNi film by controlling the sputtering technological parameters of the Ti target on the basis of ensuring the good mechanical property of the film, and further regulates and controls the structure by solution treatment so as to achieve the purpose of enhancing the corrosion resistance of the film.
Description
Technical Field
The invention relates to the technical field of metal film materials, in particular to a method for enhancing the corrosion resistance of a medium entropy alloy CoCrNi film.
Background
The surfaces of components which are used in a severe environment for a long time often have severe corrosion, which causes various uncertain dangerous factors. The passivation layer formed by the surface coating treatment can improve the corrosion resistance of the component, meet the pursuit of the industry on the production cost and efficiency, contribute to making up the insufficient corrosion resistance caused by the limitation of the component material and improve the reliability of the parts.
The CoCrNi intermediate entropy alloy is a material composed of three main element alloys, has a single FCC solid solution phase, has strength and toughness higher than those of most high entropy alloys and multi-phase alloys, has better mechanical property and corrosion resistance, is developed more mature at present, and can be used as a protective film material for popularization and use.
Magnetron sputtering is a physical vapor deposition technology, and not only can carry out large-area coating, but also has other advantages such as: the prepared film has uniform surface and good bonding force with the substrate, and the quality of the film can be further regulated and controlled by controlling magnetron sputtering parameters, so that the element content in the film can be effectively controlled.
The mechanical property of the existing medium entropy alloy CoCrNi film still can not meet the use requirement under certain use conditions, so that the mechanical property of the CoCrNi film needs to be further improved.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for enhancing the corrosion resistance of a medium-entropy alloy CoCrNi film, CoCrNi and a Ti target are co-sputtered onto the surface of a component through magnetron sputtering, on the basis of ensuring the good mechanical property of the film, the Ti content of the CoCrNi film is adjusted by controlling the sputtering technological parameters of the Ti target, and the structure is further regulated and controlled through solution treatment, so that the purpose of enhancing the corrosion resistance of the film is achieved.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for enhancing the corrosion resistance of a medium entropy alloy CoCrNi film comprises the following steps:
(1) component processing
Sequentially grinding, polishing, cleaning and drying the surface of a component to be coated for later use;
(2) target pretreatment
Respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine; fixing the member treated in the step (1) on a sample table as a base body, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in a cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value, introducing argon gas, and carrying out pre-sputtering to remove pollutants on the surface of the target material;
(3) coating film
Adjusting the air pressure in the sputtering chamber, setting the sputtering power of a CoCrNi alloy target and a Ti target, and carrying out co-sputtering coating; after sputtering is finished, cooling the component to room temperature along with the furnace and taking out;
(4) solution treatment
And heating the coated component to 1200 ℃ through a vacuum induction furnace, preserving heat for 2h, and then quenching to dissolve the excessive phase generated after the Ti element is added to the CoCrNi film into the solid solution.
Further, the member is selected from a steel-based material, a cast iron-based material, or other metal-based materials.
Further, the cleaning process in the step (1) adopts ultrasonic waves to sequentially carry out absolute ethyl alcohol cleaning and plasma water cleaning.
Further, in the CoCrNi alloy target, the atomic percentages of Co, Cr and Ni are 1:1: 1; the purity of the Ti target is more than 99.9 percent.
Further, in the step (2), sputtering in the pre-sputteringThe degree of vacuum in the chamber is 7X 10 -4 Pa, and the time of pre-sputtering is 10 min.
Further, in the step (3), the temperature of the matrix before sputtering is 100-500 ℃; adjusting the air pressure in the sputtering chamber to 0.2-0.5 Pa; the sputtering power of the CoCrNi alloy target is 100W, and the sputtering power of the Ti target is 20-100W; the sputtering time is 10-60 min.
Furthermore, in the step (2), the flow rate of argon gas is 50 sccm.
Further, oil quenching is adopted in the quenching treatment in the step (4).
The invention has the beneficial effects that:
the invention ionizes argon under the action of an electric field by co-sputtering, ionized argon ions bombard the surfaces of a CoCrNi alloy target and a Ti target, and the target material sputters a large amount of target material atoms to deposit a CoCrNi film on a component; heating the coated component through the surface of a vacuum induction furnace, preserving heat, and then quenching to promote the dissolution of the excessive phase generated after the CoCrNi film is added with Ti element into the solid solution, so as to reduce the phase interface and further improve the corrosion resistance of the film;
ti element is added into the CoCrNi film, so that intermetallic compounds can be generated on the basis of forming FCC solid solution, and Ti can promote the grain refinement of the film to a certain extent, so that the corrosion resistance of the film can be further improved;
according to the invention, the CoCrNi film is prepared by adopting a co-sputtering method, so that on one hand, the preparation quality of the film is ensured, on the other hand, the content and phase structure of Ti in the CoCrNi film can be effectively regulated and controlled through controlling the Ti target parameters, and the increase of precipitation phase caused by the addition of excessive Ti is prevented, thereby avoiding the influence of the increase of precipitation phase on the corrosion resistance of the CoCrNi film;
the method combines magnetron co-sputtering and solution treatment, regulates the Ti content of the medium-entropy alloy CoCrNi film by controlling the sputtering technological parameters of a Ti target on the basis of ensuring the good mechanical property of the film, refines the structure, and further regulates and controls the structure by solution treatment so as to achieve the purpose of enhancing the corrosion resistance;
the method has the advantages of good repeatability of production process, high deposition speed and high process controllability, and the obtained film has the advantages of excellent corrosion resistance and wear resistance, high compactness, uniform film formation and the like, is easy to realize industrialization, and can be used for surface treatment of high-end equipment components.
Drawings
FIG. 1 is an XRD pattern of the thin film of example 1 of the present invention.
FIG. 2 is a SEM image of the surface and cross-section of a thin film in example 1 of the present invention.
FIG. 3 is a graph showing the effect of the sputtering power of the Ti target on the current density and self-etching potential of the thin film.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
The invention provides a strengthening method of a medium-entropy alloy film, which comprises the following steps:
(1) component processing
Sequentially grinding, polishing, cleaning and drying the surface of a component needing film coating for later use; the component is selected from steel materials, cast iron materials or other metal materials; wherein, the cleaning process adopts ultrasonic waves to sequentially carry out absolute ethyl alcohol cleaning and plasma water cleaning;
(2) target pretreatment
Respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine; fixing the member treated in the step (1) on a sample table as a base body, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in a cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value, introducing argon gas, and carrying out pre-sputtering to remove pollutants on the surface of the target material;
wherein in the CoCrNi alloy target, the atomic percentages of Co, Cr and Ni are 1:1: 1; the purity of the Ti target is more than 99.9%; the degree of vacuum in the sputtering chamber during the pre-sputtering was 7X 10 -4 Pa, flow rate of argon gas introducedThe flow rate is 50sccm, and the pre-sputtering time is 10 min;
(3) coating film
Before sputtering, heating the substrate to 100-500 ℃; adjusting the air pressure in the sputtering chamber to 0.2-0.5 Pa, setting the sputtering power of a CoCrNi alloy target to be 100W and the sputtering power of a Ti target to be 20-100W, and carrying out co-sputtering coating; the sputtering time is 10-60 min; after sputtering is finished, cooling the component to room temperature along with the furnace and taking out;
(4) solution treatment
Heating the coated component to 1200 ℃ through the surface of a vacuum induction furnace, preserving heat for 2h, and then quenching to promote the excessive phase generated after the CoCrNi film is added with Ti to be dissolved in the solid solution, and reducing the phase interface to further improve the corrosion resistance; wherein the quenching treatment adopts oil quenching.
Example 1
(1) Component processing
Grinding the surface of a component to be coated with a film by using abrasive paper, and then polishing until the surface has no obvious scratch; sequentially cleaning the components in absolute ethyl alcohol and plasma water for ten minutes by an ultrasonic cleaner and then drying the components for later use;
(2) target pretreatment
Respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine; fixing the member processed in the step (1) on a sample table, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in the cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value of 7 multiplied by 10 -4 Introducing argon gas of 50sccm after Pa, and pre-sputtering for 10min to remove pollutants on the surface of the target material;
(3) coating film
Adjusting the air pressure in the sputtering chamber to be 0.2Pa, the matrix temperature to be 100 ℃, the sputtering power of the CoCrNi alloy target to be 100W and the sputtering power of the Ti target to be 20W, and carrying out co-sputtering coating; and after sputtering for 10min, cooling the component to room temperature along with the furnace, and taking out.
(4) Solution treatment
Heating the coated component to 1200 ℃ through the surface of a vacuum induction furnace, preserving heat for 2 hours, and then quenching to promote the excessive phase generated after the CoCrNi film is added with Ti element to be dissolved in solid solution.
Example 2
(1) Component processing
Grinding the surface of a component to be coated with a film by using abrasive paper and then polishing until the surface has no obvious scratch; sequentially cleaning the components in absolute ethyl alcohol and plasma water for ten minutes by an ultrasonic cleaner and then drying for later use;
(2) target pretreatment
Respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine; fixing the member processed in the step (1) on a sample table, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in the cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value of 7 multiplied by 10 - 4 Introducing argon gas of 50sccm after Pa, and pre-sputtering for 10min to remove pollutants on the surface of the target material;
(3) coating film
Adjusting the air pressure in the sputtering chamber to be 0.2Pa, the substrate temperature to be 100 ℃, the sputtering power of the CoCrNi alloy target to be 100W and the sputtering power of the Ti target to be 50W, and carrying out co-sputtering coating; sputtering for 20min, cooling the component to room temperature along with the furnace, and taking out;
(4) solution treatment
Heating the coated component to 1200 ℃ through the surface of a vacuum induction furnace, preserving heat for 2h, and then quenching to promote the excessive phase generated after the CoCrNi film is added with Ti element to be dissolved in solid solution.
Example 3
(1) Component processing
Grinding the surface of a component to be coated with a film by using abrasive paper and then polishing until the surface has no obvious scratch; sequentially cleaning the components in absolute ethyl alcohol and plasma water for ten minutes by an ultrasonic cleaner and then drying for later use;
(2) target pretreatment
Respectively using a CoCrNi alloy target and a Ti targetTwo direct current target positions of a vacuum magnetron sputtering film plating machine are arranged; fixing the member processed in the step (1) on a sample table, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in the cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value of 7 multiplied by 10 - 4 And introducing argon gas of 50sccm after Pa, and pre-sputtering for 10min to remove pollutants on the surface of the target.
(3) Coating film
Adjusting the air pressure in the sputtering chamber to be 0.5Pa, the substrate temperature to be 200 ℃, the sputtering power of the CoCrNi alloy target to be 100W and the sputtering power of the Ti target to be 120W, and carrying out co-sputtering coating; sputtering for 10min, cooling the component to room temperature along with the furnace, and taking out;
(4) solution treatment
Heating the coated component to 1200 ℃ through the surface of a vacuum induction furnace, preserving heat for 2h, and then quenching to promote the excessive phase generated after the CoCrNi film is added with Ti element to be dissolved in solid solution.
As shown in FIGS. 1 and 2, the thin film obtained by the method of the present invention has the advantages of excellent corrosion resistance, high compactness and uniform film formation. FIG. 3 is a graph showing the effect of the sputtering power of the Ti target on the corrosion current density and the self-etching potential of the thin film according to the present invention; as is clear from FIG. 3, when the sputtering power of the Ti target is 100W, a medium entropy alloy CoCrNi thin film having a low corrosion current density can be obtained with respect to a sputtering power of 50W.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method for enhancing the corrosion resistance of a medium entropy alloy CoCrNi film is characterized by comprising the following steps:
(1) component processing
Sequentially grinding, polishing, cleaning and drying the surface of a component to be coated for later use;
(2) target pretreatment
Respectively installing a CoCrNi alloy target and a Ti target at two direct current target positions of a vacuum magnetron sputtering coating machine; fixing the member treated in the step (1) on a sample table as a base body, closing a sputtering chamber, firstly performing low-vacuum pumping, and starting a molecular pump to perform high-vacuum pumping when the air pressure in a cavity of the sputtering chamber reaches below 4 Pa; when the vacuum degree in the sputtering chamber reaches a preset value, introducing argon gas, and carrying out pre-sputtering to remove pollutants on the surface of the target material;
(3) coating film
Adjusting the air pressure in the sputtering chamber, setting the sputtering power of a CoCrNi alloy target and a Ti target, and carrying out co-sputtering coating; after sputtering is finished, cooling the component to room temperature along with the furnace and taking out;
(4) solution treatment
And heating the coated component to 1200 ℃ through a vacuum induction furnace, preserving heat for 2h, and then quenching to dissolve the excessive phase generated after the Ti element is added to the CoCrNi film into the solid solution.
2. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film of claim 1, wherein the member is selected from steel, cast iron or other metal.
3. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film as claimed in claim 1, wherein the cleaning process of step (1) adopts ultrasonic waves to sequentially carry out absolute ethyl alcohol cleaning and plasma water cleaning.
4. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film as claimed in claim 1, wherein in the CoCrNi alloy target, the atomic percentages of Co, Cr and Ni are 1:1: 1; the purity of the Ti target is more than 99.9 percent.
5. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film according to claim 1, wherein the method is characterized in thatIn the step (2), the degree of vacuum in the sputtering chamber during the pre-sputtering is 7 × 10 -4 Pa, and the time of pre-sputtering is 10 min.
6. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film as claimed in claim 1, wherein in the step (3), the temperature of the substrate before sputtering is 100-500 ℃; adjusting the air pressure in the sputtering chamber to 0.2-0.5 Pa; the sputtering power of the CoCrNi alloy target is 100W, and the sputtering power of the Ti target is 20-100W; the sputtering time is 10-60 min.
7. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film as claimed in claim 1, wherein in the step (2), the flow rate of argon gas is 50 sccm.
8. The method for enhancing the corrosion resistance of the medium entropy alloy CoCrNi film according to claim 1, wherein the quenching treatment in the step (4) adopts oil quenching.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210675791.2A CN114959613B (en) | 2022-06-15 | 2022-06-15 | Method for enhancing corrosion resistance of medium-entropy alloy CoCrNi film |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| CN108359939A (en) * | 2018-03-06 | 2018-08-03 | 大连理工大学 | A kind of AlCoCrFeNi high-entropy alloy oxide semiconductor thin-films of variable band gap and preparation method thereof |
| CN108914074A (en) * | 2018-07-03 | 2018-11-30 | 东南大学 | A kind of high-resistivity alloy thin-film material and its preparation method and application |
| CN108998714A (en) * | 2018-06-07 | 2018-12-14 | 东南大学 | A kind of design and preparation method of two-phase medium entropy alloy |
| CN110158008A (en) * | 2019-03-28 | 2019-08-23 | 福建工程学院 | A kind of high entropy alloy coating and preparation method thereof |
| US20210054486A1 (en) * | 2017-07-26 | 2021-02-25 | Postech Academy-Industry Foundation | Medium-entropy alloy having excellent cryogenic properties |
| CN112746253A (en) * | 2020-12-29 | 2021-05-04 | 中南大学 | Steel-based surface composite modified layer and preparation method thereof |
-
2022
- 2022-06-15 CN CN202210675791.2A patent/CN114959613B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| US20210054486A1 (en) * | 2017-07-26 | 2021-02-25 | Postech Academy-Industry Foundation | Medium-entropy alloy having excellent cryogenic properties |
| CN108359939A (en) * | 2018-03-06 | 2018-08-03 | 大连理工大学 | A kind of AlCoCrFeNi high-entropy alloy oxide semiconductor thin-films of variable band gap and preparation method thereof |
| CN108998714A (en) * | 2018-06-07 | 2018-12-14 | 东南大学 | A kind of design and preparation method of two-phase medium entropy alloy |
| CN108914074A (en) * | 2018-07-03 | 2018-11-30 | 东南大学 | A kind of high-resistivity alloy thin-film material and its preparation method and application |
| CN110158008A (en) * | 2019-03-28 | 2019-08-23 | 福建工程学院 | A kind of high entropy alloy coating and preparation method thereof |
| CN112746253A (en) * | 2020-12-29 | 2021-05-04 | 中南大学 | Steel-based surface composite modified layer and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| PENG GAO ET AL.: "Ultra-strong and thermally stable nanocrystalline CrCoNi alloy", JOURNAL OF MATERIALS SCIENCE & TECHNOLOGY, vol. 106, pages 1 * |
| 赵佳琪: "CoCrNix(x=0.5~1)和CoCrNiTix(x=0.1~1)中熵合金的计算与模拟", 万方学位论文 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115786851A (en) * | 2022-11-29 | 2023-03-14 | 西北有色金属研究院 | Method for preparing high-hardness double-phase structure medium-entropy alloy film |
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