CN114990509A - Strengthening method of medium-entropy alloy coating - Google Patents

Abstract

The invention discloses a method for strengthening a medium-entropy alloy coating, which comprises the following steps: treating the surface of a component that needs to be coated; installing a medium-entropy alloy target and an Al target on two parts of a vacuum magnetron sputtering coating machine respectively At the direct current target position, the component is fixed on the sample stage as the base. When the vacuum degree in the sputtering chamber reaches a predetermined value, argon gas is introduced to carry out pre-sputtering; the air pressure in the sputtering chamber is adjusted, the sputtering power is set, and a total of Sputter coating; heat the coated component to 1200°C, then keep it warm, and then quench it; then heat the component to 600°C, then keep it warm, and cool it with the furnace to strengthen the medium-entropy alloy coating. In the present invention, the medium-entropy alloy and the Al target are co-sputtered to the surface of the component by magnetron sputtering, and an appropriate amount of intermetallic compounds are formed on the basis of ensuring the original solid solution of the coating by controlling the sputtering power of the Al target, and the solid solution Treatment and aging treatment can effectively strengthen the medium-entropy alloy coating.

Description

A kind of strengthening method of medium entropy alloy coating

technical field

The invention relates to the technical field of surface coatings, in particular to a method for strengthening a medium-entropy alloy coating.

Background technique

Medium-entropy alloy is a new type of metal material developed in recent years. It consists of three principal alloys and has a single solid solution phase. Compared with traditional metal materials, medium-entropy alloy materials have good strength, hardness and wear resistance, which are comparable to or even better than most high-entropy alloys and multiphase alloys. In terms of surface treatment, as a coating material, medium-entropy alloy can improve the reliability of components, and can be used as a hard coating material for popularization.

Magnetron sputtering is a physical vapor deposition technology, which can not only coat a large area, but also has some other advantages such as: the obtained coating surface is uniform, the bonding force between the coating and the substrate is good, and the quality of the coating can be improved. By controlling the parameters of magnetron sputtering, the content of elements in the coating can be effectively controlled.

The mechanical properties of the existing medium-entropy alloy coatings still cannot meet the application requirements under some specific use conditions, so the mechanical properties of the medium-entropy alloy coatings need to be further improved.

SUMMARY OF THE INVENTION

In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a method for strengthening the medium-entropy alloy coating, by co-sputtering the medium-entropy alloy and the Al target on the surface of the component by magnetron sputtering, and by controlling the sputtering power of the Al target. On the basis of ensuring the original solid solution of the coating, an appropriate amount of intermetallic compound is formed, and the medium-entropy alloy coating is effectively strengthened through solid solution treatment and aging treatment.

In order to realize the above-mentioned technical purpose and achieve the above-mentioned technical effect, the present invention is realized through the following technical solutions:

A method for strengthening a medium-entropy alloy coating, comprising the following steps:

(1) Component processing

The surfaces of the components that need to be coated are ground, polished, cleaned, and dried in sequence for use;

(2) Target pretreatment

The medium-entropy alloy target and the Al target are respectively installed at the two DC target positions of the vacuum magnetron sputtering coater; the component processed in step (1) is fixed on the sample stage as the base, the sputtering chamber is closed, and the low-temperature process is carried out first. Vacuum extraction, when the air pressure in the sputtering chamber reaches below 4Pa, start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches a predetermined value, pass argon gas for pre-sputtering to remove Contamination on the target surface;

(3) Co-sputtering coating

Adjust the air pressure in the sputtering chamber, set the sputtering power of the medium-entropy alloy target and the Al target, and carry out co-sputtering coating; after the sputtering is completed, the component is cooled to room temperature with the furnace and taken out;

(4) Solution treatment

The coated component was heated to 1200 °C in a vacuum induction furnace, and then kept for 2 h, and then quenched to dissolve the excess phase generated by adding Al element to the medium-entropy alloy coating into the solid solution;

(5) Aging treatment

The component processed in step (4) is heated to 600° C. in a vacuum induction furnace, then kept for 2-8 hours, and then cooled with the furnace to precipitate aluminum-based intermetallic compounds, thereby realizing the strengthening of the medium-entropy alloy coating.

Further, the components are selected from steel materials, cast iron materials or other non-ferrous metal materials.

Further, in the cleaning process of the step (1), ultrasonic waves are used to sequentially perform cleaning with absolute ethanol and cleaning with plasma water.

Further, the medium-entropy alloy target is selected from one of CoCrNi alloy target, FeCoNi alloy target, CrFeNi alloy target, and CrNiTi alloy target; the purity of the Al target is greater than 99.9%.

Further, the degree of vacuum in the sputtering chamber during pre-sputtering was 7×10 ^-4 Pa, and the time of pre-sputtering was 10 min.

Further, in step (3), the temperature of the substrate before sputtering is 100-500°C; the air pressure in the sputtering chamber is adjusted to 0.2-0.5Pa; the sputtering power of the medium-entropy alloy target is 100W, and the sputtering power of the Al target is 100W. It is 20-100W; the sputtering time is 10-60min.

Further, in step (2), the flow rate of the argon gas introduced is 50 sccm.

Further, the heating method of solution treatment and aging treatment is surface heating.

Beneficial effects of the present invention:

In the invention, argon gas is ionized under the action of an electric field by co-sputtering, the ionized argon ions bombard the surface of the entropy alloy target and the Al target, and the target material sputters out a large number of target material atoms, which are deposited on the component to form a coating; The layered component is heated by the surface of the vacuum induction furnace and then kept warm, and then subjected to quenching treatment to promote the dissolution of the excess phase generated by the addition of Al element into the medium-entropy alloy coating into the solid solution; then heated to a lower temperature for a long time for aging. treatment to achieve the strengthening effect of the medium-entropy alloy coating.

The addition of Al element to the medium-entropy alloy can generate intermetallic compounds on the basis of forming a solid solution, thereby forming a precipitation strengthening effect on the basis of solid solution strengthening, which can further improve its wear resistance.

The invention adopts the co-sputtering method to prepare the medium-entropy alloy coating, which on the one hand ensures the preparation quality of the coating, and on the other hand can effectively regulate the content and content of Al in the medium-entropy alloy coating by controlling the power parameter of the Al target. The phase composition can prevent the Al phase enrichment caused by the addition of too much Al, thereby avoiding the influence of the Al phase enrichment on the hardness and wear resistance of the coating.

The invention combines magnetron co-sputtering and subsequent heat treatment technology to control the composition and structure of the entropy alloy coating by controlling the sputtering power of the Al target, and on this basis, the solution treatment and aging treatment process are applied to the coating. The structure is further regulated to achieve effective strengthening of the medium-entropy alloy coating.

The method of the invention has the advantages of good production process repeatability, fast deposition speed and high process controllability, and the obtained coating has the advantages of excellent strength, hardness and wear resistance, high compactness, uniform film formation and the like, is easy to realize industrialization, and can be used Surface strengthening treatment of components.

Description of drawings

FIG. 1 is the XRD pattern of the co-sputtering coating of the entropy alloy CoCrNi target and the Al target in Example 1 of the present invention.

Fig. 2 is the SEM topography of the surface and cross-section of the co-sputtered coating of the entropy alloy CoCrNi target and the Al target in Example 1 of the present invention;

FIG. 3 is the change of the coating hardness under different sputtering powers of the Al target when the medium-entropy alloy CoCrNi target and the Al target are co-sputtered in Example 1 of the present invention.

Detailed ways

The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, and the protection scope of the present invention can be more clearly defined.

The invention provides a method for strengthening a medium-entropy alloy coating, comprising the following steps:

(1) Component processing

The surfaces of the components that need to be coated are ground, polished, cleaned, and dried in turn, and used for later use; the components are selected from steel materials, cast iron materials or other non-ferrous metal materials; the cleaning process is carried out by ultrasonic waves in anhydrous ethanol. cleaning and plasma water cleaning;

(2) Target pretreatment

The medium-entropy alloy target and the Al target are respectively installed at the two DC target positions of the vacuum magnetron sputtering coater; the component processed in step (1) is fixed on the sample stage as the base, the sputtering chamber is closed, and the low-temperature process is carried out first. Vacuum extraction, when the air pressure in the sputtering chamber reaches below 4Pa, start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches a predetermined value, pass argon gas for pre-sputtering to remove Contamination on the target surface;

The medium-entropy alloy target is selected from one of CoCrNi alloy target, FeCoNi alloy target, CrFeNi alloy target, and CrNiTi alloy target; the purity of the Al target is greater than 99.9%; the vacuum degree in the sputtering chamber during pre-sputtering is 7× 10 ^-4 Pa, the flow rate of argon is 50sccm, and the time of pre-sputtering is 10min;

(3) Co-sputtering coating

Before sputtering, the substrate temperature was heated to 100-500°C; the air pressure in the sputtering chamber was adjusted to 0.2-0.5Pa, the sputtering power of the medium-entropy alloy target was set to 100W, and the sputtering power of the Al target was 20-100W. Co-sputtering coating is carried out; the sputtering time is 10-60min; after the sputtering is completed, the component is cooled to room temperature with the furnace and taken out;

(4) Solution treatment

The coated component was heated to 1200 °C through a vacuum induction furnace and kept for 2 hours, and then quenched to dissolve the excess phase generated by adding Al element to the medium-entropy alloy coating into the solid solution; among them, oil was used for quenching treatment. quenched;

(5) Aging treatment

The component processed in step (4) is heated to 600° C. through a vacuum induction furnace, then kept for 2 to 8 hours, and then cooled with the furnace to precipitate aluminum-based intermetallic compounds to strengthen the medium-entropy alloy coating.

Example 1

(1) Component processing

Sand the surface of the component to be coated with sandpaper, and then polish it until there is no obvious scratch on the surface; use an ultrasonic cleaner to clean the component in anhydrous ethanol and plasma water for ten minutes each, and then dry it for later use;

(2) Target pretreatment

Install the CoCrNi alloy target and the Al target on the two DC target positions of the vacuum magnetron sputtering coater respectively; fix the component processed in step (1) on the sample stage, close the sputtering chamber, and first perform low vacuum extraction , when the air pressure in the sputtering chamber reaches below 4Pa, then start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches the predetermined value of 7×10 ^-4 Pa, pass argon gas for 50sccm, and pre-sputter for 10min To remove contaminants on the target surface;

(3) Co-sputtering coating

The air pressure in the sputtering chamber was adjusted to 0.3 Pa, the substrate temperature was 100 °C, the sputtering power of the CoCrNi alloy target was 100 W, and the sputtering power of the Al target was 20 W, and the co-sputtering coating was performed; Remove from oven after cooling to room temperature.

(4) Solution treatment

The coated component was heated to 1200 °C through a vacuum induction furnace and kept for 2 h, and then quenched to promote the dissolution of the excess phase generated by the addition of Al element into the solid solution in the medium-entropy alloy coating.

(5) Aging treatment

The component processed in step (4) is heated to 600° C. through the vacuum induction furnace surface, then kept for 2 hours, and cooled with the furnace to precipitate aluminum-based intermetallic compounds to achieve the strengthening effect of the medium-entropy alloy coating.

Example 2

(1) Component processing

The surface of the component that needs to be coated is ground with sandpaper and then polished until there is no obvious scratch on the surface; through the ultrasonic cleaner, the component is cleaned in anhydrous ethanol and plasma water for ten minutes each, and then dried for use;

(2) Target pretreatment

Install the CoCrNi alloy target and the Al target on the two DC target positions of the vacuum magnetron sputtering coater respectively; fix the component processed in step (1) on the sample stage, close the sputtering chamber, and first perform low vacuum extraction , when the pressure in the sputtering chamber reaches below 4Pa, then start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches the predetermined value of 7×10 ^{- 4} Pa, pass argon gas for 50sccm, and pre-sputter for 10min To remove contaminants on the target surface;

(3) Co-sputtering coating

The air pressure in the sputtering chamber was adjusted to 0.4 Pa, the substrate temperature was 200 °C, the sputtering power of the CrNiTi alloy target was 100 W, and the sputtering power of the Al target was 30 W, and the co-sputtering coating was carried out; Take out the furnace after cooling to room temperature;

(4) Solution treatment

The coated component was heated to 1200 °C through a vacuum induction furnace and kept for 2 h, and then quenched to promote the dissolution of the excess phase generated by the addition of Al element into the solid solution in the medium-entropy alloy coating.

(5) Aging treatment

The component treated in step (4) is heated to 600° C. through a vacuum induction furnace, and then kept for 4 hours, followed by cooling in the furnace to precipitate aluminum-based intermetallic compounds to achieve the strengthening effect of the medium-entropy alloy coating.

Example 3

(1) Component processing

The surface of the component that needs to be coated is ground with sandpaper and then polished until there is no obvious scratch on the surface; through the ultrasonic cleaner, the component is cleaned in anhydrous ethanol and plasma water for ten minutes each, and then dried for use;

(2) Target pretreatment

Install the CoCrNi alloy target and the Al target on the two DC target positions of the vacuum magnetron sputtering coater respectively; fix the component processed in step (1) on the sample stage, close the sputtering chamber, and first perform low vacuum extraction , when the pressure in the sputtering chamber reaches below 4Pa, then start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches the predetermined value of 7×10 ^{- 4} Pa, pass argon gas for 50sccm, and pre-sputter for 10min to remove contaminants from the target surface.

(3) Co-sputtering coating

The air pressure in the sputtering chamber was adjusted to 0.5Pa, the substrate temperature was 100°C, the sputtering power of the CrNiTi alloy target was 100W, and the sputtering power of the Al target was 50W, and the co-sputtering coating was performed. After sputtering for 30 minutes, the component was cooled to room temperature with the furnace and taken out;

(4) Solution treatment

The coated component was heated to 1200°C through a vacuum induction furnace, and then kept for 2 hours, and then quenched to promote the dissolution of the excess phase generated by the addition of Al element into the medium-entropy alloy coating into the solid solution;

(5) Aging treatment

The component treated in step (4) is heated to 600° C. through a vacuum induction furnace, and then kept for 6 hours, followed by cooling in the furnace to precipitate aluminum-based intermetallic compounds to achieve the strengthening effect of the medium-entropy alloy coating.

As shown in Figures 1 and 2, the coating obtained by the method of the present invention has high strength, high hardness, excellent wear resistance, high compactness and uniform film formation.

The above descriptions are only the embodiments of the present invention, and are not intended to limit the scope of the present invention. Any equivalent structure or equivalent process transformation made by using the contents of the description and drawings of the present invention, or directly or indirectly applied to other related technologies Fields are similarly included in the scope of patent protection of the present invention.

Claims (8)

1. a kind of strengthening method of medium entropy alloy coating, is characterized in that, comprises the steps: (1) Component processing The surfaces of the components that need to be coated are ground, polished, cleaned, and dried in sequence for use; (2) Target pretreatment The medium-entropy alloy target and the Al target are respectively installed at the two DC target positions of the vacuum magnetron sputtering coater; the component processed in step (1) is fixed on the sample stage as the base, the sputtering chamber is closed, and the low-temperature process is carried out first. Vacuum extraction, when the air pressure in the sputtering chamber reaches below 4Pa, start the molecular pump to extract high vacuum; when the vacuum degree in the sputtering chamber reaches a predetermined value, pass argon gas for pre-sputtering to remove Contamination on the target surface; (3) Co-sputtering coating Adjust the air pressure in the sputtering chamber, set the sputtering power of the medium-entropy alloy target and the Al target, and carry out co-sputtering coating; after the sputtering is completed, the component is cooled to room temperature with the furnace and taken out; (4) Solution treatment The coated component was heated to 1200 °C in a vacuum induction furnace, and then kept for 2 h, and then quenched to dissolve the excess phase generated by adding Al element to the medium-entropy alloy coating into the solid solution; (5) Aging treatment The component processed in step (4) is heated to 600° C. in a vacuum induction furnace, then kept for 2-8 hours, and then cooled with the furnace to precipitate aluminum-based intermetallic compounds, thereby realizing the strengthening of the medium-entropy alloy coating. 2 . The method for strengthening a medium-entropy alloy coating according to claim 1 , wherein the components are selected from steel materials, cast iron materials or other non-ferrous metal materials. 3 . 3 . The method for strengthening a medium-entropy alloy coating according to claim 1 , wherein the cleaning process of the step (1) adopts ultrasonic waves to sequentially carry out anhydrous ethanol cleaning and plasma water cleaning. 4 . 4. The method for strengthening a medium-entropy alloy coating according to claim 1, wherein the medium-entropy alloy target is selected from the group consisting of CoCrNi alloy target, FeCoNi alloy target, CrFeNi alloy target, and CrNiTi alloy target. species; the purity of the Al target is greater than 99.9%. 5. The method for strengthening a medium-entropy alloy coating according to claim 1, wherein in step (2), the vacuum degree in the sputtering chamber during pre-sputtering is 7 × 10 ^-4 Pa, and the pre-sputtering The sputtering time was 10 min. 6 . The method for strengthening a medium-entropy alloy coating according to claim 1 , wherein: in step (3), the temperature of the substrate before sputtering is 100 to 500° C.; the air pressure in the sputtering chamber is adjusted to 0.2 ~0.5Pa; the sputtering power of the medium-entropy alloy target is 100W, the sputtering power of the Al target is 20-100W; the sputtering time is 10-60min. 7 . The method for strengthening a medium-entropy alloy coating according to claim 1 , wherein: in step (2), the flow rate of the argon gas introduced is 50 sccm. 8 . 8 . The method for strengthening a medium-entropy alloy coating according to claim 1 , wherein the heating method of solution treatment and aging treatment is surface heating. 9 .

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