KR102055320B1 - Target for physical deposition, nitride hard coating using thereof and methods of fabricating the same - Google Patents

Abstract

The present invention performs a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target consisting of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al As a nitride hard film embodied, a nitride hard film is provided based on Al and containing 5 to 25 atomic% Cr and 0.1 to 4 atomic% Fe.

Description

Target for physical deposition, nitride hard coating using the same and method for manufacturing the same

The present invention relates to a target, a hard coating thereby, and a method for producing the same, and more particularly, to a target for physical vapor deposition, a nitride hard film thereby, and a method for producing the same.

In order to improve the performance of coated cutting tools, various studies have been made in the field of tool design, edge treatment, excellent base material and coating film. In the coating cutting tool, the manufacturing cost of the coating film is only about 15% of the total cost, but the performance of the cutting tool according to the presence or absence of the coating film is about 2-3 times. Based on this situation, the industrial demand for nitride hard coatings as coating coatings is increasing.

Korean Patent Registration Publication No. 1737709 (2017-05-12)

It is an object of the present invention to provide a nitride hard film, a physical vapor deposition target for implementing the same, and a method of manufacturing the same, which can secure the adhesion, heat resistance, and hardness of the hard film. However, these problems are exemplary, and the scope of the present invention is not limited thereby.

According to one embodiment of the present invention, as a physical vapor deposition target used in the manufacture of hard coating, Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance is made of an alloy consisting of Al, physical vapor deposition target To provide.

According to another embodiment of the present invention, as a target for physical vapor deposition used in the production of hard coating, Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb Any one selected from Y and V: 0.1 to 20 atomic% and the balance provides a target for physical vapor deposition, consisting of an alloy consisting of Al.

According to another embodiment of the present invention, preparing an Al powder, Cr powder and Fe powder; Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. It includes, the sintered sintered body is made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al, provides a method for producing a physical vapor deposition target.

According to another embodiment of the present invention, preparing a powder selected from Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. The sintered sintered body is completed, the sintered compact is any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 ~ Provided is a method for producing a target for physical vapor deposition, comprising an alloy consisting of 20 atomic% and the balance Al.

According to another embodiment of the present invention, a mixed gas atmosphere containing nitrogen and an inert gas with respect to a physical vapor deposition target made of an alloy composed of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic%, and the balance Al. As a nitride hard film implemented by performing a physical vapor deposition process in, based on Al, and provides a nitride hard film containing 5 to 25 atomic% Cr and 0.1 to 4 atomic% Fe.

According to another embodiment of the present invention, AlCr layer made of Al and Cr; And the nitride hard film formed on the AlCr layer.

In the multilayer coating film, the thickness ratio of the nitride hard film may be 60% to 90%.

According to another embodiment of the invention, any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 to A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas with respect to a physical vapor deposition target made of an alloy composed of 20 atomic% and the balance of Al. Provided is a nitride hard film containing any one selected from 25 atomic% Cr, 0.1 to 4 atomic% Fe, 0.1 to 3.5 atomic% Ti, Zr, Mn, Si, W, Mo, Nb, Y and V do.

According to another embodiment of the present invention, preparing a physical vapor deposition target made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al; And a physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the target for physical vapor deposition, based on Al, containing 5 to 25 atomic% Cr and 0.1 to 4 atomic% Forming a nitride hard film containing Fe; It provides a method for producing a nitride hard film comprising a.

According to another embodiment of the invention, any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 to Preparing a target for physical vapor deposition composed of an alloy consisting of 20 atomic% and the balance Al; And based on the physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target, based on Al, Cr: 5 to 25 atomic%, Fe: 0.1 to 4 atoms Any one selected from%, Ti, Zr, Mn, Si, W, Mo, Nb, Y, and V: forming a nitride hard film containing 0.1 to 3.5 atomic%; It provides a method for producing a nitride hard film comprising a.

According to the embodiment of the present invention, it is possible to implement a nitride hard film and a physical vapor deposition target for implementing the same, and a method of manufacturing the same, which can secure the adhesion, heat resistance and hardness of the hard film. Of course, the scope of the present invention is not limited by these effects.

1 is a view showing a SEM photograph (a), particle size analysis (b) and component mapping result (c) of a powder after milling in the process of manufacturing a physical deposition target according to an embodiment of the present invention.
2 is a view showing a SEM photograph (a) and a component mapping result (b) of a sintered body obtained by sintering powder after milling in the process of manufacturing a physical vapor deposition target according to an embodiment of the present invention.
3 and 4 are photographs taken in cross section of the multilayer coating film implemented under the conditions of the experimental example of the present invention.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but can be implemented in various forms, and the following embodiments are intended to complete the disclosure of the present invention, the scope of the invention to those skilled in the art It is provided to inform you completely. In addition, the components may be exaggerated or reduced in size in the drawings for convenience of description.

According to one embodiment of the present invention, as a physical vapor deposition target used in the manufacture of hard coating, Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance is made of an alloy consisting of Al, physical vapor deposition target To provide.

Method for producing a physical vapor deposition target according to an embodiment of the present invention, preparing Al powder, Cr powder and Fe powder; Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. It includes, the sintered sintered body is made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al.

In the physical vapor deposition target, Cr is relatively easy to react with Al. When the content of Cr exceeds 40 atomic%, an Al-Cr compound is produced during the preparation of the target, and the Al-Cr compound causes arc ions. Non-uniform movement of the arc spot may occur in the plating process, thereby causing a problem of generating large particles in the hard film formed using the target. On the other hand, when the content of Cr is less than 9 atomic%, the oxidation resistance and heat resistance of the target may be lowered, and the friction coefficient of the hard film realized using the target may increase.

When the content of Fe in the physical vapor deposition target exceeds 6 atomic%, a problem may occur that the oxidation resistance of the target deteriorates. When the content of Fe is less than 0.1 atomic%, the structure, composition and hardness of the target become uneven. The problem of cracking in the target may occur.

The nitride hard film using the physical vapor deposition target according to an embodiment of the present invention is nitrogen and the physical vapor deposition target made of an alloy composed of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al. A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing an inert gas, based on Al, containing 5 to 25 atomic% Cr and 0.1 to 4 atomic% Fe.

In the method of manufacturing a nitride hard film using a physical vapor deposition target according to an embodiment of the present invention, the physical vapor deposition target is made of an alloy composed of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic%, and the balance of Al. Preparing; And a physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the target for physical vapor deposition, based on Al, containing 5 to 25 atomic% Cr and 0.1 to 4 atomic% Forming a nitride hard film containing Fe; It includes.

According to another embodiment of the present invention, as a target for physical vapor deposition used in the production of hard coating, Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb Any one selected from Y and V: 0.1 to 20 atomic% and the balance provides a target for physical vapor deposition, consisting of an alloy consisting of Al.

According to another embodiment of the present invention, a method of manufacturing a physical vapor deposition target may include any one powder selected from Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y, and V. Preparing; Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. The sintered sintered body is completed, the sintered compact is any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 ~ 20 atomic% and remainder consist of an alloy consisting of Al.

In the physical vapor deposition target, Cr is relatively easy to react with Al. When the content of Cr exceeds 32 atomic%, an Al-Cr compound is produced during the preparation of the target, and the Al-Cr compound causes arc ions. Non-uniform movement of the arc spot may occur in the plating process, thereby causing a problem in that large particles are generated in the hard film formed using the target. On the other hand, when the content of Cr is less than 9 atomic%, the oxidation resistance and heat resistance of the target may be lowered, and the friction coefficient of the hard film realized using the target may increase.

When the content of Fe in the physical vapor deposition target exceeds 6 atomic%, a problem may occur that the oxidation resistance of the target deteriorates. When the content of Fe is less than 0.1 atomic%, the structure, composition and hardness of the target become uneven. Problems that cause cracks in the target may occur.

Any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V in the physical vapor deposition target may be added to improve hardness of the target, wear resistance, oxidation resistance and / or resistance to chemical reaction. Can be. For example, at least one selected from Ti, Zr, Si, W, Mo, and V may increase the hardness of the target and improve wear resistance, and at least one selected from Mn, Si, W, Mo, Nb, and Y. May improve oxidation resistance of the target, and at least one selected from Si and Y may increase resistance of the target to chemical reactivity. However, when the content of at least any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V in the physical vapor deposition target exceeds 20 atomic%, the decrease in hardness before and after heat treatment of the target is remarkably. A problem may arise that is higher (eg, the hardness drop rate is higher than 15%).

The nitride hard film using the physical vapor deposition target according to another embodiment of the present invention is Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and Any one selected from V: Nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target consisting of an alloy consisting of 0.1 to 20 atomic% and the balance, Al, Based on Al, any one selected from 5 to 25 atomic% Cr, 0.1 to 4 atomic% Fe, 0.1 to 3.5 atomic% Ti, Zr, Mn, Si, W, Mo, Nb, Y and V It contains.

According to another embodiment of the present invention, a method of manufacturing a nitride hard film using a physical vapor deposition target is Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb Any one selected from Y and V: preparing a target for physical vapor deposition consisting of an alloy consisting of 0.1 to 20 atomic% and the balance Al; And based on the physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target, based on Al, Cr: 5 to 25 atomic%, Fe: 0.1 to 4 atoms Any one selected from%, Ti, Zr, Mn, Si, W, Mo, Nb, Y, and V: forming a nitride hard film containing 0.1 to 3.5 atomic%; It includes.

According to the embodiments of the present invention described above, it is possible to implement a nitride hard film and a physical vapor deposition target for implementing the same and a method of manufacturing the same, which can ensure the adhesion, heat resistance and hardness of the hard film, in the following, Experimental examples are provided to aid in understanding the present invention. However, the following experimental examples are only for helping understanding of the present invention, and the present invention is not limited to the following experimental examples.

Target composition and physical properties

Experimental Example Target composition (at%) Experimental Example Target composition (at%) 1-1 Al ₆₀ Cr ₃₉ Fe ₁ 2-1 Al ₇₁ Cr ₂₄ Fe ₁ Ti ₄ 1-2 Al ₆₈ Cr ₃₀ Fe ₂ 2-2 Al ₇₁ Cr ₂₄ Fe ₁ Zr ₄ 1-3 Al ₇₁ Cr ₂₈ Fe ₁ 2-3 Al ₇₁ Cr ₂₄ Fe ₁ Mn ₄ 1-4 Al ₇₃ Cr ₂₆ Fe ₁ 2-4 Al ₇₁ Cr ₂₄ Fe ₁ Si ₄ 1-5 Al ₇₅ Cr ₂₄ Fe ₁ 2-5 Al ₇₁ Cr ₂₄ Fe ₁ Mo ₄ 1-6 Al ₈₀ Cr ₁₉ Fe ₁ 2-6 Al ₇₁ Cr ₂₄ Fe ₁ W ₄ 1-7 Al ₇₁ Cr ₂₄ Fe ₅ 2-7 Al ₇₁ Cr ₂₄ Fe ₁ Nb ₄ - - 2-8 Al ₇₁ Cr ₂₄ Fe ₁ V ₄

Referring to Table 1, Experimental Examples 1-1, 1-2, 1-3, 1-4, 1-5, 1-6, and 1-7 of the present invention indicate the physical vapor deposition targets used for the manufacture of hard films. As a composition, a target for physical vapor deposition is provided, which is made of an alloy composed of Cr: 9-40 atomic%, Fe: 0.1-6 atomic%, and the balance Al.

For example, Experimental Example 1-1 discloses a composition of a physical vapor deposition target for use in the manufacture of a hard film composed of an alloy composed of 39 atomic percent Cr, 1 atomic percent Fe, and 60 atomic percent Al. Example 1-2 discloses the composition of the physical vapor deposition target used in the manufacture of a hard film composed of an alloy consisting of 30 atomic% Cr, 2 atomic% Fe, and 68 atomic% Al balance. Disclosed is the composition of the physical vapor deposition target used in the manufacture of a hard film composed of an alloy consisting of 28 atomic% Cr, 1 atomic% Fe, and 71 atomic% Al, and Experimental Example 1-4 shows Cr: 26 atomic%. , Fe: 1 atomic% and the balance Al: 73 atomic% discloses the composition of the physical vapor deposition target used in the manufacture of a hard film composed of an alloy consisting of, the experimental example 1-5 is Cr: 24 atomic%, Fe: 1 atom % And the balance Al: The composition of the physical vapor deposition target used for the manufacture of a hard film composed of an alloy consisting of 75 atomic% In the present disclosure, Experimental Example 1-6 discloses a composition of a physical vapor deposition target for use in the manufacture of a hard film composed of an alloy composed of Cr: 19 atomic%, Fe: 1 atomic% and balance Al: 80 atomic%. 1-7 discloses the composition of a physical vapor deposition target for use in producing a hard film composed of an alloy composed of 24 atomic% Cr, 5 atomic% Fe, and 71 atomic% Al balance.

Method for producing a physical vapor deposition target having the above composition comprises the steps of preparing Al powder, Cr powder and Fe powder; Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. It includes.

The density of the physical vapor deposition target implemented by the manufacturing method was 94% in Experimental Examples 1-3 and Experimental Examples 1-5, and in Experimental Examples 1-2, Experimental Examples 1-6, Experimental Examples 1-7 93% and 84% in Experimental Example 1-1. According to this, in order to ensure the density of the physical vapor deposition target of 93% or more, the composition of the physical vapor deposition target used for hard film production is Cr: 9 to 30 atomic%, Fe: 0.1 to 6 atomic% and the balance Al It can be seen that the alloy consisting of consisting of.

In addition, referring to Table 1, Experimental Examples 2-1, 2-2, 2-3, 2-4, 2-5, 2-6, 2-7, and 2-8 of the present invention are used to prepare hard coatings. As a composition of the physical vapor deposition target, Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 to 20 A target for physical vapor deposition is provided, wherein the atomic% and the balance are made of an alloy composed of Al.

For example, Experimental Example 2-1 is a physical vapor deposition target used for the manufacture of a hard film composed of an alloy consisting of 24 atomic% Cr: 1 atomic% Fe, 4 atomic% Ti, and 71 atomic% Al balance. The composition of the present invention, Experimental Example 2-2 is for physical vapor deposition used in the manufacture of a hard film composed of an alloy consisting of 24 atomic% Cr: 1 atomic% Fe, 4 atomic% Zr and 71 atomic% Al balance. The composition of the target is disclosed, and Experimental Example 2-3 is a physical condition used for producing a hard film composed of an alloy composed of 24 atomic% Cr, 1 atomic% Fe, 4 atomic% Mn, and 71 atomic% Al balance. The composition of the wear target is disclosed, and Experimental Example 2-4 is a physics used for producing a hard film composed of an alloy composed of 24 atomic% Cr, 1 atomic% Fe, 4 atomic% Si, and 71 atomic% Al balance. The composition of the deposition target is disclosed, and Experimental Example 2-5 is an alloy composed of 24 atomic% Cr, 1 atomic% Fe, 4 atomic% Mo, and 71 atomic% Al balance. The composition of the physical vapor deposition target used for producing a hard film is disclosed, Experimental Example 2-6 is an alloy consisting of 24 atomic% Cr, 1 atomic% Fe, 4 atomic% W and 71 atomic% Al balance. The composition of the physical vapor deposition target used in the manufacture of the hard film consisting of the present invention, Experimental Example 2-7 is composed of Cr: 24 atomic%, Fe: 1 atomic%, Nb: 4 atomic% and the balance Al: 71 atomic% The composition of the physical vapor deposition target used in the manufacture of a hard coating made of an alloy is disclosed, and Experimental Example 2-8 is Cr: 24 atomic%, Fe: 1 atomic%, V: 4 atomic% and the balance Al: 71 atomic% Disclosed is a composition of a physical vapor deposition target for use in the manufacture of hard films composed of alloys constructed.

Method for producing a physical vapor deposition target having the above composition, Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V selected from any one powder selected from; Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. It includes.

The density of the physical deposition target implemented by the manufacturing method was found to be 95% in Experimental Example 2-4, 94% in Experimental Example 2-2, 92% in Experimental Example 2-7. It was found to be 90% in Experimental Examples 2-3, 88% in Experimental Examples 2-5 and 2-8, and 86% in Experimental Examples 2-6 and 2-1. According to this, in order to ensure the density of the physical vapor deposition target of 90% or more, the composition of the physical vapor deposition target used for the production of hard coating is Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Zr, Si Any one selected from, and Nb: 0.1 to 20 atomic% and the balance can be seen that it is preferably made of an alloy consisting of Al.

On the other hand, the powder milling process and the sintering process applied to the manufacturing method of the physical vapor deposition target of the composition shown in Table 1 specifically applied the following conditions.

First, the powder milling process is applied to the ball mill (planetary ball mill) process, the charge amount of the ball and powder (% in the container) is 10 ~ 90%, the charge ratio of the ball and powder (Ball: Powder) is 1: 1 to 20: 1, the amount of dispersant is 0 to 10 wt%, milling speed is 50 to 500 rpm, milling time is 200 hours or less, milling process atmosphere is air, argon (Ar), nitrogen ( Nitrogen) atmosphere was applied.

Spark plasma sintering, hot press (sintering) is applied to the sintering process, the sintering temperature is 300 ~ 1000 ℃, the sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less, The sintering time applied the conditions of 10-100 minutes.

1 is a view showing a SEM photograph (a), particle size analysis (b) and component mapping result (c) of a powder after milling in the process of manufacturing a physical deposition target according to an embodiment of the present invention.

Referring to Figure 1, the physical vapor deposition target according to an embodiment of the present invention has a composition of Experimental Examples 1-3 of Table 1. In the step of performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder, the average size of the Al powder is 25 ~ 40㎛, the average size of the Cr powder is 35 ~ 50㎛, the Fe powder The average size of is 10-20 μm. In the milling process, the content of ball is 1000g, the content of powder is 50g, the content of ball and powder in the container is 35%, and the content of ball and powder is 20: 1. The amount of dispersant was 2 wt%, the milling speed was 300 rpm, the milling time was 10 hours, and the milling atmosphere was applied with argon (Ar) atmosphere.

2 is a view showing a SEM photograph (a) and a component mapping result (b) of a sintered body obtained by sintering powder after milling in the process of manufacturing a physical vapor deposition target according to an embodiment of the present invention.

Referring to Figure 2, the physical vapor deposition target according to an embodiment of the present invention has a composition of Experimental Examples 1-3 of Table 1. And also the illustrated mechanical alloying the mixed powder, but do perform the sintering in a vacuum atmosphere, a sintering temperature in the sintering process is 900 ℃, sintering pressure of 60MPa is, the degree of vacuum is 3 ^-2 Torr, and the sintering time 100 minutes of conditions were applied. The sintered body implemented by performing this process can be confirmed that the powder sintering is performed well to have a high density sintered body. In addition, as a result of EDS analysis, it can be confirmed that Al is 68.77%, Cr is 29.85%, and Fe is 1.38%, and the composition error rate is within ㅁ 2%.

Composition and Properties of Hard Film

The nitride hard coating was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas for the physical vapor deposition target having the above-described composition of Table 1.

Table 2 shows the composition analysis results (EDAX) excluding nitrogen for the nitride hard film, and Table 3 shows the composition analysis results (EDAX) including nitrogen for the nitride hard film. In Table 2 and Table 3, M means any one element selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V corresponding to each experimental example.

target Al-K Cr-K Fe-K M Experimental Example 2-4 59.5 34.9 1.5 4.0 Experimental Example 2-1 63.4 30.6 1.2 4.8 Experimental Example 2-6 66.5 29.2 1.0 3.3 Experimental Example 2-5 61.5 32.2 1.4 4.9 Experimental Example 2-3 61.7 32.6 1.4 4.3 Experimental Example 2-2 59.0 34.6 1.4 5.0 Experimental Example 2-7 59.5 33.9 1.4 5.2

target Al-K Cr-K Fe-K M N Experimental Example 2-4 34.6 19.7 0.8 2.3 42.6 Experimental Example 2-1 36.4 16.8 0.7 2.1 43.6 Experimental Example 2-6 39.7 16.9 0.6 1.9 40.9 Experimental Example 2-5 36.3 18.3 0.8 2.8 41.8 Experimental Example 2-3 35.8 18.2 0.8 2.5 42.8 Experimental Example 2-2 33.4 18.8 0.7 3.5 43.6 Experimental Example 2-7 33.6 28.4 0.7 2.9 44.4

Referring to Tables 2 and 3, for example, a mixed gas containing nitrogen and an inert gas for a physical vapor deposition target having the composition (Al ₇₁ Cr ₂₄ Fe ₁ Si ₄ ) of Experimental Example 2-4 of Table 1 In the nitride hard film formed by performing physical vapor deposition in an atmosphere, the composition analysis result of excluding nitrogen was 59.5% of Al, 34.9% of Cr, 1.5% of Fe, and 4.0% of Si. It can be seen that Al is 34.6%, Cr is 19.7%, Fe is 0.8%, Si is 2.3%, and N is 42.6%.

A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target having the composition (Al ₇₁ Cr ₂₄ Fe ₁ Ti ₄ ) of Experimental Example 2-1 of Table 1 The composition analysis results excluding nitrogen were 63.4% Al, 30.6% Cr, 1.2% Fe, 4.8% Ti, and the composition analysis results containing nitrogen were 36.4% Al, 16.8% Cr and 0.7% Fe. It can be seen that%, Ti is 2.1%, and N is 43.6%.

A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target having the composition (Al ₇₁ Cr ₂₄ Fe ₁ W ₄ ) of Experimental Example 2-6 of Table 1 The composition analysis results except for nitrogen are 66.5% for Al, 29.2% for Cr, 1.0% for Fe, and 3.3% for W. The composition analysis results containing nitrogen include 39.7% for Al, 16.9% for Cr, and 0.6 for Fe. %, W is 1.9%, and N is 40.9%.

A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target having the composition of Experimental Example 2-5 of Table 1 (Al ₇₁ Cr ₂₄ Fe ₁ Mo ₄ ). The composition analysis results excluding nitrogen are 61.5% Al, 32.2% Cr, 1.4% Fe, 4.9% Mo, and the composition analysis results containing nitrogen 36.3% Al, 18.3% Cr and 0.8% Fe. It can be seen that Mo, 2.8%, and N is 41.8%.

A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target having the composition (Al ₇₁ Cr ₂₄ Fe ₁ Zr ₄ ) of Experimental Example 2-2 of Table 1 The composition analysis results excluding nitrogen are 59.0% Al, 34.6% Cr, 1.4% Fe, 5.0% Zr, and the composition analysis results containing nitrogen 33.4% Al, 18.8% Cr and 0.7% Fe. %, Zr is 3.5%, N can be confirmed that 43.6%.

A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a physical vapor deposition target having the composition (Al ₇₁ Cr ₂₄ Fe ₁ Nb ₄ ) of Experimental Example 2-7 of Table 1 The composition analysis results excluding nitrogen are 59.5% Al, 33.9% Cr, 1.4% Fe, 5.2% Nb, and the composition analysis results containing nitrogen 33.6% Al, 28.4% Cr and 0.7% Fe. It can be seen that%, Nb is 2.9%, and N is 44.4%.

Table 4 and Table 5 show the physical properties of the nitride hard film by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas for the physical vapor deposition target having the above-described composition of Table 1.

Heat treatment temperature and hardness drop rate Experimental Example Target composition (at%) Hardness before heat treatment
(Hv) Modulus of elasticity
(GPa) 1000 ℃ Drop
rate% 1100 ℃ Drop
rate% 1-1 Al ₆₀ Cr ₃₉ Fe ₁ 2609 391 2411 7.6 - - 1-2 Al ₆₈ Cr ₃₀ Fe ₂ 2718 444 2594 4.6 - - 1-3 Al ₇₁ Cr ₂₈ Fe ₁ 3072 439 2834 7.7 2400 21.9 1-4 Al ₇₃ Cr ₂₆ Fe ₁ 3129 495 2523 19.4 1975 37 1-5 Al ₇₅ Cr ₂₄ Fe ₁ 3023 462 2736 9.5 2505 17 1-6 Al ₈₀ Cr ₁₉ Fe ₁ 2380 345 2447 -2.8 - - 1-7 Al ₇₁ Cr ₂₄ Fe ₅ 2456 408 2387 2.8 2257 8.1

Heat treatment temperature and hardness drop rate Experimental Example Target composition (at%) Hardness before heat treatment
(Hv) Modulus of elasticity
(GPa) 1000 ℃ Drop
rate% 1100 ℃ Drop
rate% 2-1 Al ₇₁ Cr ₂₄ Fe ₁ Ti ₄ 3226 467 2934 9.1 2737 15.2 2-2 Al ₇₁ Cr ₂₄ Fe ₁ Zr ₄ 3113 439 3022 2.9 2927 6.0 2-3 Al ₇₁ Cr ₂₄ Fe ₁ Mn ₄ 3033 482 2627 13.4 2318 23.6 2-4 Al ₇₁ Cr ₂₄ Fe ₁ Si ₄ 3319 450 3128 5.8 2881 13.2 2-5 Al ₇₁ Cr ₂₄ Fe ₁ Mo ₄ 3134 437 2897 7.6 2612 16.7 2-6 Al ₇₁ Cr ₂₄ Fe ₁ W ₄ 2066 295 1933 6.4 1613 21.9 2-7 Al ₇₁ Cr ₂₄ Fe ₁ Nb ₄ 3308 472 3134 5.3 2510 24.1 2-8 Al ₇₁ Cr ₂₄ Fe ₁ V ₄ 2487 424 - - - -

Referring to Table 4, for example, by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target having the composition of Experimental Example 1-1 (Al ₆₀ Cr ₃₉ Fe ₁ ) In the embodied nitride hard film, the hardness before heat treatment was 2609 Hv and the elastic modulus was 391 GPa, whereas the hardness after 1000 ° C. heat treatment was 2411 Hv, resulting in a 7.6% hardness drop compared to the hardness before heat treatment.

Referring to Table 5, for example, the physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target having the composition of Experimental Example 2-1 (Al ₇₁ Cr ₂₄ Fe ₁ Ti ₄ ) In the hardened nitride film, the hardness before heat treatment was 3226 Hv and the modulus of elasticity was 467 GPa, whereas the hardness after 1000 ° C. was 2934 Hv, resulting in a 9.1% decrease in hardness compared to the hardness before heat treatment. As 2737Hv it can be seen that the hardness decrease rate of 15.2% compared to the hardness before heat treatment occurs.

Composition and Properties of Multilayer Coating Film

The physical vapor deposition process was performed in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target having the composition shown in Table 1 to implement a multilayer coating film having a nitride hard film. Hereinafter, the results of evaluating the nitride multilayer coating film and its physical properties implemented under various conditions will be described. The multilayer coating film disclosed in Tables 6 to 13 refers to a nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the target for physical vapor deposition.

Multilayer coating Experimental Example Buffer layer First layer 2nd layer 3rd layer 4th layer 3-1 Ti AlCrN AlCrFeN AlCrN - 3-2 Ti AlCrN AlCrN AlCrFeSiN AlCrN 3-3 Ti AlCrN AlCrN AlCrFeZrN AlCrN

Experimental Example Coating film
Thickness (um) Coating hardness (Hv) Scratch Test
(Lc2 [N]) 3-1 2.4 3,219 38.98 3-2 2.4 3,269 18.53 3-3 2.6 3,259 26.16

Table 6 shows the structure of the multilayer coating film implemented under the conditions of Experimental Examples 3-1 to 3-3, and Table 7 shows the results of evaluating the physical properties of the multilayer coating film.

In Experimental Example 3-1, a Ti buffer layer was first formed on a substrate, and then a 2.4 mm thick multilayer coating film in which an AlCrN layer, an AlCrFeN layer, and an AlCrN layer were sequentially stacked was implemented. In Experimental Example 3-2, a Ti buffer layer was first formed on a substrate, and then a 2.4 mm thick multilayer coating film in which an AlCrN layer, an AlCrN layer, an AlCrFeSiN layer, and an AlCrN layer were sequentially stacked was implemented. In Experimental Example 3-3, a Ti buffer layer was first formed on a substrate, and then a 2.4 mm thick multilayer coating film in which an AlCrN layer, an AlCrN layer, an AlCrFeZrN layer, and an AlCrN layer were sequentially stacked was implemented.

The AlCrN layer was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the target Al: Cr ratio 7: 3, the AlCrFeN layer is shown in Experimental Examples 1-3 of Table 1 The physical Al deposition process was carried out in a mixed gas atmosphere containing nitrogen and an inert gas to the target Al ₇₁ Cr ₂₈ Fe ₁ composition, and the AlCrFeSiN layer was Al ₇₁ Cr ₂₄ disclosed in Experimental Example 2-4 of Table 1. The target of Fe ₁ Si ₄ composition was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas, the AlCrFeZrN layer is Al ₇₁ Cr ₂₄ Fe ₁ Zr disclosed in Experimental Example 2-2 of Table 1 _It was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the target of _four compositions.

It was confirmed that the multilayer coating film according to Experimental Examples 3-1 to 3-3 all secured a hardness of 3200 Hv or more, and also excellent adhesion.

Multilayer coating Experimental Example Buffer layer First layer 2nd layer 3rd layer 3-4-1 Cr AlCrN AlCrFeSiN - 3-4-2 Cr AlCrN AlCrFeTiN - 3-4-3 Cr AlCrN AlCrFeZrN - 3-5-1 Cr AlCrN AlCrN AlCrFeSiN 3-5-2 Cr AlCrN AlCrN AlCrFeTiN 3-5-3 Cr AlCrN AlCrN AlCrFeZrN

Experimental Example Coating film
Thickness (um) Coating hardness (Hv) Scratch Test
(Lc2 [N]) 3-4-1 2.1 4,003 81.34 3-4-2 2.5 3,876 81.37 3-4-3 2.5 3,855 64.87 3-5-1 2.2 3,810 85.75 3-5-2 2.4 3,819 76.62 3-5-3 2.3 3,845 69.28

Table 8 shows the structure of the multilayer coating film implemented under the conditions of Experimental Examples 3-4-1 to 3-4-3 and the conditions of Experimental Examples 3-5-1 to 3-5-3, and Table 9 shows such multilayers. The results of evaluating the properties of the coating film are shown.

In Experimental Example 3-4-1, a Cr buffer layer was first formed on a substrate, and then a 2.1 mm thick multilayer coating film in which an AlCrN layer (53%) and an AlCrFeSiN layer (47%) were sequentially stacked was implemented. In Experimental Example 3-4-2, a Cr buffer layer was first formed on a substrate, and then a 2.5 mm thick multilayer coating film in which an AlCrN layer (53%) and an AlCrFeTiN layer (47%) were sequentially stacked was implemented. In Experimental Example 3-4-3, a Cr buffer layer was first formed on a substrate, and then a 2.5 mm thick multilayer coating film in which an AlCrN layer (53%) and an AlCrFeZrN layer (47%) were sequentially stacked was implemented. In Experimental Example 3-5-1, a Cr buffer layer was first formed on a substrate, followed by a 2.2 mm thick multilayer coating film in which an AlCrN layer (12%), an AlCrN layer (44%), and an AlCrFeSiN layer (44%) were sequentially stacked. Was implemented. In Experimental Example 3-5-2, after forming the Cr buffer layer on the substrate first, a 2.4 mm-thick multilayer coating film in which AlCrN layer (12%), AlCrN layer (44%), and AlCrFeTiN layer (44%) were sequentially stacked. Was implemented. In Experimental Example 3-5-3, after forming the Cr buffer layer on the substrate first, a 2.3 mm thick multilayer coating film in which an AlCrN layer (12%), an AlCrN layer (44%), and an AlCrFeZrN layer (44%) were sequentially stacked. Implemented Here, the percentage (%) means the thickness ratio of each layer of the total coating film thickness.

The AlCrN layer was implemented by performing physical vapor deposition in a mixed gas atmosphere containing nitrogen and an inert gas to a target with an Al: Cr ratio of 7: 3, and the AlCrFeSiN layer is shown in Experimental Example 2-4 of Table 1. The physical Al deposition process was carried out in a mixed gas atmosphere containing nitrogen and an inert gas to a target Al ₇₁ Cr ₂₄ Fe ₁ Si ₄ composition, and the AlCrFeTiN layer was Al ₇₁ disclosed in Experimental Example 2-1 of Table 1. It was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to the target of Cr ₂₄ Fe ₁ Ti ₄ composition, the AlCrFeZrN layer is Al ₇₁ Cr ₂₄ Fe disclosed in Experimental Example 2-2 of Table 1 The target of ₁ Zr ₄ composition was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas.

In the multilayer coating films of Experimental Examples 3-4-1 to 3-4-3 and Experimental Examples 3-5-1 to 3-5-3, the outermost layer thickness ratio of the coating layer using the AlCrFeX (X = Si, Ti) target was determined. The multi-layer coating film increased from 44% to 47%, all secured a hardness of 3200Hv or more, it was confirmed that excellent adhesion also secured.

Multilayer coating Experimental Example Buffer layer First layer 2nd layer 3rd layer 3-6-1 Cr AlCrN AlCrFeSiN - 3-6-2 Cr AlCrN AlCrFeTiN - 3-7-1 Cr AlCrN AlCrFeSiN - 3-7-2 Cr AlCrN AlCrFeTiN -

Element Experimental Example 3-7-1
2nd layer
(AlCrFeSiN) Experimental Example 3-7-1
First layer
(AlCrN) Experimental Example 3-7-2
2nd layer
(AlCrFeTiN) Experimental Example 3-7-2
First layer
(AlCrN) N 52.51 51.43 52.42 51.02 Al 32.75 33.30 32.78 33.75 Cr 13.61 15.27 13.52 15.23 Fe 0.34 - 0.33 - Si 0.78 - - - Ti - - 0.95 - Total 100.00 100 100.00 100.00

Experimental Example Coating film
Thickness (um) Coating hardness (Hv) Scratch Test
(Lc2 [N]) 3-6-1 2.5 3,600 69 3-6-2 2.3 3,440 78 3-7-1 2.3 3,732 74 3-7-2 2.2 3,537 54

Experimental Example Hardness (room temperature) Hardness (1000 ℃) Hardness
% Drop Hardness (1100 ℃) Hardness
% Drop 3-6-1 3,600 3,210 10.8 3,061 15.0 3-6-2 3,440 3,121 9.3 3,053 11.3 3-7-1 3,732 3,259 12.7 3,008 19.4 3-7-2 3,537 3,089 12.7 2,930 17.2

Table 10 shows the structure of the multilayer coating film implemented under the conditions of Experimental Examples 3-6-1 to 3-7-2, Table 11 is the conditions of Experimental Examples 3-7-1 and Experimental Examples 3-7-2 EDS component analysis results of the implemented multilayer coating film are shown, and Table 12 and Table 13 show the results of evaluating the physical properties of the multilayer coating film. 3 is a photograph taken a cross section of the multilayer coating film implemented under the conditions of Experimental Example 3-7-1, Figure 4 is a photograph taken a cross section of the multilayer coating film implemented under the conditions of Experimental Example 3-7-2.

In Experimental Example 3-6-1, a Cr buffer layer was first formed on a substrate, and then a 2.5 mm thick multilayer coating film in which an AlCrN layer (29%) and an AlCrFeSiN layer (71%) were sequentially stacked was implemented. In Experimental Example 3-6-2, a Cr buffer layer was first formed on a substrate, and then a 2.3 mm thick multilayer coating film in which an AlCrN layer (29%) and an AlCrFeTiN layer (71%) were sequentially stacked was implemented. In Experimental Example 3-7-1, a Cr buffer layer was first formed on a substrate, and then a 2.3 mm thick multilayer coating film in which an AlCrN layer (12%) and an AlCrFeSiN layer (88%) were sequentially stacked was implemented. In Experimental Example 3-7-2, a Cr buffer layer was first formed on a substrate, and then a 2.2 mm thick multilayer coating film in which an AlCrN layer (12%) and an AlCrFeTiN layer (88%) were sequentially stacked was implemented. Here, the percentage (%) means the thickness ratio of each layer of the total coating film thickness.

The AlCrN layer was implemented by performing physical vapor deposition in a mixed gas atmosphere containing nitrogen and an inert gas to a target with an Al: Cr ratio of 7: 3, and the AlCrFeSiN layer is shown in Experimental Example 2-4 of Table 1. The physical Al deposition process was carried out in a mixed gas atmosphere containing nitrogen and an inert gas to a target Al ₇₁ Cr ₂₄ Fe ₁ Si ₄ composition, and the AlCrFeTiN layer was Al ₇₁ disclosed in Experimental Example 2-1 of Table 1. The target of Cr ₂₄ Fe ₁ Ti ₄ composition was implemented by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas.

The multilayer coating film according to Experimental Examples 3-6-1 to 3-6-2 and Experimental Examples 3-7-1 to 3-7-2 is the outermost layer of the coating layer using AlCrFeX (X = Si, Ti) target for improving heat resistance. Bars of multilayer coatings having increased the thickness ratio of each layer from 60% to 90%, all secured a hardness of 3200Hv or more, it was confirmed that also excellent adhesion. In addition, the hardness drop rate after heat treatment at 1000 ° C. was within 15%, and the hardness drop rate after heat treatment at 1100 ° C. was within 20%, confirming that excellent heat resistance was obtained.

Although the present invention has been described with reference to the embodiments shown in the drawings, these are merely exemplary and will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible. Therefore, the true technical protection scope of the present invention will be defined by the technical spirit of the appended claims.

Claims (10)

delete delete Preparing Al powder, Cr powder and Fe powder;
Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And
Sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air; Including;
The sintered sintered body is made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al,
Characterized by producing a single target with uniform tissue, composition and hardness,
The mechanical alloying may include performing a ball mill process, wherein the loading amount of the ball and the powder in the ball mill process is 10 to 90%, and the charging ratio of the ball and the powder (Ball: Powder) Is 1: 1 to 20: 1, milling speed is 50 to 500 rpm, milling time is 200 hours or less,
The sintering step is applied to the spark plasma sintering, hot press (hot press) process, the sintering temperature is 300 ~ 1000 ℃, the sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less The sintering time is characterized by applying the conditions of 10 to 100 minutes,
Method for producing a physical vapor deposition target. Preparing a powder selected from Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y, and V;
Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And
Sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air; Including;
The sintered sintered body is 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 to 20 atomic% and The balance consists of an alloy consisting of Al,
Characterized by producing a single target with uniform tissue, composition and hardness,
The mechanical alloying may include performing a ball mill process, wherein the loading amount of the ball and the powder in the ball mill process is 10 to 90%, and the charging ratio of the ball and the powder (Ball: Powder) Is 1: 1 to 20: 1, milling speed is 50 to 500 rpm, milling time is 200 hours or less,
The sintering step is applied to the spark plasma sintering, hot press (hot press) process, the sintering temperature is 300 ~ 1000 ℃, the sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less The sintering time is characterized by applying the conditions of 10 to 100 minutes,
Method for producing a physical vapor deposition target. In a mixed gas atmosphere containing nitrogen and an inert gas for a single target for physical vapor deposition having a uniform structure, composition and hardness composed of an alloy composed of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic%, and balance Al. A nitride hard film formed by performing a physical vapor deposition process,
The nitride hard coating is based on Al, and contains 5 to 25 atomic percent Cr and 0.1 to 4 atomic percent Fe,
The single target for physical vapor deposition is preparing an Al powder, Cr powder and Fe powder; Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. The sintered sintered compact is made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic%, and the balance Al, and the mechanical alloying is performed by a ball mill process. Including the step of performing, in the ball mill process, the loading amount of the ball and the powder is 10 to 90%, the charge ratio of the ball and the powder (Ball: Powder) is 1: 1 to 20: 1, milling speed Is 50 to 500 rpm, milling time is less than 200 hours, the sintering step is applied to the spark plasma sintering, hot press process, the sintering temperature is 300 ~ 1000 ℃, The sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less, the sintering time is characterized by applying a condition of 10 to 100 minutes,
Nitride hard film. Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: alloy composed of 0.1 to 20 atomic% and the balance Al A nitride hard film formed by performing a physical vapor deposition process in a mixed gas atmosphere containing nitrogen and an inert gas to a single target for physical vapor deposition having a uniform structure, composition, and hardness,
The nitride hard coating is based on Al, 5 to 25 atomic% Cr, 0.1 to 4 atomic% Fe, 0.1 to 3.5 atomic% Ti, Zr, Mn, Si, W, Mo, Nb, Y and V Contains any one selected from
The single target for physical vapor deposition is Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V selected from any one powder selected from; Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. Implemented by performing, the sintered sintered body is any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 to 20 atomic% and the balance is made of an alloy consisting of Al, the step of performing the mechanical alloying includes the step of performing a ball mill process, the charge amount of the ball and the powder in the ball mill process is 10 ~ 90 %, The charge ratio of the ball and the powder (Ball: Powder) is 1: 1 to 20: 1, the milling speed is 50 to 500 rpm, the milling time is 200 hours or less, and the sintering step is a spark plasma Sintering (spark plasma sintering), hot press (hot press) process is applied, the sintering temperature is 300 ~ 1000 ℃, the sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less, the sintering time is 10 ~ It is characterized by applying a condition of 100 minutes,
Nitride hard film. Preparing a single target for physical vapor deposition having a uniform structure, composition and hardness consisting of an alloy composed of 9% to 40% by weight of Cr, 0.1% to 6% by weight of Fe, and Al; And
By performing a physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target, based on Al, 5 to 25 atomic% Cr and 0.1 to 4 atomic% Fe Forming a nitride hard film containing a; Including;
The preparing of the single target for physical vapor deposition may include preparing Al powder, Cr powder, and Fe powder; Performing mechanical alloying by mixing the Al powder, the Cr powder and the Fe powder; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. Including, but the sintered sintered body is made of an alloy consisting of Cr: 9 to 40 atomic%, Fe: 0.1 to 6 atomic% and the balance Al, the step of performing the mechanical alloying is to perform a ball mill process Including the step, in the ball mill process, the loading amount of the ball and the powder is 10 to 90%, the charge ratio of the ball and the powder (Ball: Powder) is 1: 1 to 20: 1, milling speed is 50 ~ 500 rpm, milling time is less than 200 hours, the sintering step is applied to the spark plasma sintering, hot press process, the sintering temperature is 300 ~ 1000 ℃, sintering pressure Is 10 to 500 MPa, the degree of vacuum is 2 ^-5 mTorr or less, and the sintering time is characterized by applying a condition of 10 to 100 minutes,
Method for producing nitride hard film. Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, any one selected from Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: alloy consisting of 0.1 to 20 atomic% and the balance Al Preparing a single target for physical vapor deposition consisting of a uniform tissue, composition and hardness; And
By performing a physical vapor deposition (PVD) process in a mixed gas atmosphere containing nitrogen and an inert gas to the physical vapor deposition target, based on Al, Cr: 5 to 25 atomic%, Fe: 0.1 to 4 atomic% Any one selected from among Ti, Zr, Mn, Si, W, Mo, Nb, Y, and V: forming a nitride hard film containing 0.1 to 3.5 atomic%; Including;
The preparing of the single target for physical vapor deposition may include preparing any one powder selected from Al powder, Cr powder, Fe powder, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; Performing mechanical alloying by mixing any one powder selected from the Al powder, the Cr powder, the Fe powder, the Ti, Zr, Mn, Si, W, Mo, Nb, Y and V; And sintering the mixed powder subjected to the mechanical alloying in a vacuum atmosphere or air. Including, wherein the sintered sintered body is completed: any one selected from Cr: 9 to 32 atomic%, Fe: 0.1 to 6 atomic%, Ti, Zr, Mn, Si, W, Mo, Nb, Y and V: 0.1 ~ 20 atomic% and the balance is made of an alloy consisting of Al, the step of performing the mechanical alloying includes the step of performing a ball mill process, the charge amount of the ball and the powder in the ball mill process is 10 ~ 90% , The charge ratio of the ball and the powder (Ball: Powder) is 1: 1 to 20: 1, the milling speed is 50 to 500 rpm, the milling time is 200 hours or less, the step of sintering spark plasma sintering (spark plasma sintering), hot press (sintering) process is applied, the sintering temperature is 300 ~ 1000 ℃, the sintering pressure is 10 ~ 500MPa, the vacuum degree is 2 ^-5 mTorr or less, the sintering time is 10 ~ 100 minutes Characterized by applying the conditions of
Method for producing nitride hard film. AlCr layer made of Al and Cr; And
It includes; the nitride hard film according to any one of claims 5 and 6 formed on the AlCr layer,
Multilayer coating film. The method of claim 9,
The thickness of the nitride hard film is characterized in that from 60% to 90% of the thickness of the multilayer coating film,
Multilayer coating film.

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